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BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to fabrication of devices formed from metallized magnetic substrates, e.g., inductors, transformers, and substrates for power applications.
2. Discussion of the Related Art
Magnetic components such as inductors and transformers are widely employed in circuits requiring energy storage and conversion, impedance matching, filtering, electromagnetic interference suppression, voltage and current transformation, and resonance. These components tend to be bulky and expensive compared to the other components of a circuit. Early manufacturing methods typically involved wrapping conductive wire around a magnetic core element or an insulating body containing magnetic core material. These early methods resulted in circuit components with tall profiles, and such profiles restricted miniaturization of the devices in which the components were used. The size restriction was particularly problematic in power circuits such as power converters.
More recent efforts to improve upon these early manufacturing methods resulted in thick film techniques and multilayer green tape techniques. In a thick film technique, a sequence of thick film screen print operations are performed using a ferrite paste and a conductor paste. Specifically, individual ferrite layers are deposited as a paste to form a substrate, while the conductor paste is deposited between the individual ferrite paste layers to form conductive patterns through the interior of the substrate. Conductor paste is also printed onto the surfaces of the resulting multilayer ferrite substrate to connect the vias, thereby forming spiral windings. Upon firing, a consolidated body containing numerous devices is typically formed.
The green tape technique uses green tape layers composed of ferrite particles and organic binder to form the substrate. Typically, as shown in FIGS. 2A to 2C, numerous holes 22 are punched through each of several green tape layers 20 (for simultaneous formation of numerous devices). As shown in FIG. 2B, the side walls of the holes 22 are subsequently coated with a conductive material 24, and then the green tape layers 20 are stacked and laminated to form a substrate 30. As shown in FIG. 2C, conductor material 32 is printed onto the opposing surfaces of the multilayer substrate 30, and connected to the conductive material 24 coated onto the side walls of the holes 22, such that continuous, conductive windings are formed. The substrate 30 is fired to form a consolidated ceramic, and, typically, a metal such as copper is electroplated onto the windings to provide improved conductivity. Such green tape techniques experience problems, however. For example, due to the numerous, relatively small vias, it is sometimes difficult to attain a uniform electroplated layer in the vias due to mass transport limitations from the electroplating bath to the via surfaces. In addition, the adhesion of the electroplated layer on the conductive material is often problematic in green tape techniques.
Improved methods for forming devices that incorporate metallized magnetic substrates, such as inductors and transformers, are desired. Particularly desired are methods that offer improved fabrication speeds and device yields from a single multilayer substrate.
SUMMARY OF THE INVENTION
The invention provides an improved process for fabricating devices containing metallized magnetic ceramic material, such as inductors and transformers. In an embodiment of the invention, reflected in FIGS. 1A-1D, several layers of unfired magnetic material, typically ferrite tape, are provided. The vias 12, 13 of the invention are punched into the layers individually, at the same locations in each layer. Each via 12, 13, as initially punched, is capable of contacting two opposing windings, as reflected in FIG, 1C. (The vias 13 along the outer edges are referred to herein as outer vias, in contrast to the inner vias 12. These outer vias 13, due to their location along the edges of the substrate, are not intended to contact two opposing windings 16 of devices. It is possible, however, as reflected in FIGS. 1C and 1D, for an outer via 13 to contact both a winding 16 of a device and an opposing connection 15 to a bus 17.)
The layers are then stacked such that the vias 12, 13 are aligned, and the layers are laminated to form a substrate 10 of the unfired magnetic material. The side walls of the aligned vias 12, 13 are coated with a conductive material 14, e.g., a silver- and palladium-containing ink (the term ink indicating a viscosity of about 5,000 to about 300,000 cp). Then, without expanding the dimensions of the vias 12, 13, e.g., without an additional punching step that contacts the vias, the top and bottom surfaces of the substrate 10 are coated with a second conductive material 16 to connect the side wall coatings of adjacent vias 12, 13, thereby forming conductive windings. It is then possible to score the substrate 10, as shown in FIG. 1D, to ease subsequent separation of devices. The substrate is fired, and additional metal, e.g., copper, is electroplated over the conductive material to form the finished devices.
The invention represents an improvement over the type of green tape technique discussed in co-assigned U.S. patent application SER. No. 08/923591 (our reference Fleming-Johnson-Lambrecht-Law-Liptack-Roy-Thomson 13-49-831-3-20-36) (referred to herein as the '591 application), the disclosure of which is hereby incorporated by reference. As reflected in FIGS. 3A to 3D, the '591 application discloses a method involving the following steps: (a) punching vias 42 in individual green ferrite sheets 40, (b) coating the side walls of the vias 42 of each sheet 40 with a conductive material 44, (c) punching large apertures 46 that intersect the vias 42 in each sheet 40 and thereby expand the dimensions of the vias 42, (d) laminating the sheets 40 with the vias 42 aligned to form a substrate 50, and (e) coating the surfaces of the substrate 50 with a second conductive material 48 to connect the coating 44 of the via 42 side walls, thereby forming windings. (Alternatively, the steps of punching the vias and punching the apertures are interchanged.) The substrate is then fired, and a metal, e.g., copper, is electroplated over the metal ink. The apertures 46 are needed to open up access to the interior of the substrate 50, because uniform electroplating is difficult to attain in the small, narrow vias 42. In practice, it is necessary, before laminating the sheets 40 in step (d), to coat the surface of internal sheets with a conductive material, i.e., provide internal metallization, to connect the exposed vias with an external electroplating bus. This internal metallization is required to distribute current for electroplating because the apertures 46, as shown in FIG. 3C, create discontinuities in the first and second conductive materials 44, 48. Unfortunately, the time and expense required to provide such internal metallization, including the cost of the metal itself (Pd and Ag are commonly used), is typically disadvantageous. Also, the presence of the internal metallization demands a greater spacing between individual devices in a substrate, thereby reducing the number of devices capable of being produced in a single substrate. And the internal metallization is not always adequate to provide uniform plating, due to the difficulty in attaining good connectivity between the external and internal metallization.
In contrast to the above process, the present invention's use of vias capable of contacting two opposing winding (see FIG. 1C) allows for device fabrication using only a single punching step for each green tape layer. The single punching step in turn makes it possible to laminate all the unfired layers prior to coating the side walls of the vias, such that the vias of all the tape layers are coated simultaneously. Moreover, since no apertures are punched, i.e., the via dimensions are not expanded, there is no need for internal metallization. The invention thereby provides for green tape fabrication of devices in a manner faster and less complex than the above method.
The invention also relates to use of an improved conductive material to coat the surfaces of the ferrite substrates and the inner walls of the vias. The conductive material, which is applied as a conductive ink, contains silver/palladium particles, ferrite particles, an organic based binder (advantageously cellulose-based), and a solvent. (As used herein, silver/palladium particles indicates the presence of silver particles and palladium particles or of silver-palladium alloy particles.) Surprisingly, when copper is electroplated onto this improved conductive material using a copper pyrophosphate bath, the plated copper advantageously exhibits a pull strength of about 5 kpsi. By contrast, use of a conventional copper sulfate acid bath typically provides pull strengths of about 2 kpsi or less. (Pull strength indicates the strength of 0.08 inch diameter, 125 μm thick copper dots electroplated onto fired conductive material, the strength measured by attaching copper studs to the dots with epoxy and measuring the pull strength by conventional methods.) In addition, it was found that use of the copper pyrophosphate bath was effective in uniformly electroplating the side walls of multilayer laminates, i.e., uniformly electroplating narrow, deep vias.
BRIEF DESCRIPTION OF THE DRAWINGS
FIGS. 1A to 1D show one embodiment of the invention.
FIGS. 2A to 2C show a prior art method for forming devices.
FIGS. 3A to 3D show an alternative green tape method for forming devices.
DETAILED DESCRIPTION OF THE INVENTION
An embodiment of the process of the invention is shown in FIGS. 1A-1D. Several green tape layers of a magnetic material are provided. It is possible to use a single layer, but greater than two layers are typically used. The magnetic material is selected from any magnetic material capable of being metallized, e.g., magnetic ceramics and polymers loaded with magnetic particles, and typically has a magnetic permeability of about 400 to about 1000, and an electrical resistivity greater than about 10 6 ohm-cm. Green tape indicates a flexible material containing an organic binder and particles of the magnetic material. Typically, the tape contains about 8 to about 10 weight percent binder, based on the weight of the tape, with the remainder composed of a ceramic powder. Advantageously, the magnetic material is a spinel ferrite of the form M 1+x Fe 2-x O 4-z , where x and z range from -0.1 to +0.1. M is typically at least one of manganese, magnesium, nickel, zinc, iron, copper, cobalt, vanadium, cadmium, and chromium. Advantageous ferrites are those exhibiting relatively high resistivities, e.g., about 10 4 ohm-cm or higher, such as nickel-zinc ferrites and certain manganese-zinc ferrites, which are also known as soft ferrites. (Soft magnetic materials such as soft ferrites have coercivity less than about 10 Oe and are typically demagnetized in the absence of an external magnetic field.) Other suitable ferrites include so-called microwave ferrites, e.g., the garnet structure, or so-called square-loop ferrites, e.g., where M is manganese or magnesium. (Microwave ferrites are used for devices such as microwave circulators at frequencies in the range of 0.5 to 50 GHz. Square-loop ferrites exhibit a hysteresis loop with moderate coercivity and moderate remanence, and thus are capable of both retaining a flux density and being demagnetized in moderate magnetic fields.)
As shown in FIG. 1A, vias 12, 13 are punched into each green tape layer, at the same locations in each, and the layers are then stacked and laminated to form a multilayer substrate 10. Some of the vias 13 will be located along outer edges of the substrate (the left and right edges of the substrate shown in FIG. 1A). As mentioned previously, these vias 13 along the outer edges are referred to herein as outer vias, in contrast to the inner vias 12. These outer vias 13, due to their location along the edges of the substrate, are not intended to contact two opposing windings of devices. Typically, however, as reflected in FIGS. 1C and 1D, an outer via 13 will contact both a winding 16 of a device and an opposing connection 15 to a bus 17. The bus distributes the needed current during electroplating. While rectangular vias are shown in the Figures, it is possible to form vias of a variety of geometries, e.g., square, circular, eliptical. Vias having aspect ratios (i.e., the ratio of the long to short axis) of about 1 to about 4 have been found to be useful. Vias 12, 13 are typically formed by placing the green tape layers in a suitable punch press. For green tapes formed from ceramic powder and organic binder, it is possible to laminate several layers of tape by pressing the layers together at a relatively low pressure, e.g., 250-3000 psi, at a temperature of about 50-100° C. To provide proper alignment of multiple layers, registration holes are typically punched in each layer during via formation, and registration rods are then placed through the holes to align the layers prior to lamination.
As shown in FIG. 1B, the side walls of the vias 12, 13 are coated with a first conductive material 14, e.g., a conductive ink. (The conductive material typically has a resistivity less than 10 -4 ohm-cm after firing.) The coating step advantageously results in formation of continuous side walls. (A few discontinuities, e.g. pinholes, are acceptable as long as the post-fired conductive material is capable of being electroplated.) Useful conductive inks include those containing silver and/or palladium particles, or silver-palladium alloy particles (the silver and palladium generally used in a 70Ag:30 Pd weight ratio). Typically, conductive inks contain the metal as a particulate suspension in an organic binder, such that the ink is capable of being coated or screen printed. To coat the side walls of the vias 12, 13 the first conductive material 14 is normally drawn through the vias using vacuum suction, optionally using a coating mask cut to match the via pattern in substrate 10. Other coating or deposition methods are also possible.
As shown in FIG. 1C, following coating of inner side walls of vias 12, 13, the top and bottom surfaces of the substrate 10 are coated with a second conductive material 16, having post-fired properties similar to the first conductive material 14. Typically, the second conductive material 16 is screen printed to form a desired metallization pattern, e.g., windings, circuit lines, and surface mount pads. The pattern formed from the second conductive material 16 contacts the material 14 coated onto the side walls of the vias 12, 13, thereby forming continuous, conductive windings. As reflected in FIG. 1C, no expansion of the dimensions of the vias are needed, e.g., the vias 12, as initially punched, are capable of contacting two opposing windings. (The description of "no expansion of the dimensions of the vias" means that no affirmative expansion is performed, e.g., by further punching steps. Expansion of the vias due to other process steps, e.g., heat expansion during firing, is contemplated.) It is also possible to provide the surface coating of conductive material prior to lamination, and/or prior to via side wall coating. A bus 17 is also formed, along with contacts 15 from the bus 17 to the first conductive material 14 deposited in the outer vias 13.
The second conductive material 16 is advantageously a conductive ink similar to the first conductive material 14 used to coat the inner side walls of the vias 12. Where the substrate 10 is formed from a ferrite, it is advantageous for the first conductive material 14 and the second conductive material 16 to be silver- and palladium-containing ink that contains ferrite particles and an organic binder, advantageously a cellulose-based binder, this conductive ink discussed in detail below. Advantageously, the ink contains the same type ferrite as the substrate to improve adhesion to the substrate upon firing. When such a silver- and palladium-containing ink is used for the second conductive material 16, the ink is typically screen printed to a wet thickness of 25 to 75 μm. Subsequent to forming the surface metallization, it is advantageous to scribe dice lines 18 into the green tape 10, as shown in FIG. 1D, to facilitate separation of devices subsequent to sintering of the article. It is also possible to omit the dice lines, and instead saw the devices apart after sintering is complete.
After the windings are formed in the substrate 10, the substrate 10 is fired. Firing drives solvent and binder from the first and second conductive material 14, 16, thereby adhering the metal particles to the substrate 10, and the firing also sinters the substrate 10 to a dense ceramic. Copper is then electroplated onto the fired conductive material 14, 16, generally to a thickness of about 1 to about 10 mils, to form the final devices. The bus 17 and contacts 15 to the outer vias 13 provide the needed current during electroplating. It is possible to use a variety of conventional electroplating baths to deposit the copper onto the conductive material, and such baths are discussed generally in Metal Finishing Guidebook, Vol. 94, No. 1A, 1996. Other conductive plating materials are also possible. Electroless plating is possible, but is typically slower and incapable of adequately providing a plating of desired thickness.
The first and second conductive materials discussed in the embodiment above are advantageously a conductive ink containing silver/palladium particles, ferrite particles, an organic binder, and a solvent, where the solvent primarily solvates the binder. Use of ferrite particles are advantageous for improving adhesion of subsequent electroplating deposits on the conductive material, and for reducing the amount of costly silver and palladium material that is required. The silver/palladium particles are typically used in a weight ratio of 60-80 Ag:40-20 Pd (typically 70 Ag:30 Pd), and have an average diameter of about 1 μm. The improved ink advantageously contains about 10 to about 50 wt. % ferrite particles, more advantageously about 20 to about 40 wt. %, in the post-fired material (i.e., based on the weight of the ferrite and conductive particles). Less than 10 wt. % ferrite particles typically results in an undesirably small increase in adhesion strength and cost reduction, while greater than 50 wt. % ferrite particles typically results in undesirably high electrical resistivity, which interferes with subsequent electroplating. The ferrite particles typically have an average diameter of about 0.2 to about 2.0 μm, advantageously about 1.5 μm. The ink typically contains about 1 to about 3 wt. % of the organic binder, and about 10 to about 40 wt. % of the solvent, based on the weight prior to firing. At lower amounts of binder and solvent, the viscosity of the ink is typically too high to use in the process described above, while at higher amounts, the viscosity is typically too low. The organic binder provides desired rheology and strength to the green structure. The binder is advantageously cellulose-based and more advantageously ethyl cellulose. A variety of solvents are useful, including α-terpineol and mineral spirits.
It is possible to fabricate the improved conductive ink by a variety of processes. In one such process, the binder is dissolved in a first solvent until substantially wet by the solvent. Particles of the ferrite and the conductive material are separately mixed with a second solvent (which is the same or different than the first solvent), e.g., ethanol, and typically a small amount, e.g., less than 1 wt. %, of a dispersant material such as oleic acid or another fatty acid. Once the powder mixture has settled, about 50-70 wt. % of the solvent is extracted. The appropriate amount of the binder solution is added to the metal powder to provide the desired amount of the binder material in the metal ink. Typically an additional amount of solvent is then added, and the components are mixed to provide the conductive ink. Viscosity of the ink is typically adjusted by altering the amount of solvent and/or binder. It is possible to use a control sample to determine the appropriate amounts of the components to provide a desired result. Normally, a less viscous ink is desired when plating the side walls of vias, e.g., 5,000 to 50,000 cp, whereas a more viscous ink, e.g., 30,000 to 300,000 cp, is useful for screen printing onto a surface of a ferrite substrate.
It was found that use of this improved conductive ink in combination with copper electroplating by a copper pyrophosphate bath provided desirable pull strengths for the plated copper. In particular, copper plated in this manner advantageously exhibits a pull strength greater than about 4 kpsi, more advantageously above 5 kpsi. (Pull strengths were measured as described in Comparative Example 1 and Example 3 below.)
A copper pyrophosphate bath generally contains four components. Copper pyrophosphate is the source of copper and a complexing ion. Potassium pyrophosphate further provides a complexing ion, and an amount of free pyrophosphate required for plating. Potassium nitrate provides for good anode corrosion. And ammonia (typically introduced as ammonium hydroxide) provides morphology control of the plated deposit. Typically, conventional pH adjusting compounds are also used. A useful, commercially-available pH lowering compound is "Compound 4A" available from ATOTECH, and pyrophosphoric acid is similarly suitable. A useful pH raising compound is potassium hydroxide. Optionally, an additive is included to provide leveled, bright deposits, such additives commercially known and available. One such additive is additive PY61H, available from ATOTECH. Typically, leveler/brighteners consist of materials having organic backbones with attached alkoxy and/or hydroxyl groups.
A variety of parameters have been found to be particularly useful for plating copper on devices, particularly in the process for forming devices discussed above, utilizing copper pyrophosphate plating baths. The temperature of the bath is advantageously 50 to 55° C. Below 50° C., the quality of the deposit is reduced, and above 55° C., pyrophosphate undesirably begins rapid conversion to orthophosphate. The pH of the bath is advantageously 7.8 to 8.5, more advantageously 8.0 to 8.5. At pH values below 7.8, pyrophosphate undesirably begins rapid conversion to orthophosphate. At pH values above 8.5 the quality of the deposit is reduced. Anodes are advantageously oxygen-free copper. The ammonia is advantageously present in an amount ranging from 6 to 10 mL per L of bath solution. At lower ammonia concentrations, line definition is typically poor and spreading of the deposit from the conductive material onto the substrate occurs. At higher ammonia concentrations, the deposit tends to exhibit undesirable internal stresses. The orthophosphate concentration is advantageously less than 60 g/L, above which the orthophosphate lowers the quality of the plated deposit. The ammonium nitrate is advantageously present at a concentration of 8 to 12 g/L, within which desirable plating efficiency is attained. The ratio of pyrophospate to copper is advantageously 7.7 to 8.5. The copper concentration is advantageously 19.0 to 25.0 g/L. Plating is advantageously performed at a current density of 25 to 50 ASF (amperes per square foot). It is possible to use a control sample to determine the particular parameters that will provide a desired result.
A useful, commercially available copper pyrophosphate bath is the UNICHROME™ bath made by ATOTECH.
In the invention, it was found that use of copper pyrophosphate electroplating provided adequate uniformity of copper on the via side walls, even with deep, narrow vias having a large depth to width ratio. Thus, there is no need to punch large apertures to provide adequate electroplating, as in U.S. patent application Ser. No. 08/923591, referenced previously. And without the apertures, there is no need for internal metallization to provide electrical contact during electroplating. Eliminating the internal metallization reduces the complexity and cost of the process by removing the steps of printing metallization on internal green tape layers. A lack of internal metallization also improves the yield of the process because the devices are able to be spaced closer together, and faults due to poor connectivity between internal and external metallization are reduced.
The invention will be further clarified by the following examples, which are intended to be exemplary.
EXAMPLE 1
Formation of Silver- and Palladium-containing Conductive Inks Containing Ferrite Particles:
A binder solution was formed by dissolving ethyl cellulose in octerpineol, at a cellulose-terpineol weight ratio of between 1:10 and 1:12. The mixture was allowed to stand until the ethyl cellulose was substantially wet. The mixture was then passed through a 3-roll mill to further mix and homogenize the solution.
Silver and palladium particles (70:30 weight ratio) and ferrite particles (the metal particles having average diameters of about 1 μm) were mixed with ethanol, in an amount approximately half the total weight of the metal particles, and 0.5 wt. % oleic acid was then added. (The amount of each type of metal was determined based on the desired ferrite loading.) The mixture was then ultrasonicated for about 5 minutes. After several hours of settling of the metal particle mixture, about 60 wt. % solvent was extracted. The metal powder, however, was not allowed to dry.
The amount of binder solution needed to provide about 1.8 wt. % ethyl cellulose, based on the weight of the total ink (metal, ferrite, binder, and solvent) was determined, and that determined amount was added to the metal powder. The mixture was manually mixed and placed onto a slow roller mill for homogenization. The mixture was placed onto a 3-roll mill to evaporate the ethanol and obtain a desired viscosity. If necessary, additional α-terpineol was added to adjust the viscosity.
As prepared, the ink contained 74±2 wt. % metal powders and 1.8±0.1 wt. % ethyl cellulose, based on the weight of the overall ink composition.
EXAMPLE 2
Formation of a Device
An array of four turn, three layer surface mountable inductors was prepared in the following manner. Three 5"×5"×0.29" green, nickel-zinc ferrite (approximately Ni 0 .4 Zn 0 .6 Fe 2 O 4 ) tape layers were provided. Each tape contained ferrite powder and about 8 to about 10 wt. % organic binder. Vias having dimensions of 0.30"×0.35" were punched in each tape layer individually, such that two adjacent devices would share four vias. Registration holes were also punched in each layer to allow subsequent stacking of the layers. Planar conductor patterns (for windings and surface mount pads of the inductors), plating buss interconnects, and reference marks for scoring between the devices (to promote later separation) were provided on the top surface of the first tape layer and the bottom surface of the third tape layer. The planar conductor patterns and buss interconnects were formed from a silver- and palladium-containing ink made according to Example 1, containing 35 wt. % ferrite particles and 2 wt. % ethyl cellulose binder, with α-terpineol included to provide a desired viscosity.
The three tape layers were then stacked on a steel registration fixture and laminated together at a temperature of about 80 to about 90° C. and a pressure of about 250 to about 500 psi. Lamination caused the binder of the three layers to soften and fuse, thereby forming a relatively strong monolithic array. The side walls of the vias were then coated with the same metal ink used for the surface metallization. The viscosity of the ink was reduced beyond that used for the above printing step by addition of α-terpineol. The side walls were coated by drawing the ink through the vias with vacuum, to leave a coating on the side walls. After the ink dried, the array was scored on its top and bottom surfaces (as reflected in FIG. 1D) to promote singulation of the inductors subsequent to sintering and electroplating.
To co-sinter the ferrite and metal components, the array was placed on a flat Alundum® setter that was dusted with a sintered ferrite powder of the same composition (to prevent the substrate from sticking to the Alundum™M). The array was then heated from room temperature to 500° C. over about 24 hours to volatilize the organic components of the tape and ink in a controlled manner. The temperature was further raised to about 1100° C. over about 24 hours, including a four hour treatment at about 1100° C. and cooling to room temperature. All heating was performed in a flowing air atmosphere (2.5 L/minute).
Plating of the fired array was performed in a copper pyrophosphate bath similar to the bath of Example 3, at 25 ASF, to a thickness of 0.005".
COMPARATIVE EXAMPLE 1
Pull Strength Measurements Using Copper Plated in Copper Sulfate Acid Bath
A set of 0.08 inch diameter dots was patterned onto a green ferrite tape, using conductive ink made according to the process of Example 1, having the ferrite loading discussed below. The tape was then fired in air at about 1100° C. for 4 hours. Copper was electroplated onto the dots to a thickness of 125 μm. The electroplating was performed in a copper sulfate acid bath at 25 ASF and room temperature. The bath contained 58.9 g/L of CuSO 4 , 120.0 mL/L of H 2 SO 4 , 3.0 mL/L of ATOTECH Cupracid Brightener, 15 mL/L of ATOTECH Cupracid BL-CT Basic Leveler, and 0.14 mL/L of HCl. Plating was performed at 25 ASF and room temperature. Copper studs were then attached to the copper dots with epoxy, and the pull strength was measured in a conventional manner using a Sebastian pull test apparatus.
This process was repeated for 8 samples using an ink containing 5 wt. % ferrite, based on the weight of the ink, and 8 samples using an ink containing 25 wt. % ferrite, based on the weight of the ink. For the 5 wt. % ferrite ink, the average pull strength was 1.70 kpsi, with a standard deviation of 74.00%. For two 25 wt. % ferrite samples, the average pull strengths were 1.26 kpsi with a standard deviation of 52.70%, and 1.68 kpsi with a standard deviation of 32.30%.
EXAMPLE 3
Pull Strength Measurements Using Copper Plated in Pyrophosphate Bath
A set of 0.08 inch dots was patterned onto a green ferrite tape, using conductive ink made according to the process of Example 1 with a ferrite loading of 25 wt. % based on the weight of the fired ink. The tape was then fired in air at 1115° C. for 4 hours. Copper was plated onto the dots to a thickness of 125 μm. The plating was performed in a copper pyrophosphate bath under the following conditions:
Bath:
210 mL of ATOTECH C-10 (66.7 g/L Cu; 499.5 g/L P 2 O 7 );
1980 mL of ATOTECH C-11 (481.5 g/L P 2 O 7 );
54 mL of NH 4 OH;
Initial pH of 10.10, adjusted and maintained at 8.15 by addition of pyrophosphoric acid.
Plating Conditions:
Temperature: 52° C.;
30 minutes at 5 ASF, followed by 200 minutes at 25 ASF.
Copper studs were then attached to the copper dots with epoxy, and the pull strength was measured in a conventional manner using a Sebastian pull test apparatus.
Nine samples were prepared in this manner. The average pull strength for the nine samples was 5.413±0.434 kpsi
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The invention provides an improved process for fabricating devices containing metallized magnetic ceramic material, such as inductors, transformers, and magnetic substrates. In particular, the unique vias utilized in the process of the invention allow fabrication of devices from multiple unfired ferrite layers with only a single via-coating step, thereby avoiding the need numerous punching steps. Moreover, there is no need for expanding the dimensions of the vias and thus no need for internal metallization. The invention therefore provides for green tape-type fabrication of devices such as inductors, transformers, and magnetic substrates in a manner faster, less complex, and more reliable than current methods. The invention also relates to use of an improved conductive material in such a process, the conductive material containing silver/palladium particles, ferrite particles, a cellulose-based or other organic binder, and a solvent. After firing of the substrate onto which the ink has been coated, and plating of copper thereon by a copper pyrophosphate bath, the plated copper exhibits a pull strength greater than about 4 kpsi, advantageously greater than about 5 kpsi. Use of a copper pyrophosphate bath also allow uniform plating within long, narrow vias.
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BACKGROUND OF THE INVENTION
The invention relates to a device for adjusting the feed amount of a fabric being sewn, and more particularly to such a device that in the case of selecting an ordinary pattern stitch by fixedly setting the fabric feed amount, such as the zigzag stitching, the feed amount is increased or decreased with respect to a reference value thereof within a determined range by rotating a feed adjusting knob outside of the machine frame. Also, and in the case of selecting a super pattern stitch, the amount of forward or backward feed is enlarged or reduced within a determined range by rotating the knob.
In conventional sewing machines having both functions, the ordinary stitching and the super stitching are both independent in adjustment of the feeding mechanism. Therefore, it is difficult to provide these two adjustments via a single member. The fabric feed amount is in general is subject to the ordinary pattern stitching only. For forming the super pattern stitching, for example, stretch stitching or honey stitching, and if the fabric has high elasticity or large thickness, the fabric feed could not be fully obtained and would result in problems in the final product.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a sewing machine which has both functions of the ordinary pattern stitching such as zigzag stitching, and the super pattern stitching to which the forward and backward feeds are automatically given. The feed amount specified to a pattern, which is given from a feed cam fixed on an operating shaft of a pattern selecting dial, is increased or decreased within a determined range by operating a feed adjusting knob outside of the machine frame, and for selecting the super pattern, the amount of the forward and backward feed given by the automatic feed cam is enlarged or reduced within the determined range by operating the feed adjusting knob. Furthermore, the ordinary and the super stitchings may be performed by adjusting the feed amount in response to conditions of the fabric to be sewn.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a sewing machine where a feed adjusting device according to the present invention is installed;
FIG. 2 is a perspective view showing an element mechanism of the sewing machine;
FIG. 3 is a partial exploded view showing the element mechanism of FIG. 2;
FIGS. 4 and 5 show views seen from arrow A in FIG. 2;
FIGS. 6 to 8 show each adjusting condition of selecting ordinary pattern stitching, wherein FIG. 6 shows setting a dial at center of adjusting range thereof, FIG. 7 shows rotation of the dial in a plus (+) direction until the maximum position of the adjusting range, and FIG. 8 shows rotation of the dial in a minus (-) direction until the maximum position of the adjusting range,
FIGS. 9 to 12 show each adjusting condition of selecting the super pattern stitching, wherein FIGS. 9 and 10 are shown settings of the dial at center of the adjusting range, each showing forward feed and backward feed by means of an automatic feed cam, and FIGS. 11 and 12 are rotation of the dial to the plus (+) direction from the conditions in FIGS. 9 and 10, each showing the forward feed and the backward feed by means of the cam.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The present invention will be explained with reference to the attached drawings. In FIG. 1, a front panel 1 of a sewing machine is disposed with a pattern selecting dial 2 and a feed control knob 3. When the ordinary pattern stitching, such as zigzag stitching, is selected by the dial 2, the fabric feed amount is continuously changed by rotating the knob 3 within a range of, e.g., ±50% under a condition that the fabric feed amount specified to each of the stitching patterns is at the reference value as will be later mentioned. When the super pattern stitching is selected, the pitch of the forward or backward feed is enlarged or reduced by the knob 3 in the forward or backward direction.
In FIG. 2, a main shaft 4 is rotatably mounted to an arm shaft of the sewing machine, and is rotated by a driving source (not shown).
Also referring to FIG. 3, a cam shaft 8 is held on an arm frame by a hole 6a defined in a support plate 6 secured to the arm frame by a screw 5. Cam shaft 8 is effected with a thrust stop by means of a grip ring 7. The cam shaft 8 is mounted with a worm wheel 10 gearing a worm 9 fixed on the main shaft 4, a cam group 11 for needle swinging amplitude which is rotated together with the worm wheel 10, and a cam 12 for automatic feed. The cam shaft 8 is rotatably mounted with a selecting plate 13 through a hole 13a defined therein which is biased by a spring (not shown) to the clockwise direction around the cam shaft 8. An operating shaft 14 is supported on the arm frame parallel to the cam shaft 8. This shaft 14 is secured with a selecting cam body 15 and a cam body 16. The selecting cam body 15 has an outer cam 15a (seen in FIG. 3) for selecting the cam group 11 and an axial cam 15b. The cam body 16 has a feed cam 16a which generates a constant feed particular to each of the stitching patterns for the zigzag stitching, and a super stitch selecting cam 16b which contacts, as later will be mentioned, a follower 17a of a feed arm 17 to a cam 12. The operating shaft 14 is operated by the pattern selecting dial 2 outside of the machine frame. The selecting cam 16b follows a pin 13b of a selecting plate 13.
A needle supporter 18 is pivoted at its upper portion on a pin 20 secured to the arm frame 19 and biased by a spring (not shown) to the counterclockwise direction in FIG. 2. It supports at its lower portion a needle bar 22 which holds a needle 21. The needle bar 22 is vertically moved in association with rotation of the main shaft 4 by means of a needle bar holder 23 fixed to the needle bar and crank mechanisms.
A swinging amplitude transmission lever 24 is rotatably pivoted in the lateral direction at its base on an upper portion of the needle bar supporter 18, and is biased by a spring 26 (FIG. 4) around the pin 25 in the clockwise direction (seen from the upper part in FIG. 2). The transmission lever 24 is formed at its end with a first amplitude follower 24a which is contacted to the cam group 11 by biasing force of a spring (not shown), and is provided at its center with a member 27 by a pin 28 and a screw 29, the member 27 being provided with a follower 27a which is integrally formed with a point contacting portion to an outer cam 15a of the selecting cam body 15 and a side contacting portion to the axial cam 15b. With reference to FIG. 5, pattern selection is carried out by meeting an indicator 30 to one of the stitching pattern indications (Pi) appearing on the pattern indicating panel 31 through rotation of the dial 2. In the course of pattern selection by rotation of the dial 2, the first follower 24 a is released from the cam group 11 by the outer cam 15a, and the swinging amplitude transmission lever 24 is rotated by the axial cam 15b around the pin 25 via the follower 27a. As a result, the first follower 24a is moved toward the direction of the cam group 11, and is contacted by the axial cam 15a to one cam of the cam group 11.
Referring to FIG. 3, a feed arm 17 is mounted on a rod portion 13c of the selecting plate 13 via a boss 17b thereof and is biased by a spring 32 to the counterclockwise direction. The feed arm 17 is effected with the thrust stop by means of E-ring 33. Further the feed arm 17 is inserted with a screw 34 into a hole 17c at its end portion, the screw 34 being secured with a nut 35 and a rod 36 via screw portion 36a. The rod 36 is inserted with a pin 37a of the feed arm 37 into a hole 36b thereof and is effected with the thrust stop by means of E-ring 38. The feed arm 37 inserts at its rod portion 37b into a holes 6b and 6c of the plate 6, and the rod portion 37b is effected with the thrust stop by means of E-ring 39. Around these holes, the selecting arm 40 is mounted on the rod portion 37b via the boss 40a, and is biased by a spring 41 to the clockwise direction, so that its pin 40b follows the feed cam 16b. The selecting arm 40 is provided on its screw portion 40c with a nut 42 and a screw 43. When selecting the ordinary stitching, the screw 43 contacts at its lower part an upper face 37c of the feed arm 37, as mentioned infra, in order to restrain rotation of the feed arm 37 in the clockwise direction in FIG. 3. A shaft 44 securing the knob 3 is equipped with a wave shaped washer 45 and E-ring 46 for generating friction with respect to the arm frame when the shaft 44 is rotated. A feed control cam 47 formed with a groove cam portion 47a is secured by a screw 48 on the shaft 44 via holes 47b and 47c. A feed adjust arm 49 is formed with holes 49a and 49b into which a pin 6d of the plate 6 is inserted, and is effected with a thrust stop by means of E-ring 50. The pin 49c is engaged in a groove portion 47a, and when the knob 3 is rotated, the feed adjusting cam 47 is rotated and the feed adjusting arm 49 is turned.
The feed arm 37 is pivoted in its hole 37d with the feed arm 51 via its pin 51b on an end thereof, which is formed with an oblong groove 51a in the vicinity of its middle part, and is effected with a thrust stop by means of E-ring 52. The oblong groove 51a is inserted with a pin 49d of the feed adjusting arm 49, and a pin 51c on the other end is connected with a rod 53 via a hole 53a, and is effected with a thrust stop by means of E-ring 54. The rod 53 is inserted in its oblong groove 53b with a pin 55a of the feed adjusting plate 55, and is effected with a thrust stop by means of E-ring 56.
A feed adjustor 57 is mounted on its boss 57a with a boss 55b of a feed adjusting plate 55. The adjustor 57 is biased in the clockwise direction by means of a spring 58 whose one end is held on one end of a pin 57b. The adjustor 57 is contacted at its upper face 57c to a screw 60 on its lower face which is secured in the screw 55c of the feed adjusting plate 55 together with a nut 59 in order to limit rotation thereof. The adjustor 57 is pivoted on a shaft 61 which is attached to the arm frame by a bush 62 and a screw 63. As mentioned above, the feed adjustor 57 is biased by the spring 58 to the clockwise direction via the pin 57b, so that the feed adjusting plate 55 is biased in the same direction via the screw 60 contacting the feed adjustor 57 on its upper face 57c, and the feed arm 51 is biased in the same direction around the pin 49d of the feed adjusting arm 49 via the rod 53, and further the feed arm 37 is biased to the shaft 37b via the pin 51b.
Reference is now made to the operation of the present device as described above. According to the feed adjusting device of the present invention when the ordinary pattern, such as the zigzag stitching, is selected by rotating the dial 2 the fabric feed amount can be continuously changed by rotating the knob 3 at the appropriate rate, for example, within a range of ±50%, under the condition that the fabric feed amount specific to each of the stitching patterns is a reference value. That is, when the ordinary stitch is selected by rotating the dial 2, the pin 40b of the selecting arm 40 follows the feed cam 16a which gives the fabric feed for the ordinary stitching. FIG. 6 shows that the knob 3 is set at the center of the adjusting range under this condition. The feed arm 51 which is indirectly biased by the spring 58 in the clockwise direction to the pin 49d of the feed adjusting arm 49 is positioned at the position where the feed arm 37 contacts the lower end of the screw 43 at its upper face 37c. Under this condition, the center of the rod portion 37b of the feed arm 37 meets the center of the pin 49d of the feed adjusting arm 49, and the feed arm 51 is made oblique by θ 1 from the position where the pin 51c gives the feeding amount 0 to the feed adjustor 57 around the pin 49d, thereby obtaining a certain forward feeding amount of the fabric.
When the feed adjusting knob 3 is rotated to the maximum in the plus (+) direction as shown in FIG. 7 the feed adjusting cam 47 rotates and the feed adjusting arm 49 is rotated by β 1 as shown at the pin 6d so that the pin 49d is moved within the oblong groove 51a, whereby the pin 51c of the feed arm 51 is made further oblique by α 1 . Then the condition shown in FIG. 6 and the feeding amount is increased by a certain rate in the forward feeding side with respect to the condition shown in FIG. 6.
When the feed adjusting knob 3 is rotated to the maximum in the minus (-) direction as shown in FIG. 8, the feed control cam 47 rotates and the feed adjusting arm 49 is rotated by β 2 as shown at the pin 6d so that the pin 49d is moved within the oblong groove 51a, whereby the pin 51c of the feed arm 51 is decreased in the obliquity by α 2 . Then the condition shown in FIG. 6 and the feeding amount is decreased by a certain rate in the forward feeding amount with respect to the condition shown in FIG. 6.
Since the knob 3 can be continuously rotated, the feed arm 51 can be continuously adjusted accordingly, with regard to the oblique angle within the range of θ 1 +α 1 and θ-α 2 in the above mentioned example, and the feeding amount can be set at the desired value.
According to the feed adjusting device of the present invention, in the selection of the super pattern the amount of the forward or backward feed may be enlarged or reduced at the certain rate. That is, when the dial 2 is rotated to select the super pattern, a corresponding cam is selected from the cam group 11 and the selecting plate 13 is rotated by the selecting cam 16b around the cam shaft 8 to the counterclockwise direction via the pin 13b, in FIG. 3, so that the feed arm 17 goes down to cause the follower 17a to contact the cam 12. Furthermore the selecting arm 40 is rotated by the selecting cam 16a around the boss 40a in the clockwise direction via the pin 40b. The arm 37, which is connected to the feed arm 17 via the screw 34 and the rod 36, is turned by the cam 12 under the condition that the upper face 37c of the feed arm 37 does not contact the lower end of the screw 43 fixed to the selecting arm 40. The feed arm 51 is turned by the feed arm 37 around the pin 49d of the feed adjusting arm 49 via the pin 51b. When the knob 3 is set at the center of the adjusting range under the above mentioned condition, the constant forward or backward feed is obtained.
In FIGS. 9 and 10, the screw 43 of the selecting arm 40 is separated from the feed arm 37, and the selecting plate 13 is rotated by the selecting cam 16b in the counterclockwise direction so that the follower 17a of the feed arm 17 follows the cam 12 and the feed amount is given by the cam 12. When the knob 3 is set at the center of the adjusting range, the center of the rod portion 37b of the feed arm 37 meets the center of the pin 49d of the feed adjusting arm 49. In FIG. 9, the follower 17a follows the concave portion of the cam 12. The feed arm 51 is made oblique by ε 1 in the clockwise direction around the pin 49d via the feed arm 17, the screw 34, the rod 36 and the feed arm 37, from the position where the pin 51c gives the feed amount 0 to the feed adjustor 57, and thus the required forward feed is obtained. In FIG. 10, the follower 17 the follows a convex portion of the cam 12. The feed arm 51 is made oblique by ε 2 in the counterclockwise direction around the pin 49d, via the feed arm 17, the screw 34, the rod 36, and the feed arm 37, from the position where the pin 51c gives the feed amount 0 to the feed adjustor 57, and thus the required backward feed is obtained. The above mentioned ε 1 and ε 2 may be made equal on design, and therefore super stitching may be performed which is equal in the forward and the backward feed.
When the knob 3 is rotated from the condition in FIGS. 9 and 10 to the plus (+) direction, the feed control cam 47 is, as shown in FIG. 11, rotated in the clockwise direction via the shaft 44. Since the feed adjusting arm 49 is rotated around the pin 6d and the pin 49d moves within the oblong groove 51a of the feed arm 51, and if the follower 17a follows the concave portion of the cam 12 as seen in FIG. 11, the pin 51c is increased in the obliquity by α 1 with respect to the condition in FIG. 9, and said forward feed is enlarged. When the follower 17a follows the convex portion of the cam 12, FIG. 12 the obliquity is increased by α 2 and said backward feed is enlarged. The above mentioned α 1 and α 2 may be made equal on design, and therefore the feed amount of the forward and backward are equal.
For forming the stretch stitch on the honey pattern as an example of the super stitch, the invention can solve the conventional disadvantage that the forward and backward feed cannot be satisfactorily provided in case of the thick fabric. When the knob 3 is rotated to the minus (-) direction, the amounts of the forward and backward feeds may be equally reduced as mentioned above.
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In a sewing machine which has both functions, such as ordinary pattern stitching, such as zigzag stitching, and a super pattern stitching to which forward and backward feeds are automatically given, an arrangement is provided which adjusts by a single member the amount of feed at selecting an ordinary pattern stitching and a super pattern stitching. The arrangement provides that the feed amount specified to a pattern, which is given from a feed cam fixed on an operating shaft of a pattern selecting dial, is increased or decreased within a determined range by operating a feed adjusting knob outside of a machine frame. For selecting the super pattern, the amount of the forward and backward feed given by an automatic feed cam is enlarged or reduced back or forth the stitching within a determined range by operating the same feed adjusting knob.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to plasma display devices generally and, more particularly, but not by way of limitation, to a novel plasma display panel which is very economically manufactured and which has increased luminous efficiency and color purity.
2. Background Art
There is a great deal of interest in plasma display panels because such display devices consume far less space in the direction normal to the plane of the picture as compared to conventional cathode ray tubes. While the use of cathode ray tubes as display devices is quite widespread, they suffer from a number of other defects or undesirable features. Cathode ray tubes have a poor small area contrast ratio due to light scattering and a further phenomenon called "halo." When an electron beam impinges on a phosphor surface, that surface radiates light forwardly toward an observer, but light is also radiated inwardly, reflected and radiated back outwardly to form a bright donut or halo spaced around the central spot. This effectively enlarges the visible spot with consequent loss of perceived detail. Present day plasmas display technologies have somewhat similar problems which reduce resolution.
The basic theory of operation of alternating current plasma displays may be found in a number of sources such as U.S. Pat. Nos. 3,559,190; 3,935,494; and 4,233,623, as well as in an article by T. N. Criscimagna and P. Pleshko titled AC PLASMA DISPLAY found in Applied Physics, Vol. 40, published by Springer Verlag in 1980, the disclosures of which patents and article are incorporated by reference hereinto.
Briefly, such display devices have a plurality of gas discharge cells arranged in a generally flat matrix, and first and second sets of spaced apart electrodes with each cell located intermediate one electrode of the first set and one electrode of the second set. The display panel is formed with a first generally flat dielectric plate having the first set of electrodes therein, a second generally flat dielectric having the second set of electrodes therein, and with the two plates sealed together about their common periphery to enclose a gas such as a neon-argon mixture. Light emission is caused either by stimulation of such a visibly luminous gas mixture or by stimulation of phosphors within the cell. Phosphors responsive to ultraviolet radiation created by a discharge in a cell through the enclosed gas are coated on the one of the two plates through which the display is viewed or the selected gas may be one such as a neon-xenon mixture which has significant radiation in the visible spectrum in which case the phosphors may be eliminated.
In such known display devices, a gas discharge in one cell may energize the phosphors associated with one or more adjacent cells, resulting in a larger than desired basic picture element and a resultant loss of color purity. Attempts have been made to eliminate this "cross-talk" between adjacent cells by providing an intermediate layer in the form of a perforated plate having individual holes corresponding to individual cells. This attempt creates problems in evacuating the display device and refilling it with the desired gas and further eliminates the desired phenomenon of "priming" wherein some intercellular photon or charged particle migration reduces the voltage necessary to fire or energize a cell. Further attempts to isolate cells and eliminate cross-talk while retaining the priming feature and allowing charging of the display device with the proper gas mixture have included a zigzag pattern of passageways between cells (U.S. Pat. No. 3,869,630), an orthogonal array of grooves or troughs (U.S. Pat. No. 3,953,756), and dielectric glass spacing bosses separating the cells (U.S. Pat. No. 4,827,186. None of these is entirely satisfactory and all are relatively expensive to manufacture.
Accordingly, it is a principal object of the present invention to provide a plasma display panel which is economical to manufacture.
It is a further object of the invention to provide such a plasma display panel which provides increased luminous efficiency and color purity.
Other objects of the present invention, as well as particular features, elements, and advantages thereof, will be elucidated in, or be apparent from, the following description and the accompanying drawing figures.
SUMMARY OF THE INVENTION
The present invention achieves the above objects, among others, by providing, in a preferred embodiment, a plasma display panel, comprising: two parallely spaced apart dielectric glass layers; a plurality of gas discharge cells formed between said dielectric glass layers, boundaries of said gas discharge cells being defined by phosphor materials, and said phosphor materials serving as barriers between said gas discharge cells; and means to cause gas discharge in said gas discharge cells.
BRIEF DESCRIPTION OF THE DRAWING
Understanding of the present invention and the various aspects thereof will be facilitated by reference to the accompanying drawing figures, submitted for purposes of illustration only and not intended to define the scope of the invention, on which:
FIG. 1 is an enlarged, schematic, end elevational view, in cross-section, of a plasma display panel constructed according to the present invention.
FIG. 2 is an enlarged, bottom plan view, looking up, of the front plate of the plasma display panel of FIG. 1.
FIG. 3 is an enlarged, top plan view of the back plate of the plasma display panel of FIG. 1.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Reference should now be made to the drawing figures, on which similar or identical elements are given consistent identifying numerals throughout the various figures thereof, and on which parenthetical references to figure numbers direct the reader to the view(s) on which the element(s) being described is (are) best seen, although the element(s) may be seen also on other views.
FIG. 1 illustrates a plasma display panel, generally indicated by the reference numeral 10, constructed according to the present invention. Panel 10 includes a front panel, generally indicated by the reference numeral 12 and a rear panel, generally indicated by the reference numeral 14.
With reference also to FIG. 2, front plate 12 includes a substrate glass layer 20 (FIG. 1) having on the lower surface thereof a thin dielectric glass layer 22. Disposed between substrate layer 20 and dielectric layer 22 are a plurality of spaced apart, parallel electrodes 24 (FIG. 2) running right and left on FIG. 2. Disposed on the lower surface of dielectric layer 22 are spaced apart areas of a red phosphor material 30, a green phosphor material 32, and a blue phosphor material 34, the areas being disposed between and adjacent electrodes 24.
With reference to FIGS. 1 and 3, back plate 14 includes a substrate glass layer 40 (FIG. 1) having on the upper surface thereof a thin dielectric glass layer 42. Disposed between substrate layer 40 and dielectric layer 42 are a plurality of spaced apart, parallel electrodes 44 (FIG. 3) running up and down on FIG. 3, orthogonal to electrodes 24 (FIG. 2). Disposed on the upper surface of dielectric layer 42 are spaced apart pairs of stripes of a red phosphor material 50, a green phosphor material 52, and a blue phosphor material 54, the stripes being disposed such that each member of a pair is adjacent one of electrodes 44.
Front plate 12 is placed over back plate 14 so that the respective spaces between phosphor materials form a plurality of cells, schematically indicated by the vertical broken lines on FIG. 1. For example, a gas discharge cell 70 is formed between dielectric plates 22 and 42 bounded by those plates and red phosphor materials 30 and 50, the phosphor materials forming barriers around the cell. Likewise, a gas discharge cell 72 is formed between dielectric plates 22 and 42 bounded by those plates and green phosphor materials 32 and 52 and a gas discharge cell 74 is formed between the dielectric plates and blue phosphor materials 34 and 54.
While the use of red, green, and blue phosphors is described as a means of attaining full color displays, this invention also contemplates the use of single (same) color phosphors to attain monochrome displays of any single desired color.
With phosphor on both dielectric layers 22 and 42, maximum conversion of ultraviolet light to visible light can be achieved because phosphor is adjacent to the cold cathode discharge on both ends of the cells, simultaneously increasing luminous efficiency and color purity. Rounded shapes, as at 80, on FIG. 1 indicate the visible glow of light following an ultraviolet light discharge.
The deposition of phosphor materials can be placed through the use of self-registering photolithographic techniques, which is simpler and less costly than forming conventional barriers and which produces higher substrate mechanical tolerances.
It will be understood that the vertical spacing of phosphor elements on FIG. 1 is greatly exaggerated compared to the thicknesses of the other elements and such spacing will normally be on the order of about 0.004-0.005 inch.
It will thus be seen that the objects set forth above, among those elucidated in, or made apparent from, the preceding description, are efficiently attained and, since certain changes may be made in the above construction without departing from the scope of the invention, it is intended that all matter contained in the above description or shown on the accompanying drawing figures shall be interpreted as illustrative only and not in a limiting sense.
It is also to be understood that the following claims are intended to cover all of the generic and specific features of the invention herein described and all statements of the scope of the invention which, as a matter of language, might be said to fall therebetween.
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In a preferred embodiment, a plasma display panel, including: two parallely spaced apart dielectric glass layers; a plurality of gas discharge cells formed between the dielectric glass layers, boundaries of the gas discharge cells being defined by phosphor materials, and the phosphor materials serving as barriers between the gas discharge cells; and apparatus to cause gas discharge in the gas discharge cells.
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FIELD OF THE INVENTION
This invention deals with substantially fluorinated but not perfluorinated ionomers, and related ionic and nonionic monomers, having pendant groups containing fluorosulfonyl methide or fluorosulfonyl imide derivatives and univalent metal salts thereof, and with the uses of said ionomers in electrochemical applications such as batteries, fuel cells, electrolysis cells, ion exchange membranes, sensors, electrochromic windows, electrochemical capacitors, and modified electrodes. Certain compositions of the invention are also useful as strong acid catalysts.
BACKGROUND OF THE INVENTION
Copolymers of vinylidene fluoride (VF2) with vinyl alkoxy sulfonyl halides are known in the art.
The disclosures in Ezzell et al. (U.S. Pat. No. 4,940,525) encompass copolymers of VF2 with vinyl ethoxy sulfonyl fluorides containing one ether linkage. Disclosed is a process for emulsion polymerization of tetrafluoroethylene (TFE) with the vinyl ethoxy comonomer.
Connolly et al. (U.S. Pat. No. 3,282,875) disclose the terpolymer of VF2 with perfluorosulfonyl fluoride ethoxy propyl vinyl ether (PSEPVE) and hexafluoropropylene (HFP). They broadly teach an emulsion polymerization process said to be applicable to copolymerization of vinyl ethers with any ethylenically unsaturated comonomer, with greatest applicability to fluorinated monomers.
DesMarteau (U.S. Pat. No. 5,463,005), incorporated herein by reference, discloses substituted perfluoro-olefins of the formula
where X═C or N, Z═H, K, Na, or Group I or II metal, R=one or more fluorocarbon groups including fluorocarbon ethers and/or sulfonyl groups and/or perfluoro non-oxy acid groups, Y=perfluoroalkyl or F, and m=0 or 1. Further disclosed by DesMarteau are copolymers formed by aqueous emulsion polymerization of the sodium salt form of (I) with tetrafluoroethylene. Further disclosed are compositions consisting of the acid-form of the imide copolymer of DesMarteau in combination with dimethylformamide (hereinafter DMF) to provide a conductive composition. Membranes or films of the acid imide polymer are cast from solution. Copolymers of the substituted perfluoroolefins with VF2 are not disclosed in U.S. Pat. No. 5,463,005.
Armand (U.S. Pat. No. 4,818,644) discloses metal salts based on anions having the structure R f —SO 2 CR—SO 2 R′ f where R f and R′ f are perfluorinated groups having from 1 to 10 carbon atoms and R is a hydrogen or an alkyl group having from 1 to 30 carbon atoms. The lithium salts of these compounds are useful in combination with organic solvents or macromolecular solvents for making electrolyte solutions for lithium batteries. Armand et al. further disclose (EP 0 850 921) salts and ionomeric polymers derived from malononitrile Z—C(CN)2 where Z represents an electron-withdrawing group and Z can also contain a polymerizable function. Ionomers based on these compounds are disclosed having styrenic or vinyl functional groups for polymerization. Copolymers of these monomers with substantially fluorinated monomers such as VF2 are not disclosed.
Xue, Ph.D. thesis, Clemson University, 1996, discloses reactions of the type RSO 2 NHX with R′SO 2 Y with X═H, Na and Y═Cl, F to form RSO 2 N(M)SO 2 R′, where R and R′ are perfluorinated groups, in the presence of MF with M═Cs, K or in the presence of Na 2 CO 3 if X═Na and Y═Cl to form monomers represented by the formula
CF 2 ═CF—OCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 NMSO 2 R f
and copolymers thereof with tetrafluoroethylene.
Armand et al, EP0850921A1 and EP0850920A1, provide a tremendous list of imide- and methide-containing ionic species, including polymers incorporating them. However, no means for making these compositions is provided, and no distinction is made among the compounds from the standpoint of utility. No disclosure is made of the particular utility and surprising attributes of the compositions of the present invention.
SUMMARY OF THE INVENTION
The present invention provides for an ionic polymer (ionomer) comprising monomer units of VF2 and further comprising 0.5-50 mol-% of monomer units having pendant groups comprising the radical represented by the formula
—(OCF 2 CFR) a OCF 2 (CFR′) b SO 2 X − (M + )(Y)(Z) c (I)
wherein
R and R′ are independently selected from F, Cl or a perfluoroalkyl group having 1 to 10 carbon atoms optionally substituted by one or more ether oxygens;
a=0, 1 or 2;
b=0 to 6;
M + is H + or a univalent metal cation;
X is C or N with the proviso that c=1 when X is C and c=0 when X is N; when c=1, Y and Z are electron-withdrawing groups selected from the group consisting of CN, SO 2 R f , SO 2 R 3 , P(O)(OR 3 ) 2 , CO 2 R 3 , P(O)R 3 2 , C(O)R f C(O)R 3 , and cycloalkenyl groups formed therewith
wherein R f is a perfluoroalkyl group of 1-10 carbons optionally substituted with one or more ether oxygens;
R 3 is an alkyl group of 1-6 carbons optionally substituted with one or more ether oxygens, or an aryl group optionally further substituted;
Y and Z are the same or different;
or, when c=0, Y may be an electron-withdrawing group represented by the formula —SO 2 R f ′ where R f ′ is the radical represented by the formula —(R f ″SO 2 N − (M + )SO 2 ) m R f ′″ where m=0 or 1, and R f ″ is —C n F 2n — and R f ′″ is —C n F 2n+1 where n=1-10, optionally substituted with one or more ether oxygens.
The present invention further provides for an ethylenically unsaturated composition represented by the formula
CF 2 ═CF(OCF 2 CFR) a OCF 2 (CFR′) b SO 2 C − (M + )(Y)(Z) (II)
wherein
R and R′ are independently selected from F, Cl or a perfluoroalkyl group having 1 to 10 carbon atoms optionally substituted with one or more ether oxygens;
a=0, 1 or 2;
b=0 to 6;
M + is H + or a univalent metal cation;
Y and Z are electron-withdrawing groups selected from the group consisting of CN, SO 2 R 3 , P(O)(OR 3 ) 2 , CO 2 R 3 , P(O)R 3 2 , C(O)R f C(O)R 3 , and cycloalkenyl groups formed therewith wherein R f is a perfluoroalkyl group of 1-10 carbons optionally substituted with one or more ether oxygens;
R 3 is an alkyl group of 1-6 carbons optionally substituted with one or more ether oxygens, or an aryl group optionally further substituted;
Y and Z are the same or different.
The present invention further provides a method for making a methide ionomer the method comprising, combining in an inert organic liquid at a temperature in the range of 0-150° C. a copolymer comprising monomer units of VF2 and 0.5-50 mol-% of monomer units represented by the formula:
CF 2 ═CF(OCF 2 CFR) a OCF 2 (CFR′) b SO 2 F (III)
wherein R and R′ are independently selected from F, Cl or a perfluoroalkyl group having 1 to 10 carbon atoms optionally substituted with one or more ether oxygens, a=0, 1 or 2, and b=0 to 6; with a carbanion derived from a methylene compound represented by the formula CH 2 YZ wherein Y and Z are electron-withdrawing groups selected from the group consisting of CN, SO 2 R f , SO 2 R 3 , P(O)(OR 3 ) 2 , CO 2 R 3 , P(O)R 3 2 , C(O)R f C(O)R 3 , and cycloalkenyl groups formed therewith, wherein R f is a perfluoroalkyl group of 1-10 carbons, optionally substituted with one or more ether oxygens, R 3 is an alkyl group of 1-6 carbons, optionally substituted with one or more ether oxygens or an aryl group optionally further substituted; and wherein Y and Z may be either the same or different to form a reaction mixture; reacting said reaction mixture until the desired degree of conversion has been achieved; and, removing the majority of said organic liquid.
The present invention further provides a method for making a methide composition the method comprising, combining an inert organic solvent at a temperature in the range of 0-100° C. a composition represented by the formula
CF 2 A—CFA(OCF 2 CFR) a OCF 2 (CFR′) b SO 2 F (IV)
wherein A is Br or Cl, R and R′ are independently selected from F, Cl or a perfluoroalkyl group having 1 to 10 carbon atoms, a=0, 1 or 2, and b=0 to 6; with a carbanion derived from a methylene compound represented by the formula CH 2 YZ wherein Y and Z are electron-withdrawing groups selected from the group consisting of CN, SO 2 R f , SO 2 R 3 , P(O)(OR 3 ) 2 , CO 2 R 3 , P(O)R 3 2 , C(O)R f C(O)R 3 , and cycloalkenyl groups formed therewith, wherein R f is a perfluoroalkyl group of 1-10 carbons, optionally substituted with one or more ether oxygens, R 3 is an alkyl group of 1-6 carbons, optionally substituted with one or more ether oxygens or an aryl group optionally further substituted; and wherein Y and Z may be either the same or different to form a reaction mixture; reacting said mixture until the desired degree of conversion has been achieved; and, removing majority of said organic liquid.
The present invention further provides a process for forming an ionomer, the process comprising combining in an aqueous reaction medium VF2 with an ionic monomer represented by the formula
CF 2 ═CF—(OCF 2 CFR) a OCF 2 (CFR′) b SO 2 X − (M + )(Y)(Z) c (II)
wherein
R and R′ are independently selected from F, Cl or a perfluoroalkyl group having 1 to 10 carbon atoms optionally substituted with one or more ether oxygens;
a=0, 1 or 2;
b=0 to 6;
M + is H + or a univalent metal cation;
X is C or N with the proviso that c=1 when X is C and c=0 when X is N;
when c=1, Y and Z are electron-withdrawing groups selected from the group consisting of CN, SO 2 R f , SO 2 R 3 , P(O)(OR 3 ) 2 , CO 2 R 3 , P(O)R 3 2 , C(O)R f C(O)R 3 , and cycloalkenyl groups formed therewith wherein R f is a perfluoroalkyl group of 1-10 carbons optionally substituted with one or more ether oxygens;
R 3 is methyl or ethyl;
Y and Z are the same or different;
or, when c=0, Y may be an electron-withdrawing group represented by the formula —SO 2 R f ′ where R f ′ is the radical represented by the formula —(R f ″SO 2 N − (M + )SO 2 ) m R f ′″ where m=0 or 1, and R f ″ is —C n F 2n n— and R f ′″ is C n F 2n+1 where n=1-10, optionally substituted by one or more ether oxygens to form a reaction mixture;
introducing a free radical initiator;
reacting said reaction mixture to form an ionomer having a melting point of 150° C. or greater.
The present invention further provides for an ionically conductive composition comprising the polymer of the invention and a liquid imibibed therewithin.
The present invention further provides for an electrode comprising at least one electrode active material, the ionomeric polymer of the present invention mixed therewith, and a liquid imbibed therewithin.
The present invention further comprises an electrochemical cell comprising a positive electrode, a negative electrode, a separator disposed between the positive and negative electrodes, and a means for connecting the cell to an outside load or source wherein at least one of the group consisting of the separator, the cathode, and the anode, comprises the ionically conductive composition of the invention.
DETAILED DESCRIPTION OF THE INVENTION
For the purposes of the present invention, the term sulfonyl methide refers to a functional group wherein an ionically bonded carbon atom is also bonded to at least one fluoroalkylsulfonyl group, while the term sulfonyl imide refers to a functional group wherein an ionically bonded nitrogen atom is also bonded to at least one fluoroalkylsulfonyl group.
Surprisingly, the conductive compositions of the present invention are readily melt processible into electrodes and separators useful in assembling batteries in low cost continuous or semi-continuous manufacturing processes. No previous ionomer based composition suitable for use in electrochemical cells is known to exhibit melt processibility.
The ionomers of the present invention comprise monomer units derived from VF2 and 0.5-50 mol-%, preferably 2-20 mol-%, most preferably 3-12 mol-%, of ionic monomer units having pendant groups comprising the radical represented by the formula
—(OCF 2 CFR) a OCF 2 (CFR′) b SO 2 X − (M + )(Y)(Z) c
wherein
R and R′ are independently selected from F, Cl or a perfluoroalkyl group having 1 to 10 carbon atoms optionally substitued by one or more ether oxygens;
a=0, 1 or 2;
b=0 to 6;
M + is H + or a univalent metal cation;
X is C or N with the proviso that c=1 when X is C and c=0 when X is N;
when c=1, Y and Z are electron-withdrawing groups selected from the group consisting of CN, SO 2 R f , SO 2 R 3 , P(O)(OR 3 ) 2 , CO 2 R 3 , P(O)R 3 2 , C(O)R f C(O)R 3 , and cycloalkenyl groups formed therewith wherein R f is a perfluoroalkyl group of 1-10 carbons optionally substituted with one or more ether oxygens;
R 3 is an alkyl group of 1-6 carbons optionally substituted with one or more ether oxygens, or an aryl group optionally further substituted;
Y and Z are the same or different;
or, when c=0, Y may be an electron-withdrawing group represented by the formula —SO 2 R f ′ where R f ′ is the radical represented by the formula —(R f ″SO 2 N − (M + )SO 2 ) m R f ′″ where m=0 or 1, and R f ″ is —C n F 2n — and R f ′″ is —C n F 2n+1 where n=1-10, optionally substituted by one or more ether oxygens.
Preferably, a=0 or 1, R═CF 3 , R′═F, b=1, and when X is C, Y and Z are CN or CO 2 R 3 where R 3 is C 2 H 5 , while when X is N, Y is preferably SO 2 R f where R f is CF 3 or C 2 F 5 and M + is H + or alkali metal cation. Most preferably M + is a lithium cation. Most preferably the ionomer of the invention exhibits a melting point of 150° C. or higher as determined by the peak of the endotherm as measured by differential scanning calorimetry (ASTMD4591).
The methide ionomers of the present invention may be formed by copolymerization of (II) with VF2 according to the teachings of Connolly, op.cit. Preferably, however, the methide ionomer is made by the process of the invention, wherein in a preparatory step is formed a copolymer of VF2 with the sulfonyl fluoride monomer (III).
The polymerization of (III) with VF2 may be conducted according to the teachings of Connolly et al, op. cit. Preferably, the polymerization is conducted with pre-emulsified liquid comonomer in a reaction mixture as taught hereinbelow. The ionomers formed from non-ionic polymer which has been polymerized in such fashion exhibit surprisingly high melting points of ca. 150° C. or higher as determined from the peak of the endotherm in differential scanning calorimetry (ASTM D4591) in view of their bulk comonomer contents.
In the process of making the methide ionomer, the non-ionic sulfonyl fluoride copolymer, however formed, is then contacted in an inert organic liquid at a temperature of 0-150° C., preferably 20-70° C., with a carbanion derived from CH 2 YZ, wherein Y and Z are electron-withdrawing groups selected from the group consisting of CN, SO 2 R f , SO 2 R 3 , P(O)(OR 3 ) 2 , CO 2 R 3 , P(O)R 3 2 , C(O)R f C(O)R 3 , and cycloalkenyl groups formed therewith wherein R f is a perfluoroalkyl group of 1-10 carbons optionally substituted with one or more ether oxygens;
R 3 is an alkyl group of 1-6 carbons optionally substituted with one or more ether oxygens, or an aryl group optionally further substituted;
Y and Z are the same or different.
Preferably Y and Z are CN or CO 2 R 3 where R 3 is C 2 H 5 , and the base used to generate reactive species from CH 2 YZ is preferably an alkali metal hydride, most preferably lithium hydride.
The combination is allowed to react until the sulfonyl fluoride is completely converted, which takes typically 15-20 hours in the preferred temperature range of 20-70° C.
Most preferably, CH 2 YZ as hereinabove described, is combined with the copolymer of VF2 and (III), and lithium hydride in the inert organic liquid in the ratio of one gram equivalent weight of CH 2 YZ and two gram equivalent weights of lithium hydride per gram equivalent weight of sulfonyl fluoride.
Suitable inert organic liquids include oxygen-containing solvents such as dialkyl ethers, dimethoxyethane, tetrahydrofuran, dioxane, sulfolane, dimethyl sulfoxide, n-methyl pyrrolidone, dimethyl formamide, and acetonitrile. The preferred solvent will also be readily removed upon completion of the reaction. Preferred is dimethoxyethane.
The metal fluoride coproduct formed in the methidization process of the invention may be removed, if desired, by extraction or a dialysis process using water.
It is found in the practice of the invention, that in the formation of ionomers, the liquid medium in which the ionic species is formed often forms highly stable solvates therewith, making it difficult to fully remove that liquid by ordinary means such as drying or distillation. The residual liquid is preferably removed by addition of another metal ion ligating agent such as an organic carbonate, sulfolane, alkylphosphate, or dimethoxyethane which replaces the residual liquid, typically at moderately elevated temperatures in an anhydrous fluid such as toluene.
A monomeric form of the methide moiety of the ionomer of the invention may be formed by starting with the unsaturated olefinic structure (III), followed by bromination as is known in the art in order to protect the double bond, reaction as hereinabove described for the analogous copolymer, followed by treatment with Zn powder to yield the polymerizable double bond.
To form the imide ionomer of the present invention, VF2 is copolymerized with the monomeric composition represented by
CF 2 ═CF(OCF 2 CFR) a OCF 2 (CFR′) b SO 2 N(M + )SO 2 R f ′ (V)
R and R′ are independently selected from F, Cl or a perfluoroalkyl group having 1 to 10 carbon atoms optionally substituted by one or more ether oxygens;
a=0, 1 or 2;
b=0 to 6;
M + is H + or a univalent metal cation, R f ′ is the radical represented by the formula —(R f ″SO 2 N—(M + )SO 2 ) m R f ′″ where m=0 or 1, and R f ″ is —C n F 2n — and R f ′″ is —C n F 2n+1 where n=1-10, optionally substituted by one or more ether oxygens.
Preferably, a=0 or 1, R═CF 3 , R′═F, b=1, and when X is R f is CF 3 or C 2 F 5 , and M + is an alkali metal cation, most preferably lithium cation.
The olefinic monomer (V) may be synthesized according to the teachings of Xue, op.cit. The polymerization may be effected according to the teachings of Connolly et al, op. cit.
It is found in the practice of the present invention that the method by which the ionomer is formed can have a large effect on the melting temperature of the ionomer formed thereby. Melting point is of importance because a higher melting ionomer will provide a higher use temperature in such applications as lithium batteries.
The prior art teaches an aqueous emulsion process for copolymerizing methide or imide monomers according to DesMarteau or Xue, op. cit, with tetrafluoroethylene (TFE). Reaction kinetics dictate that the process of DesMarteau necessarily will result in limited, nearly random incorporation of the imide or methide monomers. An alternative though less convenient process known in the art, is to polymerize in a perfluorinated solvent.
Because of very substantial differences in reaction kinetics, the rate of incorporation and distribution of a comonomer in copolymerization with VF2 depends upon the availability of the comonomer in the aqueous polymerization medium. It has been found very surprisingly than when the methide and imide ionomers herein are copolymerized with VF2 in the aqueous emulsion polymerization of the art such as in Connolly et al, op. cit., ionically rich and ionically poor regions are developed. This results in an ionomer exhibiting a melting temperature higher than that achieved when an ionomer of the same over-all composition is formed by first copolymerizing VF2 with (III) using the same process followed by forming the ionomer.
An alternative means for providing the desired higher melting ionomer while avoiding the pitfalls of unwanted side reactions associated with polymerizing the ionic species, is to copolymerize VF2 with (III) in an aqueous medium wherein the liquid-liquid interface is substantially increased over that in the method of Connolly such as that in which the water, surfactant and monomer are pre-emulsified under very high shear mixing conditions as hereinbelow described.
Alternative means for achieving the high melting ionomers of the invention are available by copolymerizing VF2 with (III) in perfluorinated solvents, but this is less preferred because of the expense and handling difficulties inherent therewith.
It is found in the practice of the invention that it is preferred to make the methide ionomer by polymerizing VF2 with (III) in a pre-emulsified state as hereinbelow described, followed by forming the methide as hereinabove described. However, the imide is preferably formed by first forming the imide monomer according to Xue, op. cit., followed by polymerizing in an aqueous medium along the lines of Connolly, op.cit. In both approaches, the preferred method results in the preferred ionomer having a melting point of 150° C. and above.
The imide analog of (II) may be synthesized by exposing a composition represented by the formula
CF 2 ═CF(OCF 2 CFR) a OCF 2 (CFR′) b SO 2 F (III)
made according to the teachings of Asahi Chemical Industry, GB 2051 831, 1980 (K. Kimoto, H. Miyauchi, J. Ohmura, M. Ebisawa et al.) to bromine or chlorine in an anhydrous inert atmosphere at a temperature of ca. 0° C. in order to protect the olefinic bond according to the teaching in U.S. Pat. No. 5,463,005 forming thereby a composition represented by (IV). After washing to remove excess halogen using for example NaHSO 3 , the thus brominated starting material is combined under dry conditions, preferably in an anhydrous, aprotic organic solvent, with anhydrous MF, where M is K or Cs, and a composition represented by the formula R f ′SO 2 NH 2 , where R f ′ is the radical represented by the formula —(R f ′SO 2 N—(M + )SO 2 ) m R f ′″ where m=0 or 1, or possibly >1, and R f ″ is C n F 2n and R f ′″ is represented by the formula C n F 2n+1 where n=1 to 10, R f SO 2 NH 2 being made according to the teachings of Meuβendoerffer and Niederprüm (Chemiker Zeitung, 96. Jahrgang (1972) No. 10, 583). Suitable solvents include acetonitrile, dioxane, and sulfolane.
Preferably R f ′ is C n F 2n+1 where n=1 to 4.
The mixture thus formed is heated to a temperature in the range of 50-150° C., preferably 70-90° C., and the reaction is allowed to proceed preferably until the R f ′SO 2 NH 2 has been consumed as determined by NMR. Upon termination of the reaction, the product, which remains in solution is separated by filtration. In order to regenerate the olefinic bond, the reaction product is then contacted with metallic zinc, preferably by slurrying Zn powder into the solution, at ambient temperature and then heated for several hours, as taught in U.S. Pat. No. 5,463,005, preferably followed by filtering and washing with an anhydrous, aprotic organic solvent such as acetonitrile. Thus formed is a composition represented by the formula:
CF 2 ═CF(OCF 2 CFR) a OCF 2 (CFR′) b SO 2 N(M)SO 2 R f ′ (V)
The lithiated imide form of structure (V) is then copolymerized with VF2 according to the teachings of Connolly et al. Unlike the methide embodiment, wherein it is preferred to first make a copolymer of VF2 and (II) followed by methidization, in the case of the imide it is highly preferred to first make the imidized monomer (V) followed by polymerization with VF2.
In many applications, the ionomer is preferably formed into a film or sheet. Films may be formed according to processes known in the art. In one embodiment, the ionomer is diluted with a solvent such as DMAC, the mixture cast onto a smooth surface such as a glass plate using a doctor knife or other device known in the art to assist in depositing films on a substrate, and the solvent evaporated. Preferably the ionomer of the invention is first combined with a plasticizer and then is formed into a film or sheet by a melt process. Most preferably, the melt process is an extrusion process.
The ionomers of the present invention, however formed, may exhibit a low level of ionic conductivity in the dry state, typically about 10 −7 S/cm at room temperature. The ionomer may be combined with a liquid to achieve higher levels of ionic conductivity. Depending upon the requirements of the application, the ionomer will be in the acid form or the metal salt form, the particular metal being determined by the application as well. The liquid employed therewith will likewise be dictated by the application. In general terms, it has been found in the practice of the invention that conductivity of the liquid-containing ionomer increases with increasing percent weight uptake, increasing dielectric constant, and increasing Lewis basicity of the liquid, while conductivity has been observed to decrease with increasing viscosity and increasing molecular size of the liquid employed. Thus, a highly basic solvent of low viscosity and small molecular size but low dielectric constant may provide superior conductivity in a given membrane than a larger, more viscous, less basic solvent of very high dielectric constant. Of course, other considerations may come into play as well. For example, the liquid may be electrochemically unstable in the intended use.
Conductive compositions may thus be formed by combining together the ionomers of the present invention with solvents using a variety of techniques known in the art such as imbibing a dry ionomer film in a mixture of solvents or exposure of a dry film to a solvent vapor under controlled conditions or combining the ionomer with the solvents in a melt state and extruding films of controlled composition. Preferred solvents include water, nonaqueous solvents such as linear and cyclic carbonates, alcohols, esters, lactones, ethers, sulfoxides, amides, sulfonamides, and sulfones, subject to the general considerations discussed above. The solvents combined with the ionomers of the present invention to form conductive compositions can optionally contain additional mobile salts which may be preferred for specific applications. Other solvents suitable for forming conductive compositions include ionic liquids such as 1-methyl-3-butyl-imidazolium trifluoromethane sulfonate.
A variety of chemical agents can be added to these conductive compositions for purposes of improving ionic conductivity through the influence of the chemical agent on the dissociation or mobility of the ions within the ionomeric polymer. Such chemical agents include but are not limited to cationic complexing agents such as crown ethers and aza ethers and anion complexing agents such as BR 3 compounds where R is aryl, fluoro-substituted alkyl or aryl.
The ionomers of the present invention provide several unexpected benefits over the ionomers of the art. It is known in the art that VF2 polymers and copolymers exhibit electrochemical stability which makes them structural materials of choice for use in lithium batteries. Compared to the ionomers in the art which contain fluorosulfonate salts, the ionomers of the present invention comprise fluorosulfonylmethide or imide salts which exhibit higher dissociation in organic solvents thereby providing conductive compositions formed therefrom with surprisingly high conductivity. The preferred conductive compositions of the present invention, comprising the lithium salt embodiments of the ionomers of the invention and aprotic organic solvents, most preferably organic carbonates and lactones, are particularly well-suited for use in lithium batteries.
In an additive effect thereto, it is found, surprisingly, that the ionomers of the present invention exhibit particularly high affinity and phase compatibility with organic solvents as compared to the ionomers of DesMarteau, op. cit., formed with TFE. The higher affinity of the ionomers of the invention to organic solvents on the one hand makes melt processing or casting of membranes a useful process for the production thereof; and, on the other hand, provides for higher uptake of the preferred organic carbonates in the preferred conductive compositions of the invention, leading to higher conductivities thereby.
It is found in the practice of the invention that certain compositions of an ionomer of the invention containing at least 50% VF2 more preferably at least 80% VF2 may become plasticized by the solvents imbibed within it, with concomitant decrease in mechanical strength of the membrane. In some applications, it may be desirable to enhance the properties of the solvent-swollen membrane. Means available for improving the mechanical properties include: 1) incorporation into the polymer by means known in the art, a non-ionic third monomer that is not solvent sensitive; 2) formation by known means of a polymer blend with a non-ionic polymer that is less solvent sensitive; 3) blending by known means of the ionomer of the invention with an inert filler; 4) blending different compositions of ionic copolymers.
In a preferred embodiment of this invention involves the use of compositionally heterogeneous —SO 2 F— containing copolymer as precursor for the ionomeric form. Combined attributes of increased conductivity and enhanced mechanical strength are thereby obtained.
Suitable third monomers which may be usefully incorporated in these ionomeric compositions include tetrafluoroethylene, chlorotrifluoroethylene, ethylene, hexafluoropropylene, trifluoroethylene, vinyl fluoride, vinyl chloride, vinylidene chloride, perfluoroalkylvinyl ethers of the formula CF 2 ═CFOR f where R f ═CF 3 , C 2 F 5 or C 3 F 7 . Preferred termonomers include tetrafluoroethylene, hexafluoropropylene, ethylene and the perfluoroalkylvinyl ethers. Termonomers are preferably present in the polymer at a concentration of up to 30 mol-%.
Polymers suitable for blending with ionomers of the invention include poly(tetrafluoroethylene) and copolymers thereof with hexafluoropropylene or perfluoroalkyl vinyl ethers, polyvinylidene fluoride homopolymer and a copolymer thereof with hexafluoropropylene, and polyethylene oxide. A preferred composition comprises 25 to 50 weight % PVF2 homopolymer blended with the VF2 ionomer of the present invention. These materials are blended together by means common in the art such as mixing in a common diluent such as DMAC or propylene carbonate and then casting a membrane.
Suitable inert fillers include SiO 2 , Al 2 O 3 , TiO 2 , or CaF 2 . High surface area particles less than 1.0 micron in diameter are desired, such as are available for the preferred grade of SiO 2 under the trade name Cab-o-sil® TS-530 silica. Loadings of up to 50 weight % filler are preferred.
The preferred electrode of the invention comprises a mixture of one or more electrode active materials in particulate form, the ionomer of the invention, at least one electron conductive additive, and at least one organic carbonate. Examples of useful anode active materials include, but are not limited to, carbon (graphitic, coke-type, mesocarbon microbeads, carbon fibers, polyacenes, and the like) and lithium-intercalated carbon, lithium metal nitrides such as Li 2.6 Co 0.4 N, lithium metal, and lithium alloys, such as alloys of lithium with aluminum, tin, magnesium, mercury, manganese, iron, antimony, cadmium, and zinc, alloy forming anode compounds with inert metallic frameworks such as tin-iron-carbon or tin-manganese-carbon ternary compounds, metal oxides or lithium metal oxides such as tin oxide, iron oxide, titanium oxide, tantalum oxide, niobium oxide, or tungsten oxide, and electronically anion or cation-doping conductive polymers such as polyaniline. Lithium intercalation anodes employing graphitic carbon such as MCMB 2528 from Osaka Gas Chemical Co. are preferred.
Useful cathode active materials include, but are not limited to, transition metal oxides such as spinel LiMn 2 O 4 , layered LiMnO 2 , LiNiO 2 , LiCoO 2 , LiNi x Co y O 2 , iron oxides or lithiated iron oxides such as LiFeO 2 , or vanadium oxides such as LiV 2 O 5 , LiV 6 O 13 , LiNiVO 4 , LiCoVO 4 , or the above compounds in nonstoichiometric, disordered, amorphous, or overlithiated or underlithiated forms (such as having metallic vacancies, oxygen vacancies or defects, etc.), the above compounds doped with small amounts of other divalent or trivalent metallic cations such as Fe 2+ , Ti 2+ , Zn 2+ , Ni 2+ , Co 2+ , Cu 2+ , Cr 3+ , Fe 3+ , Al 3+ , Ni 3+ , Co 3+ , Mn 3+ , etc., sulfur compounds such as solid sulfur, organic disulfides, or metal sulfides such as TiS 2 or MoS 2 , electronically-conducting polymers such as polyaniline and its derivatives, polypyrrole derivatives, polyparaphenylene derivatives, polythiophene derivatives, or their copolymers, or mixtures of any of the above compounds. Particle size of the active material should range from about 1 to 100 microns. Preferred are transition metal oxides such as LiMn 2 O 4 , LiNiO 2 , LiCoO 2 , and LiNi x Co y O 2 . A highly preferred electron conductive aid is carbon black, preferably Super P carbon black, available from the MMM S.A. Carbon, Brussels, Belgium, in the concentration range of 1-10%. Preferably, the volume fraction of the lithium ionomer in the finished electrode is between 4 and 40%.
The electrode of the invention may conveniently be made by dispersion or dissolution of all polymeric components into a common solvent and mixing together with the electrode active particles the carbon black particles. For cathodes the preferred electrode active material is LiNi x Co 1−x O 2 wherein 0<x<1, while for anodes the preferred electrode active material is graphitized mesocarbon microbeads. For example, a preferred lithium battery electrode of the invention can be fabricated by dispersing or dissolving ionomer of the invention in a mixture of propylene carbonate and cyclopentanone, followed by addition of particles of electrode active material and carbon black, followed by deposition of a film on a substrate and drying. Preferably, the components of the electrode are mixed together and fed to an extruder wherein they are mixed to form a homogeneous melt and extruded into a film.
The resultant preferred electrode will comprise electrode active material, conductive carbon black, and ionomer of the invention, where, preferably, the weight ratio of ionomer to electrode active material is between 0.05 and 0.8 and the weight ratio of carbon black to electrode active material is between 0.01 and 0.2. Most preferably the weight ratio of ionomer to electrode active material is between 0.1 and 0.25 and the weight ratio of carbon black to electrode active material is between 0.02 and 0.1. This electrode can then be cast from solution onto a suitable support such as a glass plate, inert polymer carrier web, or current collector metal foil, and formed into a film using techniques well-known in the art. The electrode film thus produced can then be incorporated into a multi-layer electrochemical cell structure by lamination.
Battery solvents may be added to the battery component films individually or added to the battery laminated cells using a variety of techniques known in the art such as imbibing by immersion into a solution or exposure to solvent vapors under controlled conditions. Preferred battery solvents for forming conductive compositions with the ionomeric polymers of the present invention suitable for usage in lithium batteries include dipolar aprotic liquids such as the linear and cyclic carbonates, esters, lactones, amides, sulfoxides, sulfones, sulfamides, and ethers. Preferred solvents are mixtures of cyclic carbonates or lactones such as ethylene carbonate, propylene carbonate, butylene carbonates, vinylene carbonate, gamma-butyrolactone, fluoro or chloro-substituted cyclic carbonates with linear carbonates such as dimethyl carbonate, diethyl carbonate, dipropyl carbonate, ethyl methyl carbonate, methyl propyl carbonate, and fluoro and chloro substituted linear carbonates. Especially preferred are mixtures of ethylene carbonate, propylene carbonate, and gamma-butyrolactone with linear carbonates such as diethyl carbonate and/or ethyl methyl carbonate. Most preferred are mixtures of ethylene carbonate with propylene carbonate in weight ratios of from 50:50 to 80:20 of ethylene carbonate to propylene carbonate.
These solvents can optionally be combined with additional mobile salts such as the lithium salts LiPF 6 , LiPF x Rf y where Rf=CF 3 , CF 2 CF 3 , or other perfluorinated electron-withdrawing groups, LiBF 4 , LiAsF 6 , LiClO 4 , LiSO 3 Rf where Rf=CF 3 , CF 2 CF 3 , or other perfluorinated electron-withdrawing groups, LiN(SO 2 R1)(SO 2 R2) where R1 and R2=CF 3 , CF 2 CF 3 , or other electron-withdrawing groups and R1 is not necessarily the same as R2, LiC(SO 2 R3)(SO 2 R4)(SO 2 R5) where R3, R4, and R5=CF 3 , CF 2 CF 3 , or other electron-withdrawing groups and R3, R4 and R5 are not necessarily the same and mixtures of the above salts. Preferred are LiPF 6 or LiN(SO 2 CF 2 CF 3 ) 2 .
In a preferred embodiment of the battery of the present invention, a battery is formed from one or more electrochemical cells formed by laminating together in film form the anode, cathode, and separator compositions of the present invention, all of which have been rigorously dried prior to addition of a liquid selected from the group of organic carbonates and mixtures thereof, a mixture of ethylene carbonate and propylene carbonate being most preferred.
In a more preferred embodiment of the battery of the present invention, the individual film layers consisting of an anode, separator, and cathode are compounded individually in a melt state and extruded into film form using temperatures from 90 to 130° C. These individual layers already containing the preferred battery solvents such as mixtures of ethylene carbonate and propylene carbonate are laminated together to form battery cells which do not require additional post-treatment such as drying or extraction steps.
It may be desirable to incorporate into the electrode composition of the invention additional polymers or solvents for such purposes as improving the binding of the components thereof, or providing improved structural integrity of an article fabricated therefrom. One particularly preferred additional material is PVF2 homopolymer, which may be incorporated simply by dissolving the polymer into the same solution from which the electrode is being formed or melt compounding the polymer into other components during mixing or extrusion, as hereinabove described.
EXAMPLES
Example 1
The sulfonimide CF 2 ═CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 NHSO 2 CF 3 is prepared as described by DesMarteau (U.S. Pat. No. 5,463,005 (1995) and Xue (Ph.D. thesis (1996), Clemson University, Clemson), and is converted to its lithium salt by stirring in aqueous solution with 1 equivalent of lithum hydroxide at room temperature. After evaporating the water, the dried lithium salt (29.1 g, 0.05 mole) in 500 ml of deionized water is charged to a 1-liter vertical stirred autoclave. The vessel is closed, twice pressured to 100 psi nitrogen and vented, cooled to about 5° C. and evacuated. Vinylidene fluoride (50.0 g, 0.78 mol) is added, and the stirred (750 rpm) contents are heated to 60° C. A solution of potassium persulfate (0.08 g in 20 mL water) is added over a 10 minute interval. After about 8 hours, the remaining pressure is vented and the aqueous solution is evaporated to dryness giving a copolymer containing CH 2 CF 2 and CF 2 CF(OCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 NLiSO 2 CF 3 ) units as a white solid identified by its fluorine NMR spectrum.
Example 2
The sulfonyl fluoride CF 2 ClCFClOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 F, prepared as described by DesMarteau, U.S. Pat. No. 5,463,005 (1995) is converted to the lithium methide salt CF 2 ClCFClOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 C(Li)(SO 2 CF 3 ) 2 by the procedure described by Waddell et al. in Example 4 of U.S. Pat. No. 5,514,493 (1996). Treatment of this compound with zinc dust in acetic anhydride at 80-90° C. affords the olefinic methide monomer CF 2 ═CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 C(Li)(SO 2 CF 3 ) 2 . This monomer (35.6 g, 0.05 mole) in 500 ml of deionized water is charged to a 1-liter vertical stirred autoclave. The vessel is closed, twice pressured to 100 psi nitrogen and vented, cooled to about 5° C. and evacuated. Vinylidene fluoride (50.0 g, 0.78 mol) is added, and the stirred (750 rpm) contents are heated to 60° C. A solution of potassium persulfate (0.08 g in 20 mL water) is added over a 10 minute interval. After about 8 hours, the remaining pressure is vented and the aqueous solution is evaporated to dryness giving a copolymer containing CH 2 CF 2 and CF 2 CF(OCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 C(Li)(SO 2 CF 3 ) 2 ) units as a white solid identified by its fluorine NMR spectrum.
Example 3
A copolymer of VF2 and PSEPVE was synthesized according to the following method. 150 g of PSEPVE liquid was suspended in aqueous emulsion by combining with a solution of 35 g of ammonium perfluorooctanoate in 600 ml of distilled water using a Microfluidics, Inc. microfluidizer. The suspension was then diluted to 1 liter total volume with additional distilled water. The suspension so formed was charged to a nitrogen purged 4 liter horizontal autoclave equipped with a mechanical agitator, along with an additional 1500 mL of distilled water. The reactor was evacuated, then pressurized to 0 psig with vinylidene fluoride three times, then heated to 60° C., pressurized to 300 psig with vinylidene fluoride, and agitated at 200 rpm. A solution of aqueous potassium persulfate (0.6%, 50 mL) was added over a 5 min period. Reactor pressure was maintained at 300 psi until 220 g of VF2 had been fed after initiator addition. Agitation was stopped and the reactor was cooled and vented. The resulting milky dispersion was frozen and thawed to coagulate the product which was filtered through Nylon cloth and washed with water repeatedly to remove surfactant. After air drying, polymer crumb was dried in a nitrogen-purged vacuum oven at 100° C. for 24 hr to give 364 g of product. 19 F NMR data (acetone): +45.2 (s,), −78.0 to −80.0 (m's), −90.0 to −95 (m's), −108 to −116 (series of m), −122.0 to −127.5 (m's), −143.0 (bd s), consistent with mol % PSEPVE=9.5%. TGA (10°/min, N 2 ): no weight loss until 375° C. DSC (20°/min): maximum of broad melting transition at 162° C. (23 J/g); Tg=−20° C.
A 100 mL flask was charged with malonontrile (0.63 g, 9.5 mmol) and dimethoxyethane (10 mL). Sodium hydride (0.228 g, 9.5 mmol) was added in portions. The mixture was stirred at room temperature for ca. 15 min until gas evolution was complete. 5 g of the VF2/PSEPVE copolymer, corresponding to 4.73 mequiv. of SO2F, was suspended in dimethoxyethane (50 mL), treated in one portion with the above malononitrile anion solution. The mixture was stirred for 18 hr at which time 19 F NMR spectral analysis showed essentially complete conversion of SO2F groups to SO2C(CN)2 groups: −78.0 to −82.0 (m, distinctly different lineshape vs. SO3 form, a=7.00), −92.0 to −96.6 with major intensity singlet at −92.7, minor at −93.1 and −96.6 (combined a=16.868), −109 to −113 (m) and “defect” VF2 peaks at −115.0 and −117.3, CF2SO2−at −117.9 (combined a=5.206), −123 to −128 (bd m, a=1.543), −145.8 (m, a=1.011). Integration is consistent with 9.8 mol% Na-dicyanomethide form of functional comonomer. The reaction mixture was treated with dry toluene (50 mL) and filtered to provide 5.70 g red-pink solid after removal of residual solvent at high vacuum. 1 H NMR (acetone-d6) was in accord with one dimethoxyethane molecule/polymer-bound sodium ion.
Sodium ions were exchanged for lithium ions using the following procedure. A 4.0 g sample of the sodium form of the copolymer was suspended in 100 mL water containing 4.5 g LiCl and stirred for 1 hr. The aqueous layer was decanted, then replaced with another aqueous LiCl solution further modified by addition of methanol (40 mL). After 18 hr, the top phase was decanted and replaced with another aqueous charge of LiCl, and the mixture was stirred and filtered. The solid was washed with distilled water until chloride ion in the effluent could not be detected. The red solid was air dried, then azeotropically dried using toluene. Ethylene carbonate (0.44 g, 5 mmol; dissolved in toluene (5 mL) was added to the copolymer suspension in toluene, and distillation was continued until water was no longer evident in the distillate. The resulting solid was collected by filtration under nitrogen, then placed on a high vacuum line for 3 hr. to provide 4.0 g of solid. IR (thin film) exhibited band at 2205 cm−1 assigned to CN stretch.
1H NMR was consistent with one ethylene carbonate molecule/polymer-bound Li ion. ICP showed that exchange of Li for Na was essentially complete. DSC: peak melting temperature=160.6° (15.8 J/g).
Example 4
In the present example, a small molecule reaction is presented as an analog to the formation of a cyano-substituted methide ionomer. A mixture of dimethoxyethane (30 mL), nonafluorobutane sulfonyl fluoride (1.43 g, 4.75 mmol), and sodium hydride (0.228 g, 9.5 mmol) was treated slowly with a solution of malononitrile (0.314 g, 4.75 mmol) in dimethoxyethane (4 mL). Temperature increased to 35° C. with evolution of gas. The mixture was stirred for 18 hr., filtered through glass fiber paper, and evaporated to provide 1.63 g of yellow solid. Crude product was recrystallized by dissolution in a minimal volume of tetrahydrofuran and adding diethyl ether to form solid. Mixture was cooled at −25° and filtered to afford 0.59 g of solid. IR: intense bands at 2219 cm −1 and 2195 cm −1 assigned to CN stretching bands. 19 F NMR (THF-d8): −80.93 (m, a=27.3), −113.6 (m, a=17.6), −120.7 (m, a=18.8), −125.8 (m, a=18.7), consistent with CF 3 CF 2 CF 2 CF 2 SO 2 C(CN) 2 Na.
Example 5
In the present example, VF2/PSEPVE copolymer is converted to the lithium dicyanomethide derivative. A 300 mL flask was charged with VF2/PSEPVE copolymer (5.00 g, 4.73 mequiv. of SO 2 F) and dimethoxyethane (100 mL). Lithium hydride (0.075 g, 9.5 mequiv) was added and the mixture was stirred while malononitrile (0.313 g, 4.75 mmol) was added as a solution in dimethoxyethane (5 mL). 19 F NMR (DMSO-d6) spectrum was identical with that described in Example 3 and was consistent with complete conversion of SO 2 F groups.
Bulk sample was allowed to settle and the supernatant removed. Dry toluene (100 mL) was added and the solid was collected by filtration. Removal of residual solvent under high vacuum afforded 5.54 g of red solid. 1 H NMR (DMSO-d6): dimethoxyethane signals at 3.45 and 3.25, VF2 signal 3.15 to 2.7 and 2.4 to 2.18. DSC: peak melting temperature=163.3° C. (14.5 J/g).
Example 6
1.0 gram of the lithium-form polymer of Example 3 was mixed with 2.5 grams of propylene carbonate (PC, E.M. Industries, Selectipur) on a hot plate at 100° C. in a nitrogen-purged Vacuum Atmospheres glove box until a clear deep red gel resulted. This gel was melt pressed at 120° C. with 3 klbs pressure using a Carver Hydraulic Unit Model #3912 press inside the glove box to give a 4.0 mil thick clear pink film. A 1.0 by 1.5 cm 2 section of this film was cut with a razor and assembled into a four-point-probe conductivity cell. Ionic conductivity was determined according to the method of Doyle et al, WO98/20573. The conductivity of the film under ambient conditions was equal to 7.75×10 −4 S/cm.
A second sample of this membrane was immersed into an excess of a 1:1 by volume mixture of ethylene carbonate (EC, E.M. Industries, Selectipur) and gamma-butyrolactone (GBL, E.M. Industries, Selectipur) for 30 minutes at room temperature. At the end of this period, the membrane sample was removed and blotted dry and its weight and ionic conductivity were measured. The film was highly swollen but still strong and elastic when fully imbibed with solvent. Weight uptake of the film was 766% and the ionic conductivity was 1.67×10 −3 S/cm.
A third sample of this membrane was immersed into an excess of a 1.0 M solution of LiPF6 (E.M. Industries) in 1:1 by volume EC/GBL for 30 minutes. At the end of this period, the membrane sample was removed and blotted dry and its weight and ionic conductivity were measured. The film had gained little total weight as a result of the imbibing period and its conductivity was 3.14×10 −3 S/cm.
Examples 7-16
In these examples, the following reagents were employed. Acetonitrile, purchased from EM Science (Gibbstown, N.J.) was refluxed over P 2 O 5 for at least 12 h, collected under dry nitrogen; it was stored over activated 4 Å molecular sieves and used only in a dry box. Potassium fluoride was purchased from Aldrich Chemical Company; melted in a Pt dish with a torch and placed immediately in the chamber of the dry box; ground and stored thereafter inside the dry box. CF 3 SO 2 NH 2 , purchased from TCI America (Portland, Oreg.), was sublimed twice at 10 −3 Torr while using an oil bath temperature of 60° C. and a water cooled sublimation finger. Zn dust was purchased from Aldrich (<10 microns, 98+%) and activated with HCl according to standard procedures.
PSEPVE was synthesized according to the teachings of U.S. Pat. No. 5,463,005 (1995). It was distilled under vacuum. I(CF 2 ) 4 I, available from TCI, Portland, Oreg., was converted to NaSO 2 (CF 2 ) 4 SO 2 Na followed by the reaction with chlorine to obtain ClSO 2 (CF 2 ) 4 SO 2 Cl according to the teachings of Qiu and Burton (J. Fluorine Chem., 60 (1993) 93-100). C 4 F 9 I, available from TCI, was converted to, C 4 F 9 SO 2 Cl according to the teachings of Hu and DesMarteau (Inorg.Chem. 32 (1993) 5007.
Example 7
248.0 g (0.556 mol) of distilled PSEPVE were cooled to 0° C. with an ice bath. Under a nitrogen atmosphere, 30 ml (0.582 mol) Br 2 were added dropwise with an addition funnel over a period of 6 h. The orange color of excess bromine persisted for 30 min. The reaction mixture was washed with 100 ml of a 5% NaHSO3 solution. The product turned milky. After washing with 100 ml water twice, the clear product was dried with Na 2 SO 4 over night. The drying reagent was removed by filtration through a glass frit. The colorless, clear liquid was distilled at 40-45° C. at 10 −3 Torr. 1.5 g of P 2 O 5 were added and the compound underwent a second vacuum distillation at 40-45° C. at 10 −3 Torr. Yield was 312.1 g.
Inside a dry-box filled with nitrogen, 15.4 g (104 mmol) of CF 3 SO 2 NH 2 obtained from TCI, Inc.(Portland, Oreg.) were placed in a 500 ml round bottom flask. 200 ml of anhydrous acetonitrile were added followed by 29.6 g (509.7 mmol) of anhydrous KF. 69.43 g (114.6 mmol) of the dried brominated PSEPVE prepared as hereinabove described were added. The reaction mixture was stirred and slowly heated to moderate reflux for 40 h. The reaction mixture was filtered through a paper filter inside the dry box. All volatiles were removed and the white residue was dried at 1 15° C. for 12 h under vacuum to provide 70.9 g of product.
The material was dissolved in 100 ml anhydrous DMF. 7.05 g (108 mmol) of Zn-powder were added to the filtrate and the mixture was stirred for 1 h at room temperature. The mixture was filtered and the residue was washed with additional 25 ml of anhydrous DMF.
The flask was brought outside the dry-box and most of the volatiles were removed under vacuum. The residue was heated under vacuum for 16 h at 115° C. The material contained traces of DMF. 19 F-NMR in CD 3 CN showed the product was CF 2 ═CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 N(K)SO 2 CF 3 (8F, − 77.8 -−79.3 ppm; 2F, −83.7 ppm; 1F, −112.65 ppm; 2F, −116.0 ppm; 1F, −121.0 ppm; 1F, −135.7 ppm; 1F, −144.2 ppm)
Example 8
150 ml of HCl conc. and 150 ml of deionized water were added to the product of Example 7, forming a brown, oily mixture which was stirred for 5 min and then four times extracted with fresh 100 ml aliquots of diethyl ether. The diethyl ether fractions were combined and washed three times with fresh 100 ml aliquots of deionized water. The ether was evaporated under vacuum and the remaining brown oil was transferred to a 100 ml round bottom flask. The brown, crude material underwent two shortpath distillations to obtain 50.6 g of the acid product CF 2 ═CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 N(H)SO 2 CF 3 .
Example 9
34.08 g (59.26 mmol) of an acid product synthesized as in Example 8 was dissolved in 25 ml deionized water. 121.1 ml of a 0.489N LiOH solution was added. All water was removed under vacuum and the residue was dried at 100° C. for 24 h. Yield was 34.09 g of CF 2 ═CFOCF 2 CF (CF 3 )OCF 2 CF 2 SO 2 N(Li)SO 2 CF 3 19F-NMR in D 2 0: (8F, −77.8-−79.5 ppm; 2F, −86.0 ppm; 1F, −115.5 ppm; 2F, −117.3 ppm; 1F, −123.4 ppm; 1F, −137.7 ppm; 1F, −146.1 ppm); elemental analysis: N (2.45% found, 2.41% theor.), F (49.43% found, 52.31% theor.), Li (1.15% found, 1.19% theor.), S (10.83% found, 11.03% theor.).
Example 10
30.0 g (94.2 mmol) of C 4 F 9 SO 2 Cl were placed in a 250 ml round bottom flask. 125 ml of anhydrous acetonitrile and 55.1 g (948 mmol) of fused KF was added. The reaction mixture was stirred at room temperature for 42 h. All volatiles were removed and the residue was heated at 80° C. for 18h. 78.6 g (4.62 mol) anhydrous ammonia was added to the collected volatile fraction at −196° C. The reaction mixture was warmed to room temperature under an inert argon atmosphere allowing excess ammonia to evaporate overnight. All volatiles were removed under vacuum. The residue was heated to 45° C. for 5h under vacuum.
The residue was then treated with 150 ml anhydrous acetonitrile and filtered through a paper filter inside the dry-box, and solid was washed with an additional 100 ml of anhydrous acetonitrile. The solvent was removed under vacuum and the residue was sublimed (70° C., 10 −3 Torr) to yield 19.38 g.
Inside the dry box, 32.9 g (54.3 mmol) of bromine protected PSEPVE prepared as in Example 7 was dissolved in 250 ml of anhydrous acetonitrile, 14.8 g (49.5 mmol) of the C 4 F 9 SO 2 NH 2 prepared as hereinabove described were added, followed by the addition of 15.92 g (274 mmol) of fused KF. The reaction mixture was maintained at 80° C. for 96 h. The reaction mixture was cooled to room temperature and filtered. 5.45 g (83.3 mmol) Zn powder was added to the filtrate and the reaction mixture was stirred at room temperature for 45 min. The reaction mixture was heated to 60° C. for 15 h. The excess Zn and ZnBr 2 were removed by filtration and the solvent was removed under vacuum. The yellow residue was treated with 150 mL 6N HCl and the product was extracted with four portions of 150 ml ether. The combined organic layer was washed with 100 ml water, and the solvent was evaporated to yield, after shortpath distillation, 22.3 g of CF 2 ═CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 N(H)SO 2 C 4 F 9 , as confirmed by 19 F NMR.
Example 11
Inside a dry box, 200 ml of anhydrous acetonitrile was added to ClSO 2 (CF 2 ) 4 SO 2 Cl (23.1 g, 57.9 mmol) together with anhydrous KF (28.1 g, 484 mmol). The mixture was stirred at room temperature. Fluorine NMR showed that formation of the disulfonyl fluoride was complete after 17 h. The reaction flask, maintained under inert atmosphere, was equipped with a reflux and an addition funnel. The mixture was heated to 80° C. and treated with 5.81 g (100 mmol) of KF. 4.33 g (29.1 mmol) of CF 3 SO 2 NH 2 dissolved in 45 ml of anhydrous acetonitrile was added to the stirred suspension from the addition funnel over a period of 6.5 hours. The reaction mixture was stirred and heated for a total of 71 h. The reaction mixture was filtered, and the residue was washed with anhydrous acetonitrile. Combined filtrate was evaporated under vacuum and the beige residue was heated at 90° C. for 18 hr. Yield was 14.95 g of CF 3 SO 2 N(K)SO 2 (CF 2 ) 4 SO 2 F as confirmed by 19 F NMR in CD3CN: 44.9 ppm (SO2F, s, 1F), −80.6 ppm (CF3SO2, s, 3F), −108.2 ppm (CF2SO2, s, 2F), −114.2 ppm (CF2SO2, s, 2F), −120.7 ppm (CF2CF2SO2, s, 4F).
About 55 g of anhydrous ammonia were condensed to 14.95 g (28.1 mmol) of CF 3 SO 2 N(K)SO 2 (CF 2 ) 4 SO 2 F so prepared. The pressure in the flask was brought to 1 atm with argon and the reaction mixture was allowed to warm up to room temperature over a period of 5 h. The excess ammonia was allowed to escape. The beige residue was dried under vacuum and heated to 60° C. for 18 hr. Inside the dry-box, the product was dissolved in 150 ml of anhydrous acetonitrile and filtered. All volatiles were removed from the filtrate under vacuum to provide 12.7 g of product CF 3 SO 2 N(K)SO 2 (CF 2 ) 4 SO 2 NH 2 which was dried at 90° C. for 12 hours.
Inside a dry-box, 20.2 g (33.3 mmol) of bromine-protected PSEPVE prepared as in Example 7 were added together with 125 ml of anhydrous acetonitrile to 12.7 g (24.0 mmol) of CF 3 SO 2 N(K)SO 2 (CF 2 ) 4 SO 2 NH 2 prepared as hereinabove described. The reaction was started by the addition of 7.02 g (121 mmol) of fused KF. The reaction mixture was heated to 80° C. for 76 h. The reaction mixture was filtered through a paper filter to give the product CF 3 SO 2 N(K)SO 2 (CF 2 ) 4 SO 2 N(K)SO 2 CF 2 CF 2 OCF(CF 3 )CF 2 OCFBrCF 2 Br. The product can readily be debrominated as in Example 7.
Example 12
According to the method of Example 1, a 1 liter autoclave was charged with a solution of 12.8 g (22.0 mmol) of the ionic lithium composition of Example 9 in 400 g deionized water. The solution was cooled and degassed and the reactor was charged with 15 g (0.234 mol) of vinylidene fluoride. The solution was brought to 60° C. (pressure in reactor: 116.1 psig; rpm: 750) after which 20 ml of a solution of 0.201 g potassium persulfate in 50 g deionized water was added over a period of 10 min. The reactor pressure diminished to 0 psig after 16 h. The copolymer was isolated by lyophilization. Yield was 24.9 g of copolymer characterized by 10.8 mol-% PSEPVE imide content, as shown by 19 F NMR. DSC showed T m =163° C. (2 nd heat). Elemental analysis: H (1.96% found, 1.49% theor.), N (1.25% found, 1.26% theor.), F (51.04% found, 55.68% theor.), S (5.40% found, 5.78% theor.)
1 H NMR (acetone-d6): CH 2 at 3.85 ppm
19 F NMR (acetone-d6): −77.2-−79.2 ppm (m), −91.2—−130.0 ppm (series of m); −144.6 (1F, sidechain CF).
Example 13
0.865 g of the ionomer of Example 12 and 70 ml acetone was stirred for 12 h at room temperature and then poured into a 10 cm PFA dish. The solvent was allowed to evaporate slowly to provide a copolymer film which was peeled from the dish. The membrane was heated in a vacuum oven at 100° C. for 12 hours after which it became somewhat brittle. Film thickness was 120 micrometers.
Example 14
The procedure of Example 12 was followed, except the ionic comonomer used was 12.801 g of CF 2 ═CFOCF 2 CF(CF 3 )OCF 2 CF 2 SO 2 N(Li)SO 2 CF 3 (from Example 9) and the quantity of vinylidene fluoride was 29 g. The VF2-copolymer was isolated by lyophilization. The material was dried at 110° C. for 22 hr to afford the yield was 40.7 g of ionomer containing 4.7 mol-% of the lithium imide as confirmed by 19 F NMR. DSC ( 2 nd heat) showed T m −164.5° C. Elemental analysis: H (2.06% found, 2.16% theor.), N (1.78% found, 0.74% theor.), Li (0.32% found, 0.37% theor.). 1 H NMR (acetone-d6): CH2 at 3.60 ppm. 19 F NMR (acetone-d6): −77.2-−79.2 ppm (m), −91.2-−130.0 ppm (series of m), −144.6 (sidechain CF).
Example 15
1.122 g of the ionomer of Example 14 were dissolved in 70 ml acetone and heated to reflux for 12 h. After the solution was cooled to room temperature, it was poured into a PFA dish and the solvent was allowed to evaporate slowly. A clear film was easily peeled from the PFA dish and was dried in a vacuum oven at 100° C. for 12 h. Thickness was 190 micrometers.
Example 16
A 100 mL flask is charged with 4.73 mmol of the Bromine Protected PSEPVE of Example 7, dimethoxyethane (20 mL), and lithium hydride (0.075 g, 9.5 mequiv.) The mixture is cooled to ca. −20°, then stirred while malononitrile is added as a solution in dimethoxyethane. After 18 hr, the mixture is filtered and evaporated. Following the method of Example 7, Zn powder is added to the reaction mixture to regenerate the olefinic bond.
Example 17
0.50 grams of the ionomer of Example 14 were mixed in powder form at 120° C. using a spatula with 0.5 grams of an ionomer comprising monomer units of VF2 and 9.5 mol-% of the lithium sulfonate form of PSEPVE prepared as described in copending application Ser. No. 98/23244 and 2.0 grams of a 1:1 by volume mixture of ethylene carbonate and gamma-butyrolactone, both reagents Selectipur grade from EM Industries). The mixture so formed was heated under nitrogen in a sealed glass vial to 100° C. for several hours until a homogenous, clear mixture resulted.
This mixture was then cooled to form a gel. About 0.5 g of the gel was removed from the glass vial and placed between two sheets of Kapton® polymide film (DuPont) and the combination placed between the platens of a Carver Hydraulic Unit Model #3912 preheated to 105° C., and was pressed at 1000 lbs ram force. The film that resulted was clear and uniform and 4.2-4.7 mils in thickness.
Once cooled to room temperature, a 1.0 cm by 1.5 cm membrane sample from this hot pressed film was cut using a knife and then tested using the four-point-probe test described above. Solvent uptake was nominally 200% based on the as-prepared composition of the film. Conductivity was 8.27×10 −4 S/cm.
An 18 mm diameter circular specimen was punched from the melt pressed film to serve as a battery separator membrane as hereinbelow described.
To form a cathode, the following materials were weighed and hand-mixed in a 50-ml glass jar inside a glove box under a dry nitrogen atmosphere:
0.625 grams (2.5 wt %) of Kynar Flex ® 2801 polyvinylidene fluoride,
from Atochem.
1.75 grams (7.0 wt %) of the ionomer of Example 14
15.5 grams (62 wt %) of LiCoO 2 , from EM Industries.
1.625 grams (6.5 wt %) of Super P carbon black from MMM Carbon.
5.5 grams (22 wt %) of a 1:1 by volume mixture of ethylene carbonate
and gamma-butryolactone (GBL), both Selectipur Grade,
EM Industries
The mixture so formed was fed to the feed throat of a CSI-Max extruder, model CS-194. Extrusion conditions were as follows:
Rotor temperature:
110° C.
Header temperature:
110° C.
Gap between rotor and header:
0.13 cm
Rotor speed:
192 rpm.
The thus melt-compounded material was extruded through a circular die with a diameter of 0.32 cm, and was collected in a glass jar purged with dry nitrogen.
A 1.0 gram quantity of the extrudate was was melt-pressed between the platens of the Carver press at 110° C. and 20 klbs ram force inside a nitrogen-purged glove box, followed by cooling and release of pressure thereby forming a film of 5 mil thickness. A 12 mm diameter circular specimen was punched out of the film so formed.
The separator and cathode films prepared as hereinabove described were each exposed for 2 hours to an electrolyte solution composed of 1.0 M LiPF 6 in 1:1 EC/GBL by immersion in 2-4 ml of solution in a sealed glass vial for two hours.
The so-treated cathode and separator film were assembled into size 2325 coin cells with 3 layers of 4 mil thick lithium metal as the negative electrode. The coin cell was cycled at the C/5 rate for both charge and discharge at room temperature between the voltage limits of 4.2 V and 2.8 V. Capacity during the first charge for the LiCoO 2 cathode was 157.2 mAh/g, while capacity for the first discharge was 149.7 mAh/g, giving a reversibility of 95.2%. Capacity on the tenth discharge was 147.1 mAh/g and the coin cell achieved nearly 100 cycles to 80% of its initial capacity.
Example 18
The MicroFluidizer™ of Example 3 was charged with a solution of 5 g ammonium perfluoro octanoate in 75 ml demineralized water. The pump was started and the fluids allowed to recycle to mix the surfactant solution. PSEPVE (25 g) was added to the reservoir and the system allowed to recycle for 20 min to produce a well dispersed translucent blue PSEPVE emulsion. The outflow was then directed to a 200 ml volumetric flask. After the reservoir was pumped down, 100 ml demineralized water was added and pumped through the system to flush the remaining PSEPVE emulsion through and bring the level in the volumetric flask up to the mark. The final PSEPVE emulsion contained 0.25 g/ml PSEPVE and was translucent blue.
A 4-L horizontal stainless-steel stirred polymerization reactor was flushed with nitrogen and conditioned by charging with 2 liters demineralized water, 5 g ammonium persulfate, 5 g ammonium perfluorooctanoate, then agitating at 150 rpm while heating the vessel contents to 100° C./15 min. The vessel was cooled, the contents dumped to waste and the vessel rinsed 3 times with 2 liters demineralized water.
The reactor was charged with 1.75 liter demineralized water. 4 ml of the PSEPVE emulsion prepared above and 20 g of ammonium perfluorooctanoate were combined in an additional 100 ml of distilled water and added to the reactor. The reactor was sealed and three times pressured with nitrogen to 100 psig and vented. Three times the reactor was evacuated to −14 psig and flushed with vinylidene fluoride (VF2) to 0 psig. Agitation at 200 rpm was started and the reactor temperature was brought to 60° C. The reactor was pressurized with VF2 to 300 psig at which time 20 ml of 4.5% potassium persulfate solution was pumped in at 10 ml/min. The polymerization initiated in 0.03 hr. VF2 and the PSEPVE emulsion were fed as needed at a 99:1 mole ratio of VF2:PSEPVE to maintain 300 psig reactor pressure. The polymerization was continued for 3.2 hr, feeding a total of 251 g VF2/PSEPVE for an overall rate of 80 g/hr. The run was terminated to yield a milky-white latex containing 11.5% polymer solids. A total of 5 runs were made by repeating this process. The latex from these runs were combined and mixed by stirring to form a homogeneous blend.
The combined polymer latex was frozen in dry ice and defrosted. The agglomerated polymer was white and powdery. The polymer was washed vigorously 4 times in 5 gal of 50° C. tap water then washed a final time in 5 gal demineralized water (20° C.). The washed polymer was dried at 100° C. for 48 hr under nitrogen sparged partial vacuum to yield 1028 g of fine white polymer powder. 19 F NMR analysis (DMF d ) was consistent with 0.9 mole % PSEPVE in the copolymer. DSC analysis indicated a glass transition temperature centered at Tg=−38° C. and a melting endotherm at Tm=162° C.
A 4-neck, 5 L flask maintained under dry, inert atmosphere was charged with 400 g of the 0.9 mol % VF 2 /PSEPVE copolymer made above, 1.14g of lithium hydride, and 1600 ml of THF. The stirred mixture was cooled to ca. 5° C., and 100 ml of a THF solution containing 4.71 g of malononitrile was added dropwise over a ca. 20 min period. Temperature was maintained below 10° C. during addition. Mixture was allowed to warm to room temperature after addition was complete. After 20 hr, the mixture was cooled to 5°, treated with water (dropwise at first; then in portions so that total water added was 2500 mL during a 0.5 hr period).
The pH was adjusted to 7.1 by addition of dilute acetic acid. Another 750 mL water was added and the mixture was allowed to settle. Supernatant was removed using a siphon and product was washed with water. Product was filtered through a cloth filter membrane and washed with water to remove residual THF. The product was allowed to air-dry followed by drying under vacuum at 118° C. to provide 386.6 g of product.
19 F NMR (DMF-d7) showed: −76.5 to −80.0 (m, CF 3 and OCF 2 , a=7.00), −91 to −95.0 (m, with major signals at −91.5,−94.7, (CH 2 CF 2 , a=203.21), −109 to −117 (m, with major signals at −113.5 and −115.9 (VF2 reversals), a=22.66), −122 to −127 (m, a=1.92), −144 (m, CF, a=1.17), consistent with 0.9 mol % comonomer content corresponding to the lithium methide derivative of PSEPVE.
A 1:1 (weight ratio) of ethylene carbonate/propylene carbonate (EC/PC) solution was prepared by dissolving 100 g of ethylene carbonate (EM Industries, Selectipur® grade) in 100 g of propylene carbonate (EM Industries, Selectipur® grade) at room temperature inside a nitrogen gas dry box.
The following was performed in a nitrogen gas dry box at <1 ppm moisture level. 0.5 g of the 0.9 mole % PSVF2-methide copolymer powder prepared above, and 0.5 g of the EC/PC solution were mixed inside a small vial. A portion of the mixture was then placed between two Kapton® polyimide sheets to be calendered into a film using a heated laminator. The laminator was located inside the dry box. It consisted of two heated steel rolls each of 102 mm diameter. At the front of the nip of the heated rolls was a preheat zone. The mixture was held in the preheat zone at 130° C. for about 2 minutes. The copolymer mixture was then passed through the heated rolls at 125° C. and at a speed of about 0.1 m/min. A force of about 1680 N was applied on the steel rolls. Two brass shims of 0.102 mm thick was placed, one on each side of the copolymer mixture, and fed simultaneously with the copolymer into the nip of the steel rolls to limit the minimum gap between the steel rolls. A stand-alone film of 0.083 mm thickness was formed.
A rectangular test section of this film was cut. The conductivity of this sample was determined using the 4-point-probe conductivity method of Doyle et al, WO98/20573. The conductivity of the sample was 0.067 mS/cm.
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This invention concerns ionomers comprising monomer units of vinylidene fluoride and monomer units of perfluorovinyl ethers having pendant groups containing fluoroalkyl sulfonyl methide or fluoroalkyl sulfonyl imide derivatives and univalent metal salts thereof, and with the uses of said ionomers in eledrochemical applications, electrochemical capacitors and modified electrodes.
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CROSS-REFERENCE TO RELATED APPLICATION
This application is a continuation-in-part of U.S. patent application Ser. No. 08/988,256, filed Dec. 10, 1997 now U.S. Pat. No. 5,906,161.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the art of printing and ink roller assemblies.
2. Brief Description of the Prior Art
The following are made of record: U.S. Pat. No. 3,738,269 to W. T. Wagner; U.S. Pat. No. 3,783,083 to W. A. Jenkins; U.S. Pat. No. 3,812,782 to T. Funahashi; U.S. Pat. Nos. 3,957,562; 4,280,863 and 4,334,470 to P. H. Hamisch, Jr. et al; U.S. Pat. No. 4,246,842 to L. E. Willams et al; U.S. Pat. No. 4,399,751 to J. R. Kessler; U.S. Pat. No. 4,416,201 to J. R. Kessler; U.S. Pat. Nos. 4,452,141 and 4,478,145 to J. D. Mistyurik; U.S. Pat. Nos. 5,421,869, 5,516,362 and 5,774,160 to A. Gundjian et al; and U.S. Pat. No. 5,910,227 to J. D. Mistyurik et al.
SUMMARY OF THE INVENTION
It is a feature of the invention to provide an improved ink roller assembly capable of providing a uniform application of ink over an extended period of use.
It is a feature of the invention to provide an improved ink roller assembly which supplies ink in quantities according to the inking requirements for different printing members.
It is a feature of the invention to provide an improved ink roller assembly which holds ink in quantities according to the inking requirements for different printing members.
It is a feature of the invention to provide an improved ink roller assembly which meters ink to printing characters in accordance with or as a function of the surface areas of the printing characters.
It is a feature of the invention to provide an improved ink roller assembly which has capillary sections of different lengths.
In accordance with a specific embodiment of the invention, there is provided an ink roller assembly with a first section comprised of molded plastics material, wherein the first section has a first axial shaft and a series of first discs on the first shaft, and wherein the first discs are closely spaced to provide first capillary chambers. A first porous sleeve is in contact with and spans the outer peripheries of the first discs. There is a second section also comprised of molded plastics material. The second section also has a second axial shaft and a series of second discs on the second shaft. The second discs are closely spaced to provide capillary chambers. There is a second porous sleeve in contact with and which spans the outer peripheries of the second discs. The first and second sections are axially aligned and are connected to each other.
In accordance with another embodiment of the invention, there is a first section with capillary chambers and a porous sleeve and a second section connected to the first section which has a porous sleeve but no capillary chambers.
In another embodiment of the invention, the invention provides an ink roller assembly which can be rotatably mounted on an inker shaft of an inking device. The ink roller has first and second sections connected to each other by a connector. Each of the first and second sections has a flange, a hollow shaft and a series of closely spaced discs which provide capillary chambers for retaining ink. The first section further includes a flexible resilient spring finger for releasably holding the ink roller on the inker shaft. There are preferably passages through the discs which allow for some flow of ink between capillary chambers and pressure equalization. The hollow shafts of the first and second sections have aligned openings for a receiving the inker shaft. The inker shaft has an annular groove for receiving the spring finger. There is a separate flexible resilient porous sleeve of ink retaining material in contact with and spanning the outer peripheries of the discs of both the first and second hub sections.
In yet another embodiment of the invention, a capillary section includes a series of closely spaced discs which provide capillary chambers for retaining ink. Passages interconnect the chambers to provide for some flow of ink between chambers and pressure equalization. A flange is disposed between the discs and a stub end. A porous sleeve of ink-retaining material is in contact with the outer peripheries of the discs.
In all the embodiments, varying the peripheral configurations of the discs can enhance the distribution of ink to the outer surface of the sleeve of ink retaining material.
It is preferred to have different inks in each section of the ink roller. One ink in one section can be a visible ink which can be readily seen following printing without activation or excitation, while the other ink in the other section can be a visible ink activatable or excitable following printing for coding purposes. Alternatively one ink in one section can be of one color and the other ink in the other section can be of a different color. In the event an ink is used which is visible but becomes invisible following printing, such an ink is considered to be an invisible ink in the context of this disclosure.
According to a specific embodiment, there is provided an improved method of printing on a record member, which comprises providing a print head with first and second printing members, providing an ink roller with a first porous ink-receptive sleeve containing a visible first ink and a second porous ink-receptive sleeve containing a visually alterable second ink, rolling the ink roller across the first and second printing members to cause the first sleeve to ink the first printing member with the first ink and to cause the second sleeve to ink the second printing member with the second ink, and simultaneously printing with the inked first and second printing members to produce printing with both the first and second inks on a record member.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a rotated exploded perspective view of an ink roller assembly in accordance with one embodiment of the invention;
FIG. 2 is an assembled mainly sectional view of the ink roller assembly of FIG. 1 mounted on an inker shaft of an inking mechanism;
FIG. 3 is an enlarged fragmentary sectional view of a portion of the ink roller assembly shown in FIGS. 1 and 2;
FIG. 4 is a sectional view taken along line 4 — 4 of FIG. 2;
FIG. 5 is an exploded perspective view of an ink roller assembly in accordance with another embodiment of the invention;
FIG. 6 is a top plan view of the ink roller assembly of FIG. 5, but omitting the sleeve;
FIG. 7 is a partly broken away end elevational view taken along line 7 — 7 of FIG. 6;
FIG. 8 is a vertical sectional view of the ink roller assembly taken along line 8 — 8 of FIG. 6;
FIG. 9 is a fragmentary sectional view showing an alternative construction for the discs of the embodiments of FIGS. 1 through 8;
FIG. 10 is a sectional view taken along line 10 — 10 of FIG. 9;
FIG. 11 is a developed fragmentary view showing another manner in which the discs of the embodiments of FIGS. 1 through 8 can be constructed;
FIG. 12 is an assembled sectional fragmentary view of an alternative form of ink roller assembly;
FIG. 13 is an assembled mainly sectional view of another embodiment of an ink roller assembly mounted on an inker shaft;
FIG. 14 is a sectional view taken generally along line 14 — 14 of FIG. 13;
FIG. 15 is a sectional view taken generally along line 15 — 15 of FIG. 13;
FIG. 16 is a fragmentary sectional view of a portion of the ink roller assembly of the embodiment of FIGS. 13 through 16;
FIG. 17 is a bottom plan view of a print head with a row of small dialable printing characters and a row of large dialable printing characters;
FIG. 18 is a view similar to FIG. 13, but without the inker shaft, and showing an alternative embodiment of the invention;
FIG. 19 is a view similar to FIG. 18, but showing another alternative embodiment of the invention;
FIG. 20 is a view similar to FIG. 17, but showing a fragmentary portion of yet another alternative embodiment;
FIG. 21 is an elevational view of a print head and platen and an intervening web of record members;
FIG. 22 is a view taken along line 22 — 22 of FIG. 21; and
FIG. 23 is a top plan view of a label printed according to the method of the invention, but showing a code which has been activated.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to the embodiment of FIG. 1 through 4, there is shown an ink roller assembly generally indicated at 20 . The assembly is shown to include a first capillary section 21 , a second capillary section 22 and a porous ink retaining sleeve 23 . The capillary section 21 is connected to the capillary section 22 by a connector generally at 24 . The capillary sections 21 and 22 provides a capillary ink metering unit U. The capillary section 21 has a handle 25 , a flange or bearing roll 26 , a series of closely spaced discs 27 and a shaft portion or hub 28 with a connector portion 28 ′. The shaft portion 28 has a tapered bore 38 . The connector portion 28 ′ of the connector 24 is annular and has an annular external bead or tooth 29 with a lead-in or taper 30 . The capillary section 22 has an annular internal bead or tooth 31 and a lead-in or taper 32 . The capillary section 21 also has two abutment faces 33 and 34 which cooperate with respective abutment faces 35 and 36 on the capillary section 22 . The connector 24 is of the snap-type so that when the connector portion 28 ′ is moved into bore or passage 37 , the connector portion 28 ′ snaps into a locked position with the annular bead 31 . In the locked position, the abutment faces 33 and 35 , and 34 and 36 abut each other. Because of this construction there is an ink-tight seal between ink I and the bore or passage 37 on the inside of the hub section 22 . Thus, ink I will not migrate onto grooved inker shaft 40 of an inking mechanism (not shown) but shown in U.S. application Ser. No. 08/701,259 filed Aug. 22, 1996, incorporated herein by reference. The shaft 40 is shown to be stepped with a large diameter portion 41 and a small diameter portion 42 . The small diameter portion 42 has an annular external groove 43 near its terminal end 44 . The capillary section 21 has an integral flexible resilient spring finger 45 shown to be engaged in the groove 43 . To insert an ink roller assembly 20 onto the shaft 40 , the ink roller assembly 20 is slid onto the shaft 40 until the spring finger moves into the groove 43 . To remove the ink-roller assembly 20 , the user grasps the handle 25 and pulls the ink roller assembly 20 off the shaft 40 .
The capillary section 22 has a flange 46 and a hollow shaft portion or hub 47 with a series of outwardly extending closely spaced discs 48 . The discs 27 and 48 provide a long series of capillary chambers 49 extending between the flanges 26 and 46 . Supported by the discs 27 and 48 is the flexible resilient ink-retaining porous sleeve 23 . The sleeve 23 is under hoop-tension and makes direct contact with and spans across the outer peripheries of the discs 27 and 48 . Some of the capillary chambers 49 are on the capillary section 21 , but a greater number of the capillary chambers 49 on the capillary section 22 .
The capillary sections 21 and 22 have passages 27 ′ and 48 ′ through the discs 27 and 48 in the form of radical slots or cutouts. The passages 27 ′ and 48 ′ provide for some flow of ink between the passages and pressure equalization within and between the chambers 49 .
With reference to FIG. 5, there is shown another embodiment of ink roller assembly generally indicated at 50 . The assembly 50 is shown to include a shaft or shaft portion generally indicated at 51 , closely spaced discs 52 on the shaft 51 , a flange 53 on the shaft 51 and a stub end 54 which is a part of the shaft 51 . The flange 53 has an integrally molded annular projection or shoulder 55 . It is preferred that the shaft 51 and its stub end 54 , the discs 52 , the flange 53 and the shoulder 55 be of one-piece molded plastics construction and provide a capillary ink retaining unit U 1 . The flange 53 is disposed between the discs 52 and the stub end 54 . A flange or disc 56 having opposed projections 57 and 58 is shown to have been press-fitted onto the shaft 51 in FIG. 5 through 8. An end portion of the shaft 51 is considered to be a stub end 59 . The flange 56 has an annular central hole 60 provided with straight flutes 61 which compress when the stub end is received in the hole 60 . The flange 56 is likewise of one-piece molded plastics construction.
There is ink in capillary chambers 62 between the discs 52 . A flexible resilient porous ink-retaining sleeve 63 is shown in FIG. 8 to be in contact with outer peripheries 64 of the discs 52 . The sleeve 63 is in hoop tension. As shown, there are passages 65 between the discs 52 . Each passage 65 is shown to be a radial through-cut or slot. The passages 65 are shown to be aligned in the axial direction. The shaft 51 is shown to have an axis A′ and the discs 52 are coaxial with the axis A′. The passages 65 provide for equalization of the pressure between the capillary chambers 62 and also promote some flow of ink between adjacent chambers 62 and to the sleeve 63 . This is beneficial both when charging the chambers 62 and the sleeve 63 with ink I and during use of the ink roller assembly 50 .
The charging of the chambers 49 , 62 or 74 can be performed by placing the unit U or U 1 and the respective sleeve 23 , 63 or 75 in a vat of ink and drawing a vacuum; and this charging can be accomplished either when the unit U or U 1 and the respective sleeve 23 , 63 or 75 are apart or when they are assembled.
With reference to FIGS. 9 and 10, there is shown an alternative form of discs 65 and 66 . The discs 27 , 49 and 52 can be modified as disclosed in FIGS. 9 and 10. The discs 65 and 66 have different outside diameters, with the discs 66 having a slightly larger diameter than the discs 65 . A sleeve 67 is like the sleeves 23 and 63 in that it is under hoop tension and is ink receptive. The purpose of the different diameters is to promote the transference of ink from the capillary chambers 68 to the sleeve 67 . There are aligned passages 69 through the discs 65 and 66 as shown in FIGS. 9 and 10. By way of example not limitation, the difference in the diameters of the discs 65 and 66 is on the order of 0.005 inch.
FIG. 11 shows a developed view of a series of discs in which alternate discs 70 and 71 have undulating peripheries having high points 72 and low points 73 . The discs 70 and 71 also have passages 74 like the passages 49 and 62 . By way of example not limitation, the high points 72 have a pitch P of 20 degrees and consequently the low points also have a pitch of 20 degrees. Thus, there are eighteen high points and eighteen low points per disc. Every other disc 70 and 72 is offset as illustrated in FIGS. 11 and 12 . FIG. 11 shows the high points 72 of the discs 70 aligned, and out of alignment with the high point 72 of the disc 71 . The provision of discs with a variable peripheral edge configuration as shown in FIGS. 11 and 12 is applicable to the embodiment of FIGS. 1 through 4, the embodiment of FIGS. 5 through 8, the embodiment of FIGS. 13 through 16, and the embodiments of each of FIGS. 17, 19 and 20 . Such variable edge configurations promote flow of ink from capillary passages 66 to the porous sleeve 67 .
With reference to the embodiment of FIGS. 13 through 16, there is shown an ink roller assembly generally indicated at 75 rotatably mounted on the shaft 40 . The ink roller assembly 75 is shown to have sections 76 , 77 and 78 . The section 77 has a shaft or shaft portion 79 and a series of parallel discs 80 extending radially outwardly from the shaft 79 . The discs 80 are closely spaced to provide a series of capillary chambers 81 . The discs 80 are located between flanges 82 and 83 which provide annular lands 84 and 85 . A porous ink-receptive sleeve 86 is received about or spans the discs 80 and the flanges 82 and 83 . Ink I shown by short generally horizontal lines in FIG. 16 is received in the capillary chambers 81 and in the porous sleeve 86 . The sections 77 and 78 can be considered to be ink-carrying sections. The sleeve 86 before being applied over the section 77 has a small inside diameter than the outside diameters of the discs 80 and the flanges 82 and 83 so that the sleeve 86 is under slight tension. The sleeve 86 seals against the lands 84 and 85 to obviate ink I escaping from adjacent capillary chambers 81 . The section 77 also has a flange or flange portion 87 against which one end of the sleeve 86 abuts. As is apparent from FIGS. 13, 14 and 15 , the shaft 79 , the discs 80 , the flanges 82 , 83 and 87 and the sleeve 86 are annular. The shaft 79 is shown to be hollow with a larger inside diameter than the outside diameter of the shaft portion 42 . One marginal end portion 88 of the shaft 79 is tubular and has an annular external tooth 89 which is tapered or has a lead-in as shown at 90 . The entire section 77 is of one-piece molded plastics construction.
The section 78 has a shaft or shaft portion 91 which has an annular internal tooth 92 which engages the tooth 89 to hold the sections 77 and 78 securely to each other. The plastics material of which the sections 77 and 78 are constructed can yield resiliently to enable the tooth 89 to snap over the tooth 92 during connection of the sections 77 and 78 . The teeth 89 and 92 hold the sections 77 and 78 securely locked to each other. The teeth 89 and 92 provide a snap-fit connection. The shaft 91 has a notch 93 which receives an abutment or shoulder 94 on the shaft 79 . The section 78 also has a series of closely spaced parallel discs 95 which provide a series of capillary chambers 96 . The capillary chambers 96 are disposed between the flanges 97 and 98 which provide respective lands 99 and 100 . A porous ink-receptive sleeve 101 is received about the discs 95 and the flanges 97 and 98 . Lands 99 and 100 provide a seal against seepage of ink I′. The sleeve 101 , like the sleeve 86 , has a lesser inside diameter than the outside diameter of the discs 95 and flanges 97 and 98 before assembly onto the section 78 and is thus under slight tension. The sleeve 101 abuts against flanges 87 and 102 .
As best shown in FIG. 14, there are aligned passages 103 through all the discs 80 and as best shown in FIG. 15 there are aligned passages 104 through all the discs 95 for reasons stated above.
The section 76 has similarities to the section 21 although it does not have any capillary passage. The section 76 has a shaft or shaft portion 105 with a tubular marginal end portion 106 having an annular external tooth 107 . The tooth 107 has a taper or lead-in 108 . A flexible resilient spring finger 109 projects outwardly from the other end of the shaft 105 . The shaft 79 has an annular internal tooth 110 which engages the annular tooth 107 . The tooth 110 has a taper or lead-in 111 . The plastics material of which the sections 76 and 77 are constructed can yield resiliently to enable the tooth 107 to snap over the tooth 110 during connection of the sections 76 and 77 . The teeth 107 and 110 hold the sections 76 and 77 securely locked to each other. The teeth 107 and 110 provide a snap-fit connection. The shaft 79 also has notches 112 and 113 which receive respective shoulders 114 and 115 . The teeth 107 and 110 hold the sections 76 and 77 securely locked to each other. The section 76 also has a flange 116 which abuts the flange 82 and one end of the sleeve 86 . The other end of the sleeve 86 abuts the flange 87 . The section 76 also has a handle 117 .
The shaft 40 also has a tapered portion 42 ′ which is in contact with tapered inner surface 118 of the hollow shaft 105 . Reduced portion 42 of the shaft 41 is received within and spaced from shafts 79 and 91 .
The flanges 102 and 116 serve as bearing rolls which roll along rails 119 and 120 of a print head generally diagrammatically indicated at 121 . The print head 121 is shown spaced from the ink roller assembly 75 for clarity. When the flanges 102 and 116 roll across the rails 119 and 120 the sleeves 86 and 101 ink respective rows of printing characters 122 and 123 .
FIG. 16 shows the inks I and I′ represented by short wavy lines. The inks I and I′ can be different from each other in a variety of ways because the capillary chambers 81 and the sleeve 86 are isolated respectively from the capillary chambers 96 and the sleeve 101 . For example, the inks I and I′ can differ in color, viscosity and/or type. For example one ink I can be black and the ink I′ can be red. The ink I can be of a type which is visible to the human eye under conditions of ordinary lights and the ink I′ can be a security ink invisible to the human eye under conditions of ordinary light but can become visible when excited as by a chemical or by, for example, ultraviolet light. In U.S. Pat. No. 5,774,160 to A. Gundjian, the disclosure of which is incorporated herein by reference, in EXAMPLE 2, the latent image is made visible by a developer. In another example, the entire record member to be printed is coated with a first coating and an excitable ink I′ is printed over the first coating, as in U.S. Pat. No. 5,421,869 to A. Gundjian, the disclosure of which is incorporated herein by reference. See also U.S. Pat. No. 5,516,362 to A. Gundjian, the disclosure of which is incorporated herein by reference. A difference of viscosity between the inks I and I′ will affect the rates at which ink is applied by the sleeves 86 and 101 . It should be appreciated that inks I and I′ are not shown by short wavy lines in FIGS. 13, 14 and 15 for the sake of clarity.
It is evident from FIG. 13 that each of the sections 77 and 78 has the same number of capillary chambers, namely, eleven and that the sleeves 86 and 101 are the same size. It is also evident that the printing characters 121 and 122 are the same size or area, and therefore generally the same amount of ink is required for each of the characters 122 and 123 . The ink capacity of the section 77 and the sleeve 86 and the ink capacity of the section 78 and the sleeve 101 are the same.
When it is desired to ink a print head such as the print head 124 shown in FIG. 17, wherein the areas of the printing characters 125 of one row R 1 differ from the areas of the printing characters 126 of the other row R 2 , according to the invention the ink capacity and/or the ink delivery rate of the sections is desirably tailored to the ink requirements of the characters 125 and 126 as also is evident in each of the embodiments of FIGS. 18, 19 and 20 .
Print heads 121 and 124 are preferably arranged relative to the ink roller of the invention so that the sleeve of each section is aligned with and inks one line of printing characters. Such an arrangement is disclosed in U.S. Pat. No. 4,280,863. In this arrangement the axis of the ink roller extends in a direction perpendicular to the direction in which both lines of printing characters extend. Details of a typical two-line print head are disclosed in U.S. Pat. No. 4,334,470.
The embodiment of FIG. 18 is the same as the embodiment of FIGS. 13 through 16 except that section 77 A is longer (larger) than section 77 , and section 78 A is (smaller) than section 78 . Section 77 A has a larger ink capacity and number of discs 80 A and capillary chambers 81 A and ink capacity than Section 77 , namely, the section 77 A has fifteen capillary chambers 81 A. Section 78 A has a smaller ink capacity and number of disc 95 A and capillary chambers 96 A and ink capacity than section 78 . Also, the sleeve 86 A is longer than the sleeve 86 , and the sleeve 101 A is shorter than the sleeve 101 . It is evident that the sleeve 86 A is longer than the sleeve 101 A. Thus, because of the different amounts of ink required for the printing characters 125 and 126 over the life of the ink roller assembly 75 A based on the different areas of the respective printing characters 125 and 126 , the ink capacities of the sections 77 A and 78 A are made to correspondingly large and small respectively. The ink roller assembly 75 A is identical in all other respects to the ink roller assembly 75 of the embodiment of FIGS. 13 through 16. In the embodiment of FIG. 18, the same reference characters are used wherever possible to designate like or similar components with the addition of the letter “A”.
In the embodiment of FIG. 19, the section 77 B is identical to section 77 A. The difference between sections 78 A and 78 B is that section 78 A has discs 95 and capillary chambers 96 A, whereas section 78 B has no capillary chamber. The sleeve 101 B is thicker than the sleeve 101 or 101 A and consequently contains more ink. However, the sleeve 101 B contains less ink than the amount of ink I in sleeve 101 A taken together with the amount of ink I′ in capillary chambers 96 A. The ink roller assembly 75 B is identical to the ink roller assembly 75 A in all other respects. In the embodiment of FIG. 19, the same reference characters are used wherever possible to designate like or similar components with the addition of the letter “B”.
The ink roller assembly 75 C is the same as the ink roller assembly 75 A, except that section 78 C has shorter discs 95 C and capillary chambers 96 C containing less ink than the capillary chambers 96 A and the sleeve 101 C is thicker than sleeve 101 A. The difference between the embodiments of FIGS. 18 and 20 is that the combined amounts of ink contained in the sleeve 101 A and the capillary chambers 96 A is greater than the combined amounts of ink contained in the sleeve 101 C and capillary chambers 96 C. In the embodiment of FIG. 20, the same reference characters are used wherever possible to designate like or similar components with the addition of the letter “C”.
It should be noted that the sections 77 A, 77 B and 77 C are identical.
With reference to FIG. 21, there is shown the print head 124 and a stationary platen 127 . A composite web C has record members R releasably secured to a carrier web W by pressure sensitive adhesive 128 ′. The record members R are labels, but may be tags, if desired. The printing characters 125 and 126 are inked by the respective inks I and I′ of any of the ink roller assemblies 75 A, 75 B or 75 C. In the event the printing characters 125 are inked with a visible human readable ink I and the printing characters 126 are inked with invisible ink I′, the printing caused by the printing characters will not be visible when printed on the record members R without excitation or activation of the invisible ink I′.
In order to ink the printing characters 125 and 126 , the print head 124 is moved away from the platen 127 to a greater extent than shown in FIG. 21 . The ink roller assembly 75 A, 75 B or 75 C is then rolled on the rails 119 and 120 to ink the printing characters 125 and 126 simultaneously with respective inks I and I′. Assuming that the record member R to be printed is in the printing position between the print head 124 and the platen 127 , the inked print head 124 is moved into cooperation with the platen 127 and the intervening record member R.
With reference to FIG. 22, indicia 128 have been preprinted on the record members R. The indicia 128 may take any desired form, such as a store name or logo. When the printing characters 125 print on the record member R, the resultant printing 129 is visible to the human eye under ordinary lighting conditions as shown in FIG. 22, but the printing caused by the characters 126 is not visible (and therefore not shown in FIG. 22) because, in the preferred embodiment, invisible ink I′ is used.
FIG. 23 shows one of the printed record members R applied to merchandise M. The printing 130 made by printing members 126 inked with invisible ink I′ is superimposed on the indicia 128 and is visible upon excitation or activation, as illustrated.
In the various embodiments of FIGS. 13 through 16, 18 , 19 and 20 , the sleeves are assembled onto their respective sections in subassemblies, namely, section 77 and sleeve 86 , section 78 and sleeve 101 , section 77 A and sleeve 86 A, section 77 B and sleeve 86 B, section 78 B and sleeve 101 B, section 77 C and sleeve 86 C, and section 78 C and sleeve 101 C, and each such subassembly is inked as by placing it in a tank of ink and then drawing and thereafter releasing a vacuum so that the respective capillary chambers and porous sleeves are inked. There is a different tank for each type of ink. The differently inked subassemblies are snapped together following such inking.
Various components are referred to as first, second and third, but such language does not have any special meaning or importance aside from distinguishing one part from the other for ease of understanding.
By way of example, not limitation, it is preferred that the spacing between the discs of the above disclosed embodiments be less than 0.02 inch and most preferably about 0.016 inch. The passages 27 ′, 48 ′, 65 and 74 are about 0.006 inch in width and extend from the shaft to the outer peripheries of the discs 27 , 48 , 52 , 70 and 71 . The discs 27 , 48 , 52 , 70 and 71 are preferably about 0.012 inch in thickness.
Other embodiments and modifications of the invention will suggest themselves to those skilled in the art, and all such of these as come within the spirit of this invention are included within its scope as best defined by the appended claims.
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Various embodiments of an ink roller assembly include a capillary ink metering unit and a surrounding porous ink retaining sleeve, wherein the unit is comprised of a pair of capillary sections connected to each other and wherein capillary sections include a hollow shaft and discs with intervening ink capillary chambers interconnected by passages. In another embodiment, a capillary ink metering unit includes discs on a solid shaft, wherein there are passages interconnecting capillary chambers. In yet other embodiments, separate sections are provided to enable inks of different colors, viscosities and/or types to be applied to printing members. There is also provision to meter ink to printing members having different faces or areas in accordance with or as function of the sizes of those areas. The ink roller assembly with separate sections can carry both visible ink and visually alterable ink for coding purposes.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a heat storage material for air conditioning or for waste heat recovery which principally contains magnesium chloride hexahydrate, and more particularly to a heat storage material with which a nucleator is admixed so as to suppress supercooling.
2. Description of the Prior Art
Since magnesium chloride hexahydrate (MgCl 2 .6H 2 O, melting point: 117° C.) is inexpensive and has high latent heat, it is a hopeful substance as a heat storage material for air conditioning or for waste heat recovery. However, it causes a conspicuous phenomenon of supercooling during heat release and does not release the latent heat even when the temperature has become lower by about 25° C. than its solidifying point.
In order to effectively utilize the magnesium chloride hexahydrate as a heat storage material by suppressing the supercooling thereof, heat storage materials doped with nucleators have been proposed. They are disclosed, for example, in U.S. Pat. No. 4,329,242 entitled "HYDRATED MG(NO 3 ) 2 MGCL 2 REVERSIBLE PHASE CHANGE COMPOSITIONS" and U.S. Pat. No. 4,338,208, entitled "HYDRATED MGCL 2 REVERSIBLE PHASE CHANGE COMPOSITIONS". The heat storage materials disclosed here are doped with alkaline nucleators such as strontium hydroxide (Sr(OH) 2 ), calcium oxide (CaO), calcium hydroxide (Ca(OH) 2 ), barium oxide (BaO) and barium hydroxide (Ba(OH) 2 ). Since, however, the magnesium chloride, which is the principal component, is acid, the addition of the alkaline nucleators thereto results in decomposing the heat storage materials. In the course of service, accordingly, the heat storage materials become incapable of phase changes and become useless as such.
OBJECT OF THE INVENTION
The present invention has for its object to provide a heat storage material which suppresses the supercooling phenomenon of magnesium chloride hexahydrate, which is the principal component thereof, and which is usable over a long term without being decomposed.
SUMMARY OF THE INVENTION
The heat storage material of the present invention principally contains magnesium chloride hexahydrate (MgCl 2 .6H 2 O) to which a nucleator for facilitating nucleation is added, the nucleator being at least one substance selected from the group consisting of synthetic zeolite (Molecular Sieves; M 2/n O.Al 2 O 3 .xSiO 2 .yH 2 O, such as Na 12 [(AlO 2 ) 12 (SiO 2 ) 12 ].27H 2 O), magnesium silicate (Mg 2 SiO 4 ), sodium metasilicate (Na 2 SiO 3 ), sodium silicate (Na 4 SiO 4 ), calcium silicate (CaSiO 3 .nH 2 O), alumina (Al 2 O 3 ), silicic anhydride (SiO 2 ), silicon carbide (SiC), calcium carbonate (CaCO 3 ), calcium fluoride (CaF 2 ), and derivatives thereof.
By way of example, the derivative of magnesium silicate is magnesium silicate pentahydrate (Mg 2 Si 3 O 8 .5H 2 O), and the derivatives of sodium metasilicate are sodium metasilicate pentahydrate (Na 2 SiO 3 .5H 2 O) and sodium metasilicate nonahydrate (Na 2 SiO 3 .9H 2 O).
Any one of the nucleators is neutral or acid. Accordingly, even when the nucleator is added to the magnesium chloride hexahydrate which is acid, the nucleator does not decompose the magnesium chloride hexahydrate, and the heat storage material can be utilized as such over a long period of time.
The nucleator or nucleators should, preferably, be added in a total quantity of addition ranging from 0.01 part to 10 parts by weight. The reason is that, when the quantity of addition is below 0.01 part by weight, the nucleating action is slight; whereas when it is above 10 parts by weight, the heat storage effect decreases.
Further, when glass fibers which trap or hold air bubbles within the material are added together with the nucleator or nucleators, the degree of supercooling can be more suppressed.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a graph showing the solidification characteristic of an example of the heat storage material of the present invention which comprises magnesium chloride hexahydrate and synthetic zeolite, Type 4A; and
FIG. 2 is a graph showing the solidification characteristic of another example of the heat storage material of the present invention which comprises magnesium chloride and magnesium silicate.
DETAILED DESCRIPTION OF THE INVENTION
Examples of the heat storage material of the present invention are described hereinafter.
Example 1
A mixture in which 1 gram of synthetic zeolite; Type 4A, was added to 100 grams of magnesium chloride hexahydrate and was put in a glass vessel, the vessel was held in an electric furnace at 150° C. until the mixture melted completely. Thereafter, the molten mixture was let stand for cooling in the air at a temperature of 25° C. The mixture stopped supercooling at 114° C., and started the release of latent heat when its solidifying point T s =117° C. was restored. In this experiment, it has been revealed that the degree of supercooling ΔT s ; namely, the difference between the solidifying pont T s and the supercooling recovery temperature T r becomes as small as 3° C. The result is illustrated in FIG. 1. When the same sample was subjected to similar experiments 30 times, the degree of supercooling ΔT s was also about 3° C. When the synthetic zeolite; Type 4A was replaced with synthetic zeolite; Type 5A, it has been revealed that the effect is substantially the same. The latent heat of each of the heat storage materials measured by a differential calorimeter was 41 kcal/kg.
Example 2
A mixture in which 0.01 gram of calcium silicate was added to 100 grams of magnesium chloride hexahydrate was put in a glass vessel, and experiments, as in Example 1, were conducted. As a result, it has been revealed that the degree of supercooling ΔT s is 6° C. The latent heat of the heat storage measured by the differential calorimeter was 41 kcal/kg.
Similar experiments were conducted as additional examples with other nucleators, and the results of the experiments, including those of the above examples, are listed in Table 1.
It is understood from Table 1 that any of the materials doped with the nucleators becomes much smaller in the degree of supercooling ΔT s than the material doped with no nucleator (No. 9).
Further, experiments in which a plurality of nucleators were simultaneously added were carried out. Then, it has been revealed that the effect is more enhanced than in the case of adding a single nucleator. The results are listed in Table 2.
It has also been revealed that the degree of supercooling further decreases by approximately 50% when the glass fibers which hold air bubbles are added to the heat storage material doped with a plurality of nucleators. Such an example is indicated as No. 10. The principal component of the glass fibers used in this example is SiO 2 or Na 2 Ca(SiO 2 ,4) 5 . The glass fibers serve also for the prevention of two-phase separation. The glass fibers holding air bubbles can be simply prepared in such a way that a glass fiber bundle joined long is severed fine with scissors or the like.
It will be understood that the glass fibers have a diameter of from 10 to 500 micron meter and are endless; that is, the fibers may have limitless length dependent on the dimension of the mass of the heat storage material. Also, the ratio of air bubble volume to glass fiber volume is from 1 to 70%; whereas the ratio of glass fiber volume to heat storage material volume is from 1 to 20%. It has been found that below 1%, the glass fibers do not suppress supercooling, whereas above 20%, the heat storage effect decreases. Moreover, the air bubbles are included with the bundle of glass fibers added to the material.
TABLE 1__________________________________________________________________________Measured Results of the Degrees of OvercoolingNo. Heat Storage Material Nucleator Degree of Overcooling (ΔT.sub.s)__________________________________________________________________________1 MgCl.sub.2.6H.sub.2 O (100 g) Synthetic zeolite; Type 4A (1 g) 3° C.2 MgCl.sub.2.6H.sub.2 O (100 g) Synthetic zeolite; Type 5A (1 g) 3° C.3 MgCl.sub.2.6H.sub.2 O (100 g) CaSiO.sub.3.nH.sub.2 O (0.01 g) 6° C.4 MgCl.sub.2.6H.sub.2 O (100 g) Al.sub.2 O.sub.3 (0.2 g) 12° C.5 MgCl.sub.2.6H.sub.2 O (100 g) SiO.sub.2 (0.1 g) 10° C.6 MgCl.sub.2.6H.sub.2 O (100 g) SiC (0.02 g) 7° C.7 MgCl.sub.2.6H.sub.2 O (100 g) CaCO.sub.3 (0.05 g) 11° C.8 MgCl.sub.2.6H.sub.2 O (100 g) CaF.sub.2 (0.1 g) 8° C.9 MgCl.sub.2.6H.sub.2 O (100 g) None 25° C.__________________________________________________________________________
TABLE 2__________________________________________________________________________Measured Results of the Degrees of Overcooling Degree of Over-No. Heat Storage Material Nucleators cooling (ΔT.sub.s)__________________________________________________________________________1 MgCl.sub.2.6H.sub.2 O (100 g) Synthetic zeolite; Type 4A (1 g) + SiC (1 1° C.2 MgCl.sub.2.6H.sub.2 O (100 g) Synthetic zeolite; Type 4A (0.1 g) + CaCO.sub.3 (0.5 2° C.3 MgCl.sub.2.6H.sub.2 O (100 g) Synthetic zeolite; Type 4A (0.5 g) + 1° C. CaSiO.sub.3.nH.sub.2 O (0.1 g)4 MgCl.sub.2.6H.sub.2 O (100 g) Synthetic zeolite; Type 4A (0.1 g) + CaF.sub.2 (0.5 1° C.5 MgCl.sub.2.6H.sub.2 O (100 g) Synthetic zeolite; Type 4A (0.2 g) + Al.sub.2 O.sub.3 (0.2 g) 2° C.6 MgCl.sub.2.6H.sub.2 O (100 g) Synthetic zeolite; Type 4A (0.6 g) + SiO.sub.2 (0.03 2° C.7 MgCl.sub.2.6H.sub.2 O (100 g) CaSiO.sub.3.nH.sub.2 O (0.03 g) + Sic (0.3 4° C.8 MgCl.sub.2.6H.sub.2 O (100 g) CaCO.sub.3 (0.01 g) + CaF.sub.2 (0.01 g) 6° C.9 MgCl.sub.2.6H.sub.2 O (100 g) None 25° C.10 MgCl.sub.2.6H.sub.2 O (100 g) Synthetic zeolite; Type 4A (1 g) + SiC (1 g) 0.5° C. glass fibers holding air bubbles__________________________________________________________________________
Example 3
A mixture in which 0.01 gram of magnesium silicate was added to 100 grams of magnesium chloride was put in a glass vessel, and the vessel was held in an electric furnace at 150° C. until the mixture melted completely. Thereafter, the molten mixture was let stand for cooling in the air at a temperature of 25° C. The mixture stopped supercooling at 115° C., and started the release of latent heat when its solidifying point T s =117° C. was restored. In this experiment, it has been revealed that the degree of supercooling ΔT s ; namely, the difference between the solidifying point T s and the supercooling recovery temperature T r becomes as small as 2° C. The result is illustrated in FIG. 2. When the same sample was subjected to similar experiments 20 times, the degree of supercooling ΔT s was also about 2° C. The latent heat of the heat storage material measured by a differential calorimeter was 41 kcal/kg. When a similar experiment was conducted with magnesium silicate pentahydrate substituted for the magnesium silicate, the degree of supercooling could also be suppressed to 2° C.
Example 4
A mixture in which 1 gram of sodium metasilicate pentahydrate was added to 100 grams of magnesium chloride hexahydrate was put in a glass vessel, and experiments as in Example 3 were conducted. As a result, it has been revealed that the degree of supercooling ΔT s is 5° C. The latent heat of the heat storage material measured by the differential calorimeter was 41 kcal/kg. When a similar experiment was conducted with sodium metasilicate nonahydrate substituted for the sodium metasilicate pentahydrate, the degree of supercooling could also be suppressed to 5° C.
Example 5
A mixture in which 0.05 gram of sodium silicate was added to 100 grams of magnesium chloride hexahydrate was put in a glass vessel, and experiments, as in Example 3, were conducted. As a result, it has been revealed that the degree of supercooling ΔT s is 3° C. The latent heat of the heat storage material measured by the differential calorimeter was 41 kcal/kg.
The above results are collectively listed in Table 3. From this table, it is understood that any of the materials doped with the nucleators becomes much smaller in the degree of supercooling ΔT s than the material doped with no nucleator (No. 4).
Further, experiments in which a plurality of nucleators were simultaneously added were carried out. Then, it has been revealed that the effect is more enhanced than in the case of adding a single nucleator. The results are listed in Table 4.
It has also been revealed that the degree of supercooling further decreases by approximately 50% when glass fibers holding air bubbles are mixed to the heat storage material doped with a plurality of nucleators. Such an example is indicated as No. 4 in Table 4. The glass fibers serve also for the prevention of two-phase separation.
The quantity of addition of the nucleator or nucleators may well be very slight, and even the 0.01 part by weight produces the satisfactory effect as indicated in the examples. The upper limit of the quantity of addition of the nucleator or nucleators is not especially set, but it should, preferably, be at most 10 parts by weight because the addition in a very large quantity decreases the capacity of heat storage.
TABLE 3__________________________________________________________________________Measured Results of the Degrees of OvercoolingNo. Heat Storage Material Nucleator Degree of Overcooling (ΔT.sub.s)__________________________________________________________________________1 MgCl.sub.2.6H.sub.2 O (100 g) Mg.sub.2 SiO.sub.4 or Mg.sub.2 Si.sub.3 O.sub.8.5H.sub.2 O (0.01 g) 2° C.2 MgCl.sub.2.6H.sub.2 O (100 g) Na.sub.2 SiO.sub.3.5H.sub.2 O or Na.sub.2 SiO.sub.3.9H.sub.2 O (1 g) 5° C.3 MgCl.sub.2.6H.sub.2 O (100 g) Na.sub.4 SiO.sub.4 (0.05 g) 3° C.4 MgCl.sub.2.6H.sub.2 O (100 g) None 25° C.__________________________________________________________________________
TABLE 4__________________________________________________________________________Measured Results of the Degrees of OvercoolingNo. Heat Storgae Material Nucleators Degree of Overcooling (ΔT.sub.s)__________________________________________________________________________1 MgCl.sub.2.6H.sub.2 O (100 g) Mg.sub.2 Si.sub.3 O.sub.8.5H.sub.2 O (0.01 g) 1° C. Na.sub.2 SiO.sub.3.5H.sub.2 O (1 g)2 MgCl.sub.2.6H.sub.2 O (100 g) Mg.sub.2 SiO.sub.4 (0.01 g) + Na.sub.2 SiO.sub.4 (0.05 1° C.3 MgCl.sub.2.6H.sub.2 O (100 g) None 25° C.4 MgCl.sub.2.6H.sub.2 O (100 g) Mg.sub.2 Si.sub.3 O.sub.8.5H.sub.2 O (0.01 g) 0.5° C. Na.sub.2 SiO.sub.3.5H.sub.2 O (1 g) + glass fibers holding air bubbles__________________________________________________________________________
As set forth above, according to the present invention, a neutral or acid nucleator is added to magnesium chloride which is acid. Therefore, a heat storage material is prevented from becoming incapable of phase changes on account of the decomposition of the magnesium chloride, and the heat storage material which can be effectively utilized for a long term can be provided.
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The present invention relates to a heat storage material for air conditioning or for waste heat recovery, principally containing magnesium chloride hexahydrate which is doped as a nucleator with synthetic zeolite, magnesium silicate, sodium metasilicate, sodium silicate, calcium silicate, alumina, silicic anhydride, silicon carbide, calcium carbonate and/or calcium fluoride, whereby the heat storage material can be effectively used over a long period of time.
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CROSS REFERENCE OF RELATED APPLICATION
[0001] This Non-provisional application claims priority under 35 U.S.C. §119(a) on Patent Application No. 104120050 filed in Taiwan on Jun. 22, 2015, the entire contents of which are hereby incorporated by reference.
NOTICE OF COPYRIGHT
[0002] A portion of the disclosure of this patent document contains material which is subject to copyright protection. The copyright owner has no objection to any reproduction by anyone of the patent disclosure, as it appears in the United States Patent and Trademark Office patent files or records, but otherwise reserves all copyright rights whatsoever.
BACKGROUND OF THE PRESENT INVENTION
Field of Invention
[0003] The present invention relates to a method of preparing nitrogen-doped graphene and a method of producing a composite heat dispatching plate thereof, more particularly, to a method of preparing nitrogen-doped graphene using solid-state nitrogen containing precursor, and a method of producing a composite heat dispatching plate coated with nitrogen-doped graphene.
Description of Related Arts
[0004] The structure of graphene was determined and proven in 2004, and has since become the most promising and advantageous material in carbon related researches. Graphene is a layer of graphite with the stacked thickness of between one and ten carbon atoms, where carbon atoms are densely packed in two dimensional hexagonal patterns.
[0005] Graphene has many extraordinary properties including great conductivities of heat and electricity, resistance to fire, high absorption rate to electromagnetic waves and it is nearly transparent.
[0006] Furthermore, the internal electrical and thermal conductivities of graphene can be adjusted by adding various elements. Conventionally, nitrogen-doped graphene is used to produce composite materials for electrical components, where liquid nitrogen sources or gas nitrogen sources are used during doping processes. However, a process using liquid nitrogen doping sources such as disclosed in Chinese patent CN103818895A and CN104229789A require additional solvents that may cause unnecessary pollutions, as well as complicate the preparation procedures. On the other hand, using gas nitrogen during doping processes requires more energy to allow nitrogen elements to effectively dope into graphene structures. Therefore, the present invention discloses a solid-state nitrogen doping process for graphene, where the solid-state nitrogen source may be obtained at reduced costs and also transported and stored easily. In addition, the present solid-state doping process may be conducted under normal pressure, hence effectively reduces levels of difficulty and danger during production. Additionally, the process can reduce pollutions to the environment greatly as well.
SUMMARY OF THE PRESENT INVENTION
[0007] The object of the present invention is to provide a method of preparing nitrogen-doped graphene (referred as “N-graphene” hereafter) and a method of producing a high thermal conductive composite heat dispatching plate that are suitable for continuous industrial productions. The composite heat dispatching plate may be composite heat dispatching materials such as N-graphene with copper foil, N-graphene with aluminum substrate or N-graphene with other relevant metal substrates. The present invention is to dope nitrogen into oxygen functional groups of graphene where the structural composition of graphene does not comprise of nitrogen (N). A graphene precursor may be expanded graphite, graphite intercalation compound, graphite, or the combinations thereof. Various types of solid-state nitrogen are then added and sintered under a high temperature and reducing atmosphere to obtain N-graphene. The solid-state nitrogen sources include organic and inorganic solid-state nitrogen sources, and nitrogen is doped into the structure of graphene during the doping process. Solid-state nitrogen does not only replace oxygen to carry out doping, but also improve the completeness of the lattices of graphene so that the crystallinity and thermal conductivity of graphene are bettered. Furthermore, the doping process may be conducted under normal pressure which prevents lattice defect caused by changes or breakage of the graphene crystal structure under a high pressure, and is applicable to various types of graphene. The present invention improves the structural completeness of carbon molecules in graphene in a simple and efficient manner. The organic or inorganic solid-state nitrogen sources may be easily obtained at low costs that are advantageous in effectively reducing overall manufacturing costs. Another object of the present invention is to repair structural defects in graphene by doping nitrogen with a simple solid-state preparation. Common industrial coating methods are utilized to coat N-graphene onto suitable metal substrates to form a high thermal conductive composite heat dispatching plates to meet requirements for industrial productions.
[0008] For above objects, the present invention provides the method of preparing N-graphene, comprising mixing at least one solid-state nitrogen-containing precursor with a graphene to form a mixture, and sintering the mixture under a reducing atmosphere to obtain the N-graphene. Once sintered, optional grinding may be applied to obtain N-graphene powder or other solid-state N-graphene.
[0009] The present invention further provides the method of producing a composite heat dispatching plate, comprising mixing the N-graphene obtained with previously mentioned method with a polymer bonding agent to form a mixture slurry, coating the mixture slurry onto at least one surface of a metal substrate to form a composite material, drying the composite material, and obtaining the composite heat dispatching plate with a film of N-graphene. The coating of the mixture slurry on the metal substrate may be applied on one side or both sides, and the thickness of the coating layer may be thin or thick.
[0010] In the present invention, the N-graphene has the following bonding configurations: Pyridinic N(398.1˜399.3 eV) and Graphitic N(401.1˜402.7 eV).
[0011] In the present invention, the composite heat dispatching plate coated with the N-graphene film may be attached to a base material using a double sided tape, wherein the base material may be composed of metal or plastic as a panel. The N-graphene film may be positioned towards a heat source, on either side of the metal substrate, facing or against the heat source. The composite heat dispatching plate may absorb and carry away heats generated by a heat source such as a CPU or a battery through thermal conductivity or thermal radiation, so that damages to electrical parts or reduced battery performance of an electronic product due to accumulated heats may be prevented. In addition, the method of preparing N-graphene according to the present invention may also use ready formulated or commercially available organic or inorganic solid-state nitrogen sources.
[0012] Nitrogen is doped into graphene structures, the completeness of the graphene lattices is improved, and the crystallinity and thermal conductivity are bettered as a result. The graphene may be selected from at least one of monolayer graphene, multilayer graphene, graphene oxide, reduced graphene oxide and graphene derivatives.
[0013] The method of preparing N-graphene aforementioned, wherein the solid-state nitrogen containing precursor and the graphene may be mixed using solid phase mixing method to form the mixture.
[0014] The method of preparing N-graphene aforementioned, wherein the solid-state nitrogen containing precursor may be an organic solid-state nitrogen source, an inorganic solid-state nitrogen source, or the combination thereof. The organic solid-state nitrogen source may be selected from at least one of the following: C 6 H 12 N 4 , C 6 H 5 COONH 4 , (NH 4 ) 2 CO 3 , HOC(CO 2 NH 4 )(CH 2 CO 2 NH 4 ) 2 , HCO 2 NH 4 , C 11 H 7 N, C 3 H 3 N 6 , C 10 H 6 (CN) 2 and C 12 H 7 NO 2 . The inorganic solid-state nitrogen source may be selected from at least one of NH 4 NO 3 and other inorganic nitrate salts.
[0015] The method of preparing N-graphene aforementioned, wherein the graphene is preferably selected from at least one of monolayer graphene, multilayer graphene, graphene oxide, reduced graphene oxide and graphene derivatives.
[0016] The method of preparing N-graphene aforementioned, wherein the N-graphene preferably has bonding configurations of Pyridinic N (398.1˜399.3 eV) and Graphitic N (401.1˜402.7 eV).
[0017] The method of preparing N-graphene aforementioned, the total mass of the graphene and the solid-state nitrogen containing precursor being the comparing basis, wherein the mass mixing ratio between the solid-state nitrogen containing precursor and the graphene is preferably over 1 (one).
[0018] The method of preparing N-graphene aforementioned, wherein the mass mixing ratio between the graphene and the solid-state nitrogen containing precursor is preferably between 1:1 and 1:30.
[0019] The method of preparing N-graphene aforementioned, wherein the nitrogen content in the N-graphene is preferably 0.04 to 5 wt %.
[0020] The method of preparing N-graphene aforementioned, wherein the mixture is preferably sintered under the temperature between 300° C. and 800° C. .
[0021] The method of preparing N-graphene aforementioned, the mixture is preferably sintered for 0.5 to 10 hours.
[0022] The method of producing the composite heat dispatching plate aforementioned, wherein the preferred polymer bonding agent is Carboxymethyl Cellulose (CMC).
[0023] The method of producing the composite heat dispatching plate aforementioned, wherein the mixture slurry may further include a conductive agent, an adhesive agent, or the combination thereof. The conductive agent may be, but not limited to: Timcal® KS-6 (electrical conductive graphite) and Super-P (electrical conductive carbon black). The adhesive agent may be, but not limited to: Styrene-Butadiene Rubber (SBR).
[0024] The method of producing the composite heat dispatching plate aforementioned, wherein the preferred N-graphene content in the mixture slurry is 50 to 90 wt %, even more preferred is 89 to 92 wt %.
[0025] The method of producing the composite heat dispatching plate aforementioned, wherein the preferred metal substrate is a copper foil.
[0026] The method of producing the composite heat dispatching plate aforementioned, wherein the preferred thickness of the N-graphene is between 15 and 65pm.
BRIEF DESCRIPTION OF THE DRAWINGS
[0027] The above and other objects, features and advantages of the present invention will be apparent from the following detailed description of the embodiments of the invention in conjunction with the accompanying drawings, in which:
[0028] FIG. 1 is a schematic illustration of the structure of a composite heat dispatching plate of experimental samples 1 to 5, 7 to 9, 12 and embodiments 12 to 14 according to the present invention;
[0029] FIG. 2 is a schematic illustration of a testing device of the composite heat dispatching plate of experimental sample 1 to 5, 7 to 9, 12 and embodiments 12 to 14 according to the present invention;
[0030] FIG. 3A is a scanning electron microscope (SEM) image of a graphene as a basis for comparison according to the present invention;
[0031] FIG. 3B is a X-ray Photoelectron spectroscopy (XPS) bond energy chart of the nitrogen-doped graphene according to the present invention;
[0032] FIG. 3C is a XPS bond energy chart of the nitrogen-doped graphene of the embodiment 6 according to the present invention;
[0033] FIG. 4 is a schematic illustration of the structure of a composite heat dispatching plates of experimental samples 6, 10-11 and 13 of the present invention;
[0034] FIG. 5 is a microscope image of a copper foil coated with graphene not being nitrogen doped of experimental sample 5 of the present invention;
[0035] FIG. 6 is a temperature distribution chart (thermograms) on the overall observation on the composite heat dispatching plate coated with nitrogen-doped graphene (left) and copper foil (right) of embodiment 12 of the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0036] The present invention is explained in relation to its embodiments and experimental samples. Any person of ordinary skills in the art shall understand methods disclosed in the present invention and appreciate advantages and benefits other than mentioned therein. It is to be understood that many other possible modifications and variations can be made without departing from the spirit and scope of the invention as hereinafter claimed.
[0037] The following description discloses a nitrogen-doped graphene (referred as “N-graphene” hereafter), a method of preparing the N-graphene, and embodiments of a testing device thereof. The description further discloses a composite heat dispatching plate coated with N-graphene and a method of producing thereof, as well as effects of various coating thicknesses, single or double sided coated, and facing direction of the film. It should be noted that drawings in the description are only schematic representatives of features of the present invention, and are not scaled to actual dimensions.
[0038] The present invention provides an N-graphene, including the following chemical bonding configurations: Pyridinic N (398.1˜399.3 eV) and Graphitic N (401.1˜402.7 eV), wherein solid-state nitrogen sources may be organic or inorganic nitrogen sources, the organic nitrogen sources include C 6 H 12 N 4 (HMT), C 6 H 5 COONH 4 , (NH 4 ) 2 CO 3 , HOC(CO 2 NH 4 )(CH 2 CO 2 NH 4 ) 2 , HCO 2 NH 4 , C 11 H 7 N, C 3 H 3 N 6 , C 10 H 6 (CN) 2 and C 12 H 7 NO 2 , and the inorganic nitrogen sources include NH 4 NO 3 and other inorganic nitrate salts.
[0039] The method of preparing N-graphene of the present invention may also utilize graphene obtained from mechanical exfoliation or oxidation reduction; and then mix the graphene with the organic or inorganic nitrogen sources, dope nitrogen into structures of graphene, improve completeness of graphene lattices, and better crystallinity and thermal conductivity of the graphene. The graphene may be selected from at least one of monolayer graphene, multilayer graphene, graphene oxide, reduced graphene and graphene derivatives.
[0040] With reference to FIGS. 1 and 2 , schematic illustrations of the structure of the composite heat dispatching plate and the testing device thereof of experimental samples 1 to 5 , 7 to 9 , 12 and embodiments 12 to 14 of the present invention, the composite heat dispatching plate 100 comprises a copper foil 102 and a N-graphene film 101 coated on one of the surfaces of the copper foil 102 . The present invention discloses a temperature testing method as following: applying a double sided tape 103 or other adhesive material on a surface of the copper foil 102 of the composite heat dispatching plate 100 , attaching the composite heat dispatching plate 100 together with the double sided tape 103 on a base material 106 , and then placing above in a testing device for temperature tests. The testing device may be regarded as a simulation of a tablet PC, wherein a heating chip 107 of one square centimeter (1×1 cm 2 ) in size is attached to the copper plate 105 to simulate an operating CPU, and a tin foil 111 attached thereunder is to simulate other electrical parts of the tablet PC. This testing device has three sensing spots for temperature tests, namely a thermal spot 110 on the heating chip 107 , a first testing spot 108 on the base material 106 on top of the heating chip 107 , and a second testing spot 109 which is also on the base material 106 and 0.5 (zero point five) to 5 (five) centimeters apart from the first testing spot 108 . This temperature testing method measures the gap between a temperature difference T 1 (° C.) and another temperature difference T 2 (° C.), wherein the temperature difference T 1 is measured between the first testing spot 108 and the second testing spot 109 of the copper foil 102 , and the temperature difference T 2 is measured between the first testing spot 108 and the second testing spot 109 of the composite heat dispatching plate 100 . In this embodiment, the horizontal distance between the first testing spot 108 and the second testing spot 109 is 0.5 (zero point five) centimeter, but not restricted thereto in other embodiments of the present invention. With reference to FIG. 2 , the temperature on the thermal spot 110 is higher than the temperature on the first testing spot 108 , and the temperature on the first testing spot 108 is higher than the temperature on the second testing spot 109 . Heats are effectively directed away from the heating chip 107 when the composite heat dispatching plate 100 has a good heat dispatching performance, the temperature on the first testing spot 108 and the temperature on the second testing spot 109 are closer as a result. The temperature difference T 2 between the first testing spot 108 and the second testing spot 109 of composite heat dispatching plate 100 is smaller, the temperature difference T 1 between the first testing spot 108 and the second testing spot 109 of the copper foil 102 is larger, hence T 1 (° C.) is greater than T 2 (° C.). Therefore, a positive value of T 1 minus T 2 indicates a good heat dispatching performance of the composite heat dispatching plate 100 , where the greater the value, the better the heat dispatching performance.
[0041] With reference to Table 1 below, 1 (one) gram of graphene is analyzed for its nitrogen, oxygen and carbon contents using X-ray photoelectron spectroscopy (XPS). The results as indicated in column 1 of Table 1 are used as a basis for comparison for content analysis of embodiments 1 to 7. In addition, scanning electron microscope (SEM) image of the graphene as another basis for comparison is shown in FIG. 3A . The graphene may be in a power form or other forms of solids, and not restricted thereto in the present invention.
[0042] Embodiment 1 of the present invention provides a structure of N-graphene and a preparing method thereof with the following steps: mixing 1 (one) gram of graphene and 1 (one) gram of solid-state Hexamethylenetetramine (HMT) (C 6 H 12 N 4 ) thoroughly to form a mixture, grinding and placing above mixture in a crucible (or thoroughly mixing without grinding, not restricted thereto in the present invention), placing the crucible in a high temperature sintering furnace to sinter under the temperature of 800° C. and a H2/N2 reducing atmosphere for 8 (eight) hours, and finally removing the crucible and obtaining N-graphene from the furnace. The N-graphene may be in the form of powder or any other forms of solids, and not restricted in the present invention.
[0043] With reference to Table 1, the N-graphene obtained in embodiment 1 is analyzed for nitrogen, oxygen and carbon contents using XPS, and the result is shown in column 2 of Table 1.
[0044] Embodiments 2 to 7 of the present invention provide a structure of N-graphene and preparing methods thereof, wherein the steps, conditions and the type of solid-state nitrogen containing precursor are the same as embodiment 1. The differences in embodiment 2 to 7 are different masses of solid-state HMT are added. The mass ratios between graphene and solid-state EMT are 1:3, 1:5, 1:7, 1:10, 1:20 and 1:30 respectively. The nitrogen, oxygen and carbon contents in each of embodiment 2 to 7 are subsequently analyzed using XPS, and the results are as shown in Table 1 and bond energies thereof in FIGS. 3B and 3C .
[0045] With reference to Table 1, embodiment 6 is a result of additional 20 wt % solid-state HMT to the basis for comparison, wherein the nitrogen content is 3.92% higher as compared to the basis. With further reference to FIG. 3C , which indicates the XPS bond energy chart of the N-graphene of embodiment 6, and the bonding configuration is known as Pyridinic N (398.1˜399.3 eV) and Graphitic N (401.1˜402.7 eV). In contrast to the bonding configuration consists of mainly C and O bonding in the basis for comparison, the bonding configuration of embodiment 6 have additional C and N bonding. Because C and N bonding reduces the structural defects in graphene lattices, embodiment 6 produces a result of better thermal conductivity, which translates to a better heat dispatching performance. Similarly, N-graphene of embodiments 1, 2 to 5 and 7 also achieve better heat dispatching performances. In the present invention, the nitrogen content in N-graphene is 0.04 to 5 wt %, the preferred nitrogen content is 2 to 5 wt %, and the more preferred nitrogen content is 4 wt %.
[0046] Embodiments 8 to 11 provide a structure of N-graphene and a preparing method thereof, wherein the steps and conditions of solid-state nitrogen containing precursor mixing ratio are the same as embodiment 1. The differences in embodiment 8 to 11 are different organic and/or inorganic solid-state nitrogen sources adding to them. The added organic and/or inorganic solid-state nitrogen sources are (NH 4 ) 2 CO 3 , NH 4 NO 3 , NCO 2 NH 4 and C 3 H 3 N 6 respectively, as indicated in Table 2.
[0047] The nitrogen, oxygen and carbon contents of N-graphene of embodiments 8 to 11 are analyzed using XPS, and the results are shown as in Table 2.
[0000]
TABLE 1
graphene:HMT
C wt. %
O wt. %
N wt. %
Basis for
1:0
86.65
10.2
0
comparison
Embodiment 1
1:1
80.78
12.19
3.27
Embodiment 2
1:3
77.7
14.05
3.04
Embodiment 3
1:5
78.81
14.32
2.41
Embodiment 4
1:7
81.62
11.85
3.34
Embodiment 5
1:10
82.37
10.51
4.61
Embodiment 6
1:20
80.13
12.75
3.92
Embodiment 7
1:30
82.63
11.9
3.53
[0000]
TABLE 2
Solid-state
Embodiment
nitrogen source
C wt. %
O wt. %
N wt. %
8
(NH 4 ) 2 CO 3
90.57
8.21
1.14
9
NH 4 NO 3
91.78
8.22
0.04
10
HCO 2 NH 4
92.37
6.25
1.3
11
C 3 H 3 N 6
89.17
7.47
3.36
[0048] Experimental samples 1 to 13 provide a structure of composite heat dispatching plate coated with graphene that is not nitrogen doped. With reference to FIG. 1 , the structure of experimental samples 1 to 13 is similar to that of embodiments 1 to 11, except the N-graphene film 101 is replaced by a graphene film not being nitrogen doped. With reference to FIG. 1 and Table 3, mixture slurry used for experiments is similar to that of aforementioned basis for comparison, with additional non-essential ingredients such as KS-6, Super-P, CMC, SBR . . . etc. The mixture slurry is used to experiment different heat dispatching performances with various graphene mass contents, mixture slurry coating thicknesses, and the copper foil 102 is coated on single side or double sides. Once the best performance condition is determined, heat dispatching performance of N-graphene will be further experimented. Because N-graphene has additional C and N bonding to reduce structural defects in graphene lattices, N-graphene performs better in heat dispatching as compared to graphene not being nitrogen doped. Methods of preparing experimental samples 1 to 13 are similar, except different proportions of graphene, polymer bonding agent (CMC), electrical conductive agent (KS-6, Super-P), and adhesive agent (SBR) are mixed. Respective mass mixing ratios between graphene and the whole mixture slurry are 50, 60, 70, 80, 89, 92 and 93 wt %. The amount of KS-6, Super-P, CMC and SBR added depending on the content of graphane is changed as shown in Table 3. To avoid repeated descriptions, only experimental sample 5 and Table 3 are discussed in details, and experimental samples 1 to 4 and 6 to 13 may be prepared accordingly.
[0049] Experimental sample 5 of the present invention provides a structure of a composite heat dispatching plate coated with graphene not being nitrogen doped, and a preparing method thereof, including following steps: preparing 1.5 g graphene, 0.1011 g CMC, 0.0506 g Super-P, 0.0337 g SBR, adding water as solvent and aforementioned ingredients orderly into a homogenizer mixer, mixing thoroughly to form a mixture slurry, applying the mixture slurry onto a copper foil 102 , coating the mixture slurry onto the copper foil 102 using a coating applicator, placing the coated copper foil 102 into a high temperature furnace to remove water at the temperature 40° C. to 100° C. to obtain a composite material, measuring the thickness of the composite material, and pressing the composite material to 50 μm with appropriate pressing rate to obtain the composite heat dispatching plate 100 coated with the graphene film not being nitrogen doped 101 .
[0050] With reference to FIG. 2 , the composite heat dispatching plates 100 prepared in experimental samples 1 to 5 , 7 to 9 and 12 have the graphene film not being nitrogen doped 101 coated on single side thereof, and a double sided tape 103 or other adhesive material is attached. The composite heat dispatching plate 100 coated with the graphene film not being nitrogen doped 101 and the double sided tape 103 are then attached to a base material 106 , and then positioned in a testing device. A heating energy of 3W is provided to a heating chip 107 to increase the temperature for measuring the gap between temperature difference T 1 (° C.) and another temperature difference T 2 (° C.), wherein the temperature difference T 1 is measured between the first testing spot 108 and the second testing spot 109 of the copper foil 102 , and the temperature difference T 2 is measured between the first testing spot 108 and the second testing spot 109 of the composite heat dispatching plate 100 coated with the graphene film not being nitrogen doped 101 . With reference to Fig. 4 , the composite heat dispatching plates 200 prepared in experimental samples 6 , 10 , 11 and 13 have the graphene film not being nitrogen doped 101 coated on double sides thereof, which means the two opposite surfaces of the copper foil 102 are both coated with the graphene film not being nitrogen doped 101 . Same experiments are conducted as shown in FIG. 2 for experimental samples 6 , 10 , 11 and 13 , except the composite heat dispatching plate 100 is replaced with the composite heat dispatching plate 200 as shown in FIG. 4 , and the results are as shown in Table 3.
[0051] With reference to Table 3, experimental sample 5 is the result of additional 40 wt % to experimental sample 1 . Comparing to experimental sample 1 , the coating thickness is 10 μm thinner, but the heat dispatching performance is 1.27° C. higher. With further reference to FIG. 5 , which is a microscope image of the copper foil 102 single side coated with the graphene film not being nitrogen doped 101 according to experimental sample 5 of the present invention. It is noted that the dispersion uniformity of graphene and other additives is higher when high graphene content is added, thus the heat dispatching performance is also higher as compared to when low graphene content is added.
[0052] Experimental samples 10 and 13 have the same graphene content of 60 wt %, the same proportions of KS-6, Super-P, CMC and SBR, and both have the graphene film not being nitrogen doped 101 coated on double sides. The only difference is coating thicknesses and the result is that the heat dispatching performance of experimental sample 13 is 0.7° C. higher than that of experimental 10 . Therefore, a thicker graphene film not being nitrogen doped has higher graphene content and better heat dispatching performance as compared to a thinner graphene film not being nitrogen doped.
[0053] Experimental samples 12 and 13 have the same graphene content of 60 wt %, the same proportions of KS-6, Super-P, CMC and SBR, and both have the same thickness of the graphene film not being nitrogen doped 101 . The only difference is the coating method where experimental sample 12 being single side coated with the graphene film not being nitrogen doped 101 and experimental sample 13 being double sides coated. The result is that the heat dispatching performance of experimental sample 13 is 0.8° C. higher than that of experimental 12 . Therefore, a double sides coating allows one side of the graphene film not being nitrogen doped 101 to absorb heats, and another side of the graphene film not being nitrogen doped 101 to dispatch heats. Therefore, the double sides coating has better heat dispatching performance as compared to the single side coating.
[0000]
TABLE 3
Single/
Copper
Double
Foil/Coating
Experimental
Graphene
KS-6
Super-P
CMC
SBR
Side
thickness
T1-T2
Sample
(wt.) %
(wt.) %
(wt.) %
(wt.) %
(wt.) %
coating
(μm)
(° C.)
1
50
35
5
6
4
Single
35/25
0.03
2
60
25
5
6
4
Single
35/25
0.1
3
70
15
5
6
4
Single
35/25
0.3
4
80
5
5
6
4
Single
35/25
0.4
5
89
—
3
6
2
Single
35/15
1.3
6
89
—
3
6
2
Double
35/65
1.9
7
90
—
—
10
—
Single
35/25
0.3
8
92
—
—
8
—
Single
35/15
0.7
9
93
—
—
7
—
Single
35/15
0.34
10
60
25
5
6
4
Double
35/25
0.2
11
60
25
5
6
4
Double
35/25
0.6
12
60
25
5
6
4
Single
35/50
0.1
13
60
25
5
6
4
Double
35/50
0.9
[0054] Embodiment 12 of the present invention provides a structure and a method of preparing a composite heat dispatching plate coated with N-graphene, wherein the preparing steps and conditions are similar to experimental sample 5 , except embodiment 12 uses the same N-graphene obtained in embodiment 6. The N-graphene content is 89 wt % and the proportions of KS-6, Super-P, CMC and SBR, coating thickness, and coating method are the same. Table 4 indicates differences in heat dispatching performances between N-graphene and graphene not being nitrogen doped.
[0055] With reference to FIG. 2 , the composite heat dispatching plate 100 coated with N-graphene film 101 is attached with a double sided tape 103 or other adhesive material, attached to the base material 106 , and then positioned in a testing device. A heating energy of 3 W is provided to a heating chip 107 to increase the temperature for measuring the gap between temperature difference T 1 (° C.) and another temperature difference T 2 (° C.), wherein the temperature difference T 1 is measured between the first testing spot 108 and the second testing spot 109 of the copper foil 102 , and the temperature difference T 2 is measured between the first testing spot 108 and the second testing spot 109 of the composite heat dispatching plate 100 coated with N-graphene film 101 . Table 4 indicates the results where the single side coating with the graphene film not being nitrogen doped of experimental sample 5 is replaced by the single side coating with N-graphene film of embodiment 12. The heat dispatching performance of embodiment 12 is 1.4° C. higher that of experimental sample 5 . Therefore, the N-graphene film has better heat dispatching performance than the graphene film not being nitrogen doped.
[0056] Embodiments 13 and 14 of the present invention provide a structure and a method of preparing a composite heat dispatching plate coated with N-graphene, wherein the preparing steps and conditions are similar to experimental sample 5 , except embodiments 13 and 14 use the same N-graphene obtained in embodiment 6. The N-graphene contents of embodiments 13 and 14 are 89 wt % and 92 wt % respectively. Proportions of Super-P, CMC and SBR of embodiment 13 are 3 wt %, 6 wt % and 2 wt % respectively. Proportions of Super-P, CMC and SBR of embodiment 14 are 0 wt %, 8 wt % and 0 wt % respectively. Embodiments 13 and 14 are both single side coated with the thickness of 15 μm. Table 4 indicates different heat dispatching performances between different content proportions of N-graphene.
[0057] With reference to FIG. 2 , the composite heat dispatching plate 100 coated with N-graphene film 101 is attached with a double sided tape 103 or other adhesive material, attached to the base material 106 , and positioned in the testing device. A heating energy of 3 W is provided to a heating chip 107 to increase the temperature by 15° C. for measuring the gap between temperature difference T 1 (° C.) and another temperature difference T 2 (° C.), wherein the temperature difference T 1 is measured between the first testing spot 108 and the second testing spot 109 of the copper foil 102 , and the temperature difference T 2 is measured between the first testing spot 108 and the second testing spot 109 of the composite heat dispatching plate 100 coated with N-graphene film 101 . Table 4 indicates the results where the heat dispatching performance of embodiment 13 is 0.2° C. higher than embodiment 14. The reason being the added Super-P assists in filling gaps formed during stacking process of N-graphene. Therefore, N-graphene with added Super-P has better heat dispatching performance than that of without Super-P.
[0058] It is further noted in results of experimental sample 5 and embodiments 12 to 14 in Table 4, the heat dispatching performances drop when the temperature of the heating chip 107 reaches 90° C. . The reason being the high temperature causes N-graphene molecules to vibrate at a higher frequency, hence the contacting surface between the coated N-graphene film 101 and the copper foil 102 is reduced and causing the dropping heat dispatching performance. Even the heating chip 107 is heated to 90° C. as shown in embodiments 13-14, the temperature testing method of T 1 -T 2 (° C.) in the present invention is positive, which is still better than the copper foil 102 using alone and can effectively enhance the ability of heat dispatching performance about 0.2-0.4° C.
[0000]
TABLE 4
Graphene or
Single/
Copper
N-graphene
Heating Chip
Double
Foil/Coating
N-graphene
film
Temperature
Super-P
CMC
SBR
side
thickness
T1-T2
film
(wt.) %
(° C.)
(wt.) %
(wt.) %
(wt.) %
coating
(μm)
(° C.)
Experimental
No
89
75
3
6
2
Single
35/15
1.3
Sample 5
Embodiment
Yes
89
75
3
6
2
Single
35/15
2.7
12
Embodiment
Yes
89
90
3
6
2
Single
35/15
0.4
13
Embodiment
Yes
92
90
—
8
—
Single
35/15
0.2
14
[0059] With reference to FIG. 6 , a structure of a composite heat dispatching plate coated with N-graphene film and a testing method thereof are disclosed. FIG. 6 is an overall observation on temperature distribution changes in zones. The same testing device as shown in FIG. 2 is used and a heating energy of 3 W is provided to the heating chip 107 . After heating for 5 (five) minutes, temperature distribution changes in zones are observed using a thermal imaging camera. P 1 and P 4 are the sensing spots on top of the heating chip 107 . P 2 and P 3 are sensing spots that are one and two centimeters extended from P 1 respectively. P 5 and P 6 are one and two centimeters extended from P 4 respectively. A higher temperature indicates that heats are more effectively carried away from the heat source horizontally and vertically. The image on the left and the image on the right of FIG. 6 are comparisons of heat dispatching performances between the composite heat dispatching plate 100 coated with N-graphene film 101 and the copper foil 102 obtained in embodiment 12.
[0060] The observation results of the thermal imaging camera show that the composite heat dispatching plate 100 coated with N-graphene film 101 increases heat radiation absorption and thermal conduction efficiency. With reference to FIG. 6 , after heating for 5 (five) minutes, temperatures of P 1 , P 2 and P 3 of the composite heat dispatching plate 100 coated with N-graphene film 101 are higher than temperatures of P 4 , P 5 and P 6 of the copper foil 102 . Therefore, the composite heat dispatching plate 100 coated with N-graphene film 101 of the present invention have improved heat radiation absorption and thermal conduction efficiency vertically (temperature of P 1 is higher than P 4 ) and horizontally (temperature of P 3 is higher than P 6 ), and have a better heat dispatching performance as compared to the copper foil 102 of the image on the right.
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The present invention relates to a method of preparing nitrogen-doped graphene, comprising: mixing at least one solid-state nitrogen containing precursor with a graphene to form a mixture, and sintering the mixture under a reducing atmosphere to obtain the nitrogen-doped graphene. The present invention further provides a method of producing a composite heat dispatching plate coated with nitrogen-doped graphene film, comprising: mixing a nitrogen-doped graphene obtained aforementioned with a polymer bonding agent to form a mixture slurry, coating the mixture slurry onto at least one surface of a metal substrate to form a composite material, drying the composite material, and obtaining the composite heat dispatching plate with a film of nitrogen-doped graphene. Structural defects of graphene lattices are reduced during doping process so that crystallinity and thermal conductivity are improved. Methods of the present invention may be conducted under normal pressure using commercially available solid-state nitrogen sources without adding polluting solvents to provide a safe, stable and cost effective preparation of composite heat dispatching material.
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RELATED APPLICATIONS
This is a continuation of U.S. patent application Ser. No. 08/873,855, filed Jun. 12, 1997, now U.S. Pat. No. 6,281,879, which is a continuation of U.S. patent application Ser. No. 08/709,529, filed Sep. 6, 1996, now abandoned, which is a File Wrapper Continuation of U.S. patent application Ser. No. 08/260,558, filed Jun. 16, 1994, now abandoned, which applications are incorporated herein by reference.
TECHNICAL FIELD
The present invention relates generally to data processing systems and, more particularly, to the displaying of graphical information in data processing systems.
BACKGROUND OF THE INVENTION
Many conventional application programs utilize tool bars. Tool bars provide the user with a number of tools that assist the user in performing tasks. Typically, a separate control is provided for each tool on the tool bar. The control may be a pushbutton or another graphical object that allows the user to invoke the desired tool. Often times the controls on the tool bar have icons on their faces that indicate the nature of the tool. Unfortunately, as the typical number of controls on the tool bar has grown for applications, it has become more and more difficult for the user to discern the nature of the tool solely from the icons shown as part of the tool bar. As such, many users have difficulty using the tools on the tool bar.
SUMMARY OF THE INVENTION
The limitations of the prior art are overcome by the present invention. In accordance with a first aspect of the present invention, a method is practiced in a data processing system having a video display for displaying a cursor that points to positions on the video display. The data processing system also includes an input device for manipulating the cursor. In accordance with this method, it is first determined that the cursor points to a position within a region on the video display. A velocity metric of the cursor is measured. Where the velocity metric does not exceed a predetermined threshold value, an event is triggered. On the other hand, where the velocity metric exceeds the predetermined threshold value, the event is inhibited.
In accordance with a second aspect of the present invention, it is determined that a cursor points to a position within a region on the video display. A time period metric that specifies how long the cursor has remained pointing within the region is measured. A velocity metric of the cursor within the region is also measured. Based upon these metrics, a determination is made whether to trigger an event.
In accordance with an additional aspect of the present invention, a method is practiced in a data processing system having a video display for displaying a cursor that points to positions in the video display and an input device for manipulating the cursor. In accordance with this method, a graphical object is displayed on the video display. The user uses the input device, and in response, the data processing system positions the cursor to point at the graphical object. A predetermined period of time, such as a time greater than 0.4 seconds, is allowed to pass and then a determination is made whether the cursor still points at the graphical object. If it is determined that the cursor still points at the graphical object, information about the graphical object is displayed adjacent to the graphical object on the video display.
In accordance with another aspect of the present invention, a method is practiced wherein a tool bar having tools is displayed on the video display. When the user uses the input device, the cursor is position to point at a selected one of the tools on the tool bar. The system waits a predetermined non-negligible amount of time. The system also measures a velocity metric of the cursor within the first graphical object. If the cursor still points at the selected tool after waiting the predetermined non-negligible amount of time and the velocity metric has remained below a predetermined threshold during the predetermined non-negligible amount of time, information about the selected tool is displayed in the video display. The position is adjacent to the selected tool.
In accordance with a further aspect of the present invention, a method is practiced in a computer system having a video display for displaying a cursor that points to positions on the video display and an input device for moving the cursor on the video display. In this method, a first graphical object is displayed on the video display. In response to the user using the input device, the cursor is positioned to point at the first graphical object. The system waits a non-negligible predetermined amount of time. A determination is made whether the cursor still points at the graphical object after the non-negligible predetermined amount of time has passed. Where the cursor still points at the first graphical object, a number of steps are performed. These steps include displaying information about the first graphical object adjacent to the first graphical object of the video display. The non-negligible predetermined amount of time is then reset to a substantially shorter amount of time. A second graphical object is displayed on the video display and, in response to the user using the input device, the cursor is positioned to point at the second graphical object on the video display. The system waits the substantially shorter amount of time. Where the cursor is still pointing at the second graphical object after waiting the substantially shorter period of time, information about the second graphical object is displayed adjacent to the second graphical object on the video display.
In accordance with a still further aspect of the present invention, a data processing system includes a video display for displaying video data. The video display displays a first graphical object and a cursor that points to the first graphical object. An input device is included in this part of the data processing system for moving the cursor on the video display. A message generator is provided for displaying information about the first graphical object. The information is displayed adjacent to the first graphical object on the video display when the cursor remains pointing at the first graphical object for a predetermined non-negligible amount of time. The message generator includes a comparator and a message source. The comparator determines whether the cursors remain pointing at the first graphical object for the predetermined non-negligible amount of time. The message source provides and displays information about the first graphical object adjacent to the first graphical object on the video display when the comparator determines that the cursor has remained pointing at the first graphical object for the specified amount of time.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram of a data processing system that is suitable for practicing a preferred embodiment of the present invention.
FIG. 2A is a diagram illustrating a tool bar and a tool tip that is provided for a print button in accordance with the preferred embodiment of the present invention.
FIG. 2B is a diagram illustrating a tool bar and a tool tip that is provided for a font list box in accordance with the preferred embodiment of the present invention.
FIG. 3A is a flow chart illustrating the steps performed to initially set a timer when a cursor is positioned over a control on the tool bar in accordance with the preferred embodiment of the present invention.
FIG. 3B is a flow chart illustrating the steps performed to determine the magnitude of the velocity of the cursor when the cursor is positioned over a control on the tool bar in accordance with the preferred embodiment of the present invention.
FIG. 4 is a flow chart illustrating the steps performed to determine whether a tool tip is to be displayed in the preferred embodiment of the present invention.
FIG. 5 is a flow chart illustrating the steps performed when a cursor no longer points within the tool bar in the preferred embodiment of the present invention.
FIG. 6 is a low chart illustrating the steps that are performed relative to the timer when the cursor leaves the tool bar in the preferred embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The preferred embodiment of the present invention displays a tool tip when a mouse cursor points to a tool or a tool bar for a sufficient amount of time and the magnitude of the velocity of the mouse cursor remains below a predetermined threshold. A tool tip is a brief textual message, such as a name of a tool, that identifies the nature of the tool. The preferred embodiment of the present invention provides a delay between when the mouse cursor is initially positioned to point at the tool control on the tool bar and when the tool tip is displayed. This delay prevents the user from receiving undesired tool tips when the user inadvertently passes the mouse cursor over a control on the tool bar. The delay is sufficiently long (i.e., it is non-negligible) to allow the user to move the mouse cursor if he does not want to receive a tool tip. The delay is shortened when an initial tool tip is displayed so as to allow the user to quickly browse the tool controls that are available on the tool bar. The magnitude of the velocity of the mouse cursor is measured to determine whether the user likely intends to point at the tool to receive a tool tip or whether the user, instead, is merely passing over the tool while moving to another destination.
Although the preferred embodiment of the present invention concerns controlling when tool tips for tools on a tool bar are displayed, those skilled in the art will appreciate that the present invention may generally be applied to other regions of a video display (such as other types of graphical objects) for which graphical information is to be provided. It should be appreciated that the present invention may be applied to both visible and invisible graphical objects.
FIG. 1 is a block diagram of a data processing system 10 that is suitable for practicing the preferred embodiment of the present invention. The data processing system 10 includes at least one central processing unit (CPU) 12 . The CPU 12 is connected to a number of peripheral devices, including a mouse 14 , a keyboard 16 and a video display 18 . The CPU 12 is also connected to a memory 20 and a secondary storage device 22 , such as a hard disk drive. The memory 20 holds a copy of an operating system 24 , such as the Microsoft Windows, version 3.1, operating system sold by Microsoft Corporation of Redmond, Wash. The memory 20 also holds a copy of an application program 26 . The implementation of the preferred embodiment of the present invention will be described below with reference to use of tool tips within the application program 26 . Nevertheless, it should be appreciated that the tool tips may alternatively be implemented in the operating system 24 or as a system resource.
FIG. 2A shows the tool bar 34 that is generated and displayed on the video display 18 when the application program 26 is run on the CPU 12 . The tool bar 34 includes a number of controls, such as buttons and list boxes, that enable a user to access the tools of the tool bar. When the user positions a mouse cursor 30 over one of the buttons and clicks the mouse (i.e., quickly depresses and releases a predefined one of the mouse buttons), the tool associated with the button is invoked. Similarly, by positioning the mouse cursor 30 over one of the buttons of the list boxes, a drop-down list appears, and the user may select one of the options on the drop-down list using the mouse 14 .
The tool bar 34 is created as a window by the application program 26 . The operating system 24 facilitates the definition of such windows (as is provided in the Microsoft Windows, version 3.1, operating system). FIG. 2A shows the mouse cursor 30 pointing to a print button 32 on the tool bar 34 . When a user positions the mouse cursor 30 over the print button 32 and clicks the mouse button, the document currently displayed in the window of the application program is printed.
The user interface provided for the application program 24 is logically divisible into a number of windows. One of these windows is the tool bar 34 . In general, each window of the user interface has a separate window procedure associated with it. The operating system 24 maintains a message queue for each program that generates windows. Accordingly, the application program 26 has its own message queue. Since the application program 26 may generate multiple windows, the message queue may hold messages for multiple windows. When an event occurs, the event is translated into a message that is put into the message queue for the application program 26 . The application program 26 retrieves and delivers the message to the proper windows by executing a block code known as the “message loop.” The window procedure that receives the message then processes the message.
Movements of the mouse 14 are reflected in messages that are placed into the message queue of the application program 26 . In particular, when a user positions the mouse cursor 30 with the mouse 14 over a window or clicks the mouse by depressing one of the mouse buttons within a window, the procedure for the window receives a mouse message. The operating system 24 provides a number of predefined mouse messages. The mouse messages specify the status of mouse buttons and the position of the mouse cursor 30 within the window. The position of the mouse cursor 30 within the window is specified in (X, Y) coordinates relative to the upper left-hand corner of the window. Thus, when the mouse cursor 30 moves within the tool bar 34 , the position of the mouse cursor 30 within the tool bar is reflected and a mouse message that specifies (X, Y) coordinates of the mouse cursor relative to the upper left-hand corner of the tool bar. The window procedure receives the mouse message and utilizes the information contained in the message to respond to the mouse 14 activities.
As mentioned above, the application program 26 specifies the window that constitutes the tool bar 34 . The application program 26 paints each of the controls, including print button 32 , at known locations within the window of the tool bar 34 . When the mouse cursor 30 is positioned within the tool bar, mouse messages specify the position of the mouse cursor within the tool bar 34 . The mouse messages are sent to the window procedure that is responsible for the tool bar window. The window procedure for the tool bar 34 compares the coordinates specified by the mouse message with the known location of the controls within the tool bar. Accordingly, the window procedure for the tool bar 34 can determine whether the mouse cursor 30 is pointing at any of the controls. When it is determined that the mouse cursor 30 is pointing at one of the controls of the tool bar 34 , a tool tip 28 may be displayed if the mouse cursor 30 has remained pointing at the control for a sufficient period of time and the magnitude of the velocity of the mouse cursor is below a predetermined threshold. Hence, in the example shown in FIG. 2A, the message “Print” is displayed as a tool tip 28 , given that the mouse cursor 30 is pointing to the print button 32 .
Tool tips are provided not only for buttons on the tool bar 34 but are also provided for other types of controls. For example, as shown in FIG. 2B, a mouse cursor 38 points to a portion of a list box 40 that concerns the font which the user wishes to utilize. Accordingly, a tool tip 36 is displayed that includes the text “Font”. It is worth noting that the mouse cursor 38 changes from an arrow to a cross bar, since the cursor points to a portion of a list box that contains text rather than a button as in FIG. 2 A.
Tool tips are displayed using text output commands that are provided by the operating system 24 . Specifically, the ExtTextOut( ) function that is provided by the Microsoft Windows, version 3.1, operating system is used in the preferred embodiment. The format of this function is as follows:
BOOL ExtTextOut(hdc, nXStart, nYStart, fuOptions, lprc, lpszString, cbString, lpDx)
HDC hdc;
/* handle of device context
*/
int nXStart;
/* x-coordinate of starting position
*/
int nYStart;
/* y-coordinate of starting position
*/
UINT fuOptions;
/* rectangle type
*/
const RECT FAR* lprc;
/* address of structure with rectangle
*/
LPCSTR lpszString;
/* address of string
*/
UINT cbString;
/* number of bytes in string
*/
int FAR* lpDx;
/* spacing between character cells
*/
The hdc parameter of this function specifies a handle (i.e., a numerical identifier) for a device context. In this case, the device context specifies attributes that determine how the operating system interacts with the video display 18 . The nXStart parameter specifies the logical X coordinate at which the string of the tool tip message begins. Similarly, the nYStart parameter specifies the logical Y coordinate at which the string begins. The fuOptions parameter specifies the type of rectangle for the tool tip. The operating system 24 provides predefined data structures that specify rectangle types. In this case, the rectangle type is defined as a clipped rectangle. The lprc parameter is a pointer to a structure that holds a rectangle and the lpszString is a pointer to a structure that holds the textual string to be displayed in the tool tip. The cbString parameter specifies the number of bytes in the string and the lpDx parameter specifies spacing between character cells.
When the window procedure for the tool bar 34 receives a mouse message that indicates that the mouse cursor 30 (see FIG. 2A) is positioned over one of the controls of the tool bar 34 , a sufficient time has elapsed and the measured magnitude of the velocity of the mouse cursor 30 is below a predetermined threshold, the procedure determines the string that is to be displayed in the tool tip for the control to which the mouse cursor points. The address of this string is passed as the lpszString parameter to the ExtTextOut( ) function. This function then proceeds to draw the tool tip.
As the rectangle for the tool tip is a clipped rectangle, the background color may be specified. In the preferred embodiment of the present invention, the background color is yellow, as specified in red/green/blue (RG3) coordinates as (255, 255, 128). The size of the rectangle used for the tool tip is as follows: height equals the height of the text as specified by the font (i.e., the point of the font) plus 4, and length equals length of the text plus 4.
The tool tips are displayed at predefined locations relative to the controls. In general, tool tips are displayed centered under edit boxes and combo boxes and displayed relative to tool bar buttons at a position where the upper left-hand corner of the tool tip rectangle is 2 pixels to the left of the top left corner of the button and 15 pixels below the hot spot of the mouse 14 . Those skilled in the art will appreciate that tool tips may be displayed at other locations that are adjacent to the tools.
The discussion will now focus on the controls for determining when to display the tool tip. When the mouse cursor 30 is initially positioned to point to a tool bar control (i.e., the first time that the mouse cursor points to a control while it has been in the tool bar 34 ), the steps shown in FIG. 3A are performed. Initially, the window procedure for the tool bar 34 determines that the mouse cursor 30 points to a tool bar control (step 42 in FIG. 3 A). The application program 26 uses a timer to determine whether or not to display a tool tip. This timer may be a system-provided resource that is provided by the operating system 24 or may be a separate component that is provided by the application program 26 . The tip is displayed when the timer counts up to a preset trigger point and the magnitude of the velocity of the mouse cursor is an acceptable range. The timer trigger point is then set to 0.7 seconds (step 43 in FIG. 3 A). Those skilled in the art will appreciate that the choice of 0.7 seconds is not intended to be limiting of the present invention; rather, 0.7 seconds is a value used in the preferred embodiment of the present invention, which appears to empirically produce desirable results. The timer is then reset to zero seconds so that it can begin counting time.
As mentioned above, the magnitude of the velocity of the mouse cursor 30 is also used to control whether a tool tip is displayed. FIG. 3B shows the steps that are performed to determine the magnitude of velocity of the mouse cursor 30 . Initially, a mouse message is received (step 45 ). As discussed above, the mouse message includes the (X, Y) coordinates that specify the most recent position of the mouse cursor 30 . The coordinates are utilized to determine whether the mouse cursor 30 points to a tool bar control (step 46 ). As was discussed above, the system knows the locations of the tool bar controls within the tool bar 34 . This knowledge is used to determine whether the cursor points to a tool bar control. Mouse messages are generated periodically as the mouse cursor position changes. The time interval between mouse messages is reasonably fixed. Hence, the magnitude of the velocity of the mouse cursor 30 may be determined by comparing the (X, Y) coordinates for the most recently received mouse message with the coordinates from the last previous mouse message. The Euclidean distance between these two sets of coordinates may be calculated and, since the time interval is known, the magnitudes of velocity can then be calculated. However, since the time interval is fixed, there is no need to calculate the magnitude of velocity in each instance; rather, the measure of the distance traveled quantifies the magnitude of the velocity of the mouse cursor 30 . Accordingly, the preferred embodiment of the present invention merely measures the distance in pixels since the last mouse message as the velocity metric (step 47 ).
Those skilled in the art will appreciate that in alternative embodiments, the present invention may use the magnitude of the velocity as the measure that must exceed a predetermined empirically derived threshold. Alternatively, the vector value of the velocity may be utilized and compared to a vector threshold to determine whether a tool tip should be displayed or not. Moreover, those skilled in the art will appreciate that mouse cursor velocity may be used alone to determine whether a tool tip is displaced or, as employed in the preferred embodiment of the present invention, may be used in conjunction with time metrics to determine whether to display a tool tip or not. In addition, it should be realized that the controls described herein may be applied more broadly to any events that are triggered by measuring the time and velocity variables or velocity variable alone of a mouse cursor within a region of a user interface.
Whenever the mouse cursor 30 is positioned to point to a control within the tool bar 34 of the application program 26 , the steps shown in FIG. 4 are performed. Initially, the timer is initiated to run (step 48 ). When the timer expires (step 50 ), a determination is made whether the mouse cursor 30 is still pointing at the same control on the tool bar 34 (step 51 in FIG. 4) and whether the measured velocity metric has remained below an empirically derived threshold value during the time period (step 52 ). If both of these conditions are met, a tool tip is displayed as discussed above (step 54 in FIG. 4 ). In an alternative embodiment, the velocity metric is only measured as the timer expires rather than during the entire time interval. In addition to the tool tip being displayed, the timer trigger point is set to 0.1 seconds (step 56 ). The setting of the timer trigger point to a shorter duration (e.g., 0.1 seconds) facilitates browsing, so that the tool tips will be more quickly displayed when the user moves to an adjacent button or other control on the tool bar 34 . If either of the conditions is not met, a tool tip is not displayed and the timer is reset to 0 seconds (step 53 ).
The time duration for which the mouse cursor 30 remains pointing at a tool bar control and the measured magnitude of the velocity of the mouse cursor provide helpful indicators of the intent of the user. Empirical tests indicate that users typically will leave the mouse cursor pointing at a control for a time period greater than 0.7 seconds if they wish to use the control. Similarly, users tend to move the mouse cursor slowly over a tool bar control when they wish to utilize the tool bar control. In contrast, when users do not wish to use a tool bar control and are merely passing over a tool bar control, the users move the mouse cursor with a sufficient magnitude of velocity to indicate their intent.
FIG. 5 is a flow chart illustrating the steps performed when a mouse cursor is positioned to no longer point at a tool bar control (step 58 ). As soon as the cursor no longer points at the tool bar control, the tool tip is no longer displayed (step 60 ).
When the mouse cursor is positioned so as to no longer point within the tool bar, the steps shown in FIG. 6 are performed. In particular, when the cursor leaves the tool bar (step 62 ), the timer is cleared (step 64 ). The clearing of the timer allows the processing to be reinitiated when the cursor again returns to point to a location within the tool bar.
While the present invention has been described with reference to a preferred embodiment thereof, those skilled in the art will appreciate that various changes in form and detail may be made without departing from the intended scope of the present invention as defined in the appended claims. For example, the timing control described above relative to the preferred embodiment of the present invention may also be applied to graphical objects other than tools on a tool bar. Moreover, the timing parameters utilized by the preferred embodiment of the present invention are intended to merely illustrative. Other timing parameters may be utilized as well. Still further, pointing devices other than the mouse may be used to position the cursor.
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Time and velocity metrics are used to control when information about a graphical object to which a cursor points is displayed on a video display. The time metric is used to ensure that a non-negligible amount of time passes between the time at which the cursor initially points to the graphical object and the time at which the information about the graphical object is displayed on the video display. The time delay helps to eliminate such information being displayed inadvertently when the user quickly passes the cursor over graphical objects in the video display. In addition, the timing control facilitates the shortening of the delay when it appears that the user wishes to browse amongst several related graphical objects that are shown in the video display. For example, when it appears that the user wishes to browse tools on the tool bar, the delay is shortened. The velocity metric is used to determine the likelihood that the user intended to point to the graphical object and serves to minimize instances where undesired information about the graphical object is displayed.
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BACKGROUND OF THE INVENTION
This invention relates to an electrostatographic printing machine, and more particularly concerns an improved development system for use therein.
An electrostatographic printing process forms an electrostatic latent image and reproduces the image in viewable form on a copy sheet. The field of electrostatography includes electrophotography and electrography. Electrophotography employs a photosensitive medium to form, with the aid of electromagnetic radiation, the electrostatic latent image. Electrography utilizes an insulating medium to form, without the aid of electromagnetic radiation the electrostatic latent image. In both of the foregoing processes, the latent image is rendered viewable by the process of development, i.e. depositing particles thereon. Frequently, the particles are transferred from the latent image to a copy sheet, or, in some processes, the recording sheet on which the latent image is produced, may serve also as the copy sheet after the particles have been deposited thereon. In either of the foregoing cases, the resultant toner powder image deposited on the sheet is permanently affixed applying heat and/or pressure thereto. Hereinafter, an electrophotographic printing machine will be described as an illustrative embodiment of these processes.
In electrophotographic printing, the photoconductive member is charged to sensitize its surface. The charged photoconductive member is exposed to a light image of the original document being reproduced. Exposure of the sensitized photoconductive surface discharges the charge selectively in the irradiated areas. This creates an electrostatic latent image on the photoconductive surface corresponding to the original document being reproduced. Development of the electrostatic latent image recorded on the photoconductive surface isachieved by bringing developer material into contact therewith. Typical developer material comprises dyed or colored heat settable plastic powders, known in the art as toner particles, which are mixed with coarser carrier granules, such as ferro-magnetic granules. The toner particles and carrier granules are selected such that the toner particles require the appropriate charge relative to the electrostatic latent image recorded on the photoconductive surface. Thus, when the developer material is brought into contact with the latent image recorded on the photoconductive surface, the greater attractive force thereof causes the toner particles to transfer from the carrier granules and adhere to the electrostatic latent image. This concept was originally disclosed by Carlson in U.S. Pat. No. 2,297,691 and is further amplified and described by many related patents in the art.
With the advent of multi-color electrophotographic printing, it became highly desirably to reproduce color originals as color copies, or even black and white originals as color copies. Heretofore, the process of color electrophotographic printing required the utilization of filters to form successive single color light images from the colored original document. These single color light images record successive single color electrostatic latent images on the photoconductive surface. Each single color electrostatic latent image is developed with toner particles of a color complementary to the color of the filtered light image. These toner powder images, each of a different color, are transferred to the copy sheet in superimposed registration with one another. Thereafter, the multi-layer toner powder image is permanently affixed to the copy sheet. This produces a multi-color copy from a colored original document. The foregoing is fully described in U.S. Pat. No. 3,854,449 issued to Davidson in 1974.
Recently, it has been highly desirable to create a copy containing information in two or more colors. This may be achieved in high speed electrophotographic printing machines by masking selected portions of the original document or utilizing two or more original documents and reproducing the information contained therein on a common copy sheet in different colors. Different colors in the electrophotographic printing machine may be achieved by changing the color of the developer material employed in the development system. Thus, a black and white electrophotographic printing machine may be converted to a color printing machine simply by changing the color of the developer material contained within the development system. This requires cleaning the chamber storing the developer material so that no residual developer material remains therein prior to the introduction of the differently colored developer material. This is ncessary to prevent the contamination of the new charge of developer material by the residual developer material from the prior charge. Hence, it would be highly desirable to utilize a development apparatus containing a plurality of differently colored developer materials stored therein for subsequent application to the latent image automatically.
Accordingly, it is a primary object of the present invention to improve the multi-color capability of the development apparatus of an electrophotographic printing machine.
SUMMARY OF THE INVENTION
Briefly stated, and in accordance with the present invention, there is provided an apparatus for developing a latent image arranged to be recorded on a member with particles.
Pursuant to the features of the invention, the development apparatus includes a housing defining a chamber for storing a supply of particles therein. Means, disposed in the chamber of the housing, deposit particles on the latent image. Storing means store a plurality of differently colored particles remotely from the chamber of the housing. Means are provided for cleaning the particles from the chamber of the housing. Operator selectable means advance particles of a selected color from the storing means to the chamber in the housing.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects and advantages of the present invention will become apparent upon reading the following detailed description and upon reference to the drawings, in which:
FIG. 1 is a schematic elevational view depicting an electrophotographic printing machine incorporating the features of the present invention therein;
FIG. 2 is a fragmentary sectional elevational view illustrating the development apparatus employed in the FIG. 1 printing machine; FIG. 3 is a schematic perspective view showing the remote containers storing the differently colored developer material associated with the FIG. 2 development apparatus;
FIG. 4 is a schematic perspective view depicting the vacuum blower system for removing particles from the FIG. 2 development apparatus; and
FIG. 5 is a fragmentary elevational view illustrating the drive system of the FIG. 2 development apparatus.
While the present invention will hereinafter be described in connection with a preferred embodiment thereof, it will be understood that it is not intended to limit the invention to that embodiment. On the contrary, it is intended to cover all alternatives, modifications and equivalents as may be included within the spirit and scope of the invention as defined by the appended claims.
DETAILED DESCRIPTION OF THE INVENTION
For a general understanding of the illustrative electrophotographic printing machine, in which the features of the present invention may be incorporated, reference is had to the drawings. In the drawings, like reference numerals have been used throughout to designate identical elements. FIG. 1 schematically illustrates the various components of a printing machine incorporating the development system of the present invention. Although the development system is particularly well adapted for use in the FIG. 1 printing machine, it will become evident from the following discussion that it is equally well suited for use in a wide variety of electrostatographic printing machines and is not necessarily limited in its application to the particular embodiment shown herein.
Inasmuch as the art of electrophotographic printing is well known, the various processing stations employed in the FIG. 1 printing machine are only shown schematically and their operation described briefly with reference thereto.
As illustrated in FIG. 1, the electrophotographic printing machine employs a belt 10 having a photoconductive surface. By way of example, belt 10 may be made from a selenium alloy deposited on a conductive substrate, such as aluminum. Belt 10 moves in the direction of arrow 12 to advance sequentially through the various processing stations disposed about the path thereof. Rollers 14, 16 and 18 support belt 10. A drive mechanism, i.e. a suitable motor, is coupled to roller 14 so as to advance belt 10 in the direction of arrow 12.
Initially, a portion of belt 10 passes through charging station A. At charging station A, a corona generating device, indicated generally by the reference numeral 20, charges the photoconductive surface of belt 10 to a relatively high substantially uniform potential. A suitable corona generating device is described in U.S. Pat. No. 2,836,725 issued to Vyverberg in 1958.
Thereafter, the charged portion of belt 10 rotates through exposure station B. At exposure station B, an original document 22 is placed upon transparent platen 24 face down. An illumination system flashes light rays upon original document 22 to produce image rays corresponding to the informational areas contained therein. The image rays are projected by means of an optical system 26 onto the charged portion of photoconductive belt 10. In this manner, the charged photoconductive surface of belt 10 is exposed to a light image of the original document. Exposure of the charged portion of the photoconductive surface to the light image discharges the charge thereon in accordance with the intensity of the light image projected thereto. In this way, an electrostatic latent image is recorded on the photoconductive surface of belt 10.
The electrostatic latent image recorded on belt 10 is advanced to development station C. At development station C, developer unit 28 has a plurality of magnetic brushes 30, 32, 34 and 36 disposed in housing 38 to move developer material adjacent to the electrostatic latent image recorded on belt 10. The developer mix comprises carrier granules having toner particles adhering thereto. Generally, the carrier granules are formed from a ferro-magnetic material while the toner particles are made from a heat settable plastic. In a typical magnetic brush system, a chain like array of developer mix extends in an outwardly direction from each magnetic brush to contact the electrostatic latent image recorded on the photoconductive surface. The latent image attracts electrostatically the toner particles from the carrier granules forming a toner powder image on belt 10.
Developer unit 28 is adapted to deposit toner particles of a pre-selected color onto the electrostatic latent image recorded on belt 10. Conduit 38 is one of a plurality of conduits for delivering operator selectable developer material of different colors from remote storage containers. Tube 40 is coupled to a vacuum blower system for removing developer material from developer unit 28 so as to enable differently colored developer material to be introduced therein via conduit 38. The detailed structure of developer unit 28 will be discussed hereinafter with reference to FIGS. 2 through 5, inclusive.
After development, the toner powder image is transported by belt 10 to transfer station D. Transfer station D is located at a point of tangency on belt 10 as it moves around roller 14. Transfer roller 42 is disposed at transfer station D with the copy sheet being interposed between transfer roller 42 and belt 10. Transfer roller 42 is electrically biased to a suitable magnitude and polarity so as to attract the toner powder image to the surface of the copy sheet in contact therewith. After transferring the toner powder image to the copy sheet, conveyer 44 advances the copy sheet in the direction of arrow 46 to fixing station E.
Fixing station E includes a fuser assembly indicated generally by the reference numeral 48. Fuser assembly 48 has a heated fuser roll engaging a backup roll. The surface of the copy sheet having the toner powder image thereon passes between the fuser roll and backup roll with the toner powder image contacting the fuser roll. In this manner, the toner powder image is permanently affixed to the copy sheet. After fusing, conveyers 50 and 52 advance the copy sheet to catch tray 54 for subsequent removal therefrom by the machine operator.
Referring now to the sheet feeding apparatus, sheet transport 56 advances, in seriatum, successive copy sheets from stack 58 or, in lieu thereof, stack 60. The machine programming permits the operator to select the desired stack from which the copy sheet will be advanced. In this way, the selected copy sheet is advanced to transfer station D where the toner powder image is transferred thereto.
It is believed that the foregoing description is sufficient for purpose of the present application to illustrate the general operation of an electrophotographic printing machine incorporating the features of the present invention therein. Referring now to the specific subject matter of the present invention, FIGS. 2 through 5, inclusive, depict the development apparatus employed in the FIG. 1 of the printing machine.
Turning now to FIG. 2, there is shown the detailed structure of developer unit 28. As shown therein, housing 62 has a chamber 64 for storing a supply of developer mix therein. Paddle wheel 66 includes a substantially tubular member 68 having vanes 70 extending outwardly in a radial direction therefrom. Paddle wheel 66 rotates in the direction of arrow 72 to advance the developer material to magnetic brush 30. Magnetic brushes 30, 32, 34 and 36 form a blanket of developer material moving in the direction of arrow 12 and positioned closely adjacent to the latent image recorded on belt 10. In this manner, the toner particles are attracted electrostatically from the carrier granules to the latent image in image configuration. Each of the developer rollers rotate in the direction of arrows 74, 76, 78 and 80, respectively. After the first original document has been reproduced in the first color, for example, black, the next successive original document may be reproduced in a second or different color on the same or another copy sheet. Changing developer material colors requires s cleaning the initial charge of developer material from chamber 64 of housing 62.
Mounted for rotation within chamber 64 of housing 62 are four magnetic brush developer rollers 30, 32, 34 and 36 positioned with their axis parallel with one another below belt 10. Each magnetic brush developer roller comprises an outer cylinder or tubular member 82 made of a non-magnetizable material and extending almost the length of housing 62. Tubular members 82 are mounted for rotation in housing 62. Disposed within each tubular member 82 is a bar magnet 84. The only distinction between each magnetic brush developer roller is the polarity of the bar magnet. Thus, magnetic brush developer roller 30 has the polarity of bar magnet 84 oriented in one direction, while magnetic brush developer roller 32 has the polarity of bar magnet 84 oriented in the opposite direction. Magnetic brush developer roller 34 has the polarity of bar magnet 84 oriented in the same direction as magnetic brush developer roller 30. Magnetic brush developer roller 36 has the polarity of bar magnet 84 oriented in the same direction as magnetic brush developer roller 32. As shown in FIG. 2, the peripheral walls of tubular members 82 are relatively close to each other. During a development cycle, tubular members 84 rotate in unision with the respective magnetic bars 84 being held substantially stationarily. The magnetic field emanating from bar magents 84 causes the developer mix to be attracted to the upper surface of tubular members 82. As tubular members 82 rotate in the direction of arrows 74, 76, 78 and 80, respectively, the developer mix advances across the upper surface of each tubular member 82. In this manner, the bristles of developer mix extend in an outwardly direction from housing 62 in contact with the electrostatic latent image recorded on belt 10. After passing magnetic brush developer roller 36, the remaining developer mix returns to chamber 64 of housing 62.
In cleaning developer unit 28, the developer material is drained from chamber 64 of housing 62 through tube 40 by a vacuum blower system, such as is shown in FIG. 4. The vacuum blower system will be discussed hereinafter in greater detail with reference thereto. Screen 86 is disposed in the opening of tube 40 to prevent contaminants from passing with the developer material into the vacuum blower system. After the developer mix of the first color is drained from chamber 64 of housing 62, a new color developer mix is introduced therein. Conduit 38 is one of a plurality of conduits in communication with housing 62 for introducing developer material of a different color therein. Referring now to FIG. 3, the system for advancing differently colored developer mix into chamber 64 of housing 62 will be described. Advancing system 88 includes a conduit 38, motor 90 and storage container 92. Advancing systems 94 and 96 are substantially identical to advancing system 88 with the only distinction being the color of the developer mix contained within the storage container thereof. Hence, only advancing system 88 will be described hereinafter in detail. Conduit 38 couples storage container 92 to chamber 64 of housing 62. Conduit 38 is flexible and includes an outer tube 98 (FIG. 2) made preferably of Nylon, having a helical spring 100 mounted in bore 102 thereof. (FIG. 2). Helical spring 100 is connected to motor 90. Tube 98 has one aperture in communication with storage container 92 and another aperture in communication with chamber 64. In this way, developer mix from the storage container 92 descends into bore 102 and is advanced by helical spring 100 during the rotation thereof by motor 90. Hence, energization of motor 90 rotates helical spring 100 to advance developer mix from storage container 92 into chamber 64 of housing 62. Thus, the operator may select the desired color of developer material by energizing the appropriate motor associated with the corresponding developer material storage container. For example, energization of advancing system 82 could furnish blue developer material to chamber 64 of housing 62. However, energization of advancing system 94 could furnish red developer material, while energization of advancing system 96 could furnish green developer material thereto. Although three systems for advancing developer material of different colors to chamber 64 of housing 62 have been shown, one skilled in the art will appreciate that any number may be employed and only the size of the developer unit constrains the number of advancing systems associated therewith.
Referring now to FIG. 4, the system for removing the developer material from chamber 64 of housing 62 will be described hereinafter in greater detail. As shown, tube or duct 40 is coupled to housing 62. Motor driven blower or fan 104 coupled to duct 40 has an impeller mounted for rotation therein and is arranged to remove air and developer mix from chamber 64 of housing 62 through duct 40 and out again through duct 106 into containers 108. Activation of blower 104 removes the developer mix from chamber 64. The developer mix is sucked through the system and stored in containers 108. One container is associated with a corresponding color of developer material. This prevents intermixing of the different colored developer material enables the developer material to be reclaimed for subsequent reuse. After cleaning chamber 64 of housing 62, a new charge of developer mix, in a new color, may be introduced into chamber 64 for subsequent use in the printing machine to produce differently colored copies.
With continued reference to the drawings, FIG. 5 depicts the drive system associated with developer unit 28. The drive system includes a motor 110, a pulley 112 secured to the motor shaft, a smaller pulley 114 also secured to the motor shaft and timing belts 116, 118 for connecting pulleys 112 and 114, respectively, to the rotary components. Specifically, belt 116 is drivingly engagable with pulleys 120 and 122 mounted on the drive shafts of tubular members 76 of magnetic brushes 30 and 32, respectively. An idler pulley 124 and pulleys 126 and 128 secured to the drive shafts of tubular members 176 of magnetic brushes 34 and 36, respectively, are also in driving engagement with belt 116. Belt 118 connects drive pulley 114 with pulley 130 secured to the shaft of paddle wheel 66. This insures that paddle wheel 66 and tubular member 82 move in unision with one another. In this manner, tubular members 82 rotate in the direction of arrows 74, 76, 78 and 80, respectively. Similarly, paddle wheel 66 rotates in the direction of arrow 72.
In recapitulation, the development apparatus of the present invention includes a plurality of storage containers located remotely from the chamber of the developer housing. Each storage container has a supply of differently colored developer mix. Activation of a vacuum blower system removes the developer mix contained within the chamber of the developer housing. This permits an advancing system to move differently colored developer mixes into the chamber of the developer housing. In this manner, copies may be reproduced in different colors or have portions thereof color high-lighted.
It is, therefore, evident that there has been provided in accordance with the present invention, an apparatus for developing an electrostatic latent image in any one of a plurality of different colors. The apparatus of the present invention fully satisfies the objects, aims and advantages hereinbefore set forth. While this invention has been described in conjunction with a specific embodiment thereof, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art. Accordingly, it is intended to embrace all such alternatives, modifications and variations that fall within the spirit and borad scope of the appended claims.
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An apparatus arranged to develop a latent image recorded on a member with particles stored in the chamber of the housing. A plurality of differently colored particles are housed remotely from the chamber. Particles of a selected color are advanced to the chamber so as to be deposited on the latent image.
The foregoing abstract is neither intended to define the invention disclosed in the specification, nor is it intended to be limiting as to the scope of the invention in any way.
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BACKGROUND OF THE INVENTION
1. Field of the Invention:
This invention relates to a latch mechanism and more particularly to a selectively operable latch mechanism that can be combined with an unbalance-sensitive latch release mechanism to provide a means for positively locking the access door of a centrifugal extractor during an extraction operation and to means for unlocking said access door responsive to an unbalance condition.
2. Description of the Prior Art:
The prior art shows a continuing search for a control system for a rotating apparatus, such as a laundry appliance, to insure safe operation of the apparatus. Previous work in the appliance field also shows it to be desirable to prevent access to the fabric container of a centrifugally operable washing machine during the extraction operation. Early systems for achieving this desired objective disclose switching means responsive to the opening of the access door for de-energizing the drive system so that the container is not driven while the access door is in the open position. Also shown in prior art are control systems including solenoid or relay operated lid switches controlled by sequential control means so that the solenoid or relay is energized for locking the access door upon energization of the drive system for the extraction operation to avoid or prevent access to the spinning container. Apparatus for solving or otherwise obviating the problems associated with a mechanical, selectively operable normally disengaged latch mechanism is not, however, shown in prior art.
SUMMARY OF THE INVENTION
It is an object of the instant invention to provide a positive latch mechanism that is mechanically operable at predetermined portions of a machine cycle.
It is a further object of the instant invention to provide a positive latch release mechanism responsive to an unbalance condition in the apparatus.
It is a further object of the instant invention to provide access to the fabric container in event of said unbalance condition.
Briefly, the instant invention achieves these objects in a normally disengaged latch mechanism that includes mechanically actuated connecting means operatively disposed between a sequential control means and latching means.
Operation of the device and further objects and advantages thereof will become evident as the description proceeds and from an examination of the accompanying three page of drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
The drawings illustrate a preferred embodiment of the invention with similar numerals referring to similar parts throughout the several views, wherein:
FIG. 1 is a partial front view of an automatic washing machine showing the cabinet top, control panel and dial.
FIG. 2 is a fragmentary sectional view through the control panel and cabinet top portions generally taken along Section Line 2--2 of FIG. 1 showing part of the unbalance release mechanism.
FIG. 3 is a view similar to the lower portion of FIG. 2 showing the unbalance release mechanism in the unbalance condition.
FIG. 4 is a fragmentary sectional view through the cabinet top taken generally along a horizontal plane indicated by Section Line 4--4 of FIG. 1 showing the latch mechanism and also showing the cable adjustment and cornering device.
FIG. 5 is a view similar to FIG. 4 showing elements in the unbalance condition. FIG. 6 is a view taken generally along Section Line 6--6 of FIG. 2 generally showing cam surfaces, latch actuator, unbalance release mechanism, actuating means and unbalance mechanism.
FIG. 7 is similar to the lower portion of FIG. 6 showing elements in the unbalance condition.
FIG. 8 is shown between FIGS. 1 and 2 and is a fragmentary view taken generally along Section Line 8--8 of FIG. 4 showing the latch catch and the latch stop.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to the drawings, there is shown in FIG. 1 a partial view of an automatic washing machine including a cabinet 10. The cabinet 10 includes a control panel 11 accommodating various control members such as sequential control means or timer indicated by numeral 13 in FIG. 2 and actuatable by a dial 14.
Mounted within the cabinet 10, as in FIG. 2, is a tub assembly 15 nutationally supported and within which is journalled a rotatable clothes basket 17. The tub assembly 15 includes a tub top cover 16 on which is fixed a bumper 19 that moves with the tub assembly 15 and tub top cover 16. The position of the bumper 19 with respect to the cabinet 10 therefore is determined by the gyration of the tub assembly 15 when the washing machine is energized in the extraction part of the series of operations. The entire washing machine is supported on a frame (not shown).
The cabinet structure 20 includes an access opening 21 through which fabrics may be inserted or removed from the rotatable clothes basket 17. The access opening 21 is closed by an access door 23. The door 23 is pivoted about a fulcrum 24 spaced a short distance from the rear end of the door 23. The rear end 25 of the door 23 functions as a lever with respect to the fulcrum 24 for engaging the unbalance mechanism 26.
The unbalance mechanism 26 is attached to the cabinet top 29 as shown in FIGS. 2 and 3 by means of a pair of screws 27 extending through the cabinet top 29 and threading into the molded plastic body of the unbalance mechanism frame 30.
A plunger 31 is slidingly supported within the frame 30 of the unbalance mechanism. The front end of the plunger 31 is in the form of a projecting nose 33 extending through the cabinet top 29. The plunger 31 further includes, as best shown in FIGS. 6 and 7, a pair of spaced apart side rails 34 joined at the front and rear. The rear end of the plunger 31 includes a downwardly extending flange 35. The plunger 31 also includes an undercarriage 36 for pivotally supporting the unbalance actuator 39 on the plunger 31.
The unbalance actuator 39 is pivotally supported by the plunger undercarriage 36 and includes a rear end 40 engageable with the bottom edge 41 of the rear flange 35 of the plunger 31. The unbalance actuator 39 further includes a depending lever end 43 extending substantially downwardly from the pivot connection 44 between the unbalance actuator 39 and the plunger 31. The depending lever 43 of the unbalance actuator 39 is positioned for engagement by the bumper 19 upon excessive gyration of the tub assembly 15.
A biasing spring 45 is disposed between the unbalance mechanism frame 30 and the unbalance actuator 39. This angularly disposed biasing spring 45 provides upwardly and forwardly directed components of biasing force. The upwardly directed component of force maintains the rear end 40 of the unbalance actuator 39 against the plunger rear flange 35 or against the lower side of a switch plunger 46. The forwardly directed component of force biases the actuator 39 and plunger 31 in a forward direction to maintain engagement of the plunger nose 33 with the access door 23.
A switch 49 is attached to the cabinet top 29 by a pair of threaded members 50. This switch 49 includes a pair of connector terminals 51 by which the switch 49 may be connected into the circuitry of the drive motor. The switch plunger 46 is biased to the left so that, in the absence of an externally applied force to the right, the plunger 46 will automatically return under the spring biasing to a normal position.
The unbalance mechanism 26 operating in cooperation with the access door 23 causes the plunger 31 of the unbalance mechanism 26 to bias the switch plunger 46 to the right as shown in FIG. 2. In this position, the contacts of the switch are closed and the circuit is completed across the terminals 51 for energizing the drive motor.
The construction and operation of the unbalance mechanism 26 are more clearly and specifically shown in the following patent, which is assigned to the assignee of the instant invention: Mellinger, U.S. Pat. No. 3,488,463 issued Jan. 6, 1970.
Referring to FIG. 2, the sequential control device or timer mechanism 13 is mounted on the rear of the control panel 11 with the operating shaft 53 extending through the control panel 11. Mounted on this operating shaft 53 is a dial 14 which indicates the progression of the washer through its series of operations. As best shown in FIG. 6, the rear of the dial 14 has cam surfaces 54 that correspond to the periods of high speed spinning for water extraction. A latch actuator 55 is pivotally mounted to the control panel 11 behind the dial 14 with the upper portion 56 engaging the cam surface 54 of the dial 14. The lower portion 59 of the latch actuator 55 is angularly displaced to the left and downwardly toward the cabinet top 29. The lower portion 59 has a rectangular notch 60 near the tip to receive the first looped end of the cable 61.
Mounted to the cabinet top 29 to the right of the switch 49, as in FIGS 6 and 7, is a pivot bracket 63. This bracket 63 has an extending arm which in turn has a stud-like projection 62 on which is pivotally mounted a bell crank shaped unbalance-sensitive latch release member 64. The first arm 65 of the bell crank is normally engaged with a downwardly projecting lip 66 of the unbalance mechanism frame 30 and juxtaposed to the rear end 40 of actuator 39 as in FIG. 6. This first arm 65 is biased into this engaging position by a spring 69. One end of this spring 69 is inserted into a through holes 67 on the second arm 70 with the other end attached to a notch 68 in the fixed cabinet top panel 29. The second arm 70 of the crank has two molded slots 71 with the remaining material between the slots 71 acting as a pulley-like cable guide 73 for changing the cable 61 direction.
From the latch actuator 55, the cable 61 travels around the pulley-like guide 73 of the unbalance-sensitive latch release member 64 behind the cabinet top 29 to the left side of the washing machine to a point, as in FIGS. 4 and 5, where a right angle corner must be negotiated to continue the path to the second connection position. At this cornering point a pivotally mounted cable adjustment and corning device 74 is mounted to the underside surface of the cabinet top 29 by means of a self-threading member (not shown). This cornering device 74 has an extending arm with a molded arcuate groove to serve as a cable cornering guide 75. The cable 61 coming from the pulley-like cable guide 73 of the unbalance-sensitive latch release member 64 is placed into the cable cornering guide 75 thereby turning the corner and continuing toward the front of the washing machine. Located between the pivot point 76 and the cable cornering guide 75 is a molded pilot hole 77 for receiving a threaded fastener 79. When this threaded fastener 79 is engaged with the pilot hole 77 and turned, the fastener 79 extends through the body of the cable adjustment and cornering device 74 and contacts the cabinet top wall 80. As the fastener 79 is further turned, the cable adjustment and cornering 74 is forced to pivot thereby tightening or loosening the cable 61 to achieve correct operating tension.
The latch mechanism for latching the access door 23 in the closed position relative to the cabinet top 29 includes, as in FIGS. 4 and 5, an access door mounted latch assembly and a cabinet top mounted latch assembly.
The access door 23 mounted latch assembly as best shown in FIG. 5 comprises a housing 78 which is secured by a pair of screws and provides a pair of slots 82 for slidably supporting a latch stop 81. A leaf spring 87 biases the latch stop 81 toward the left for engagement, as shown in FIGS. 4 and 8, with the bell crank shaped latch catch 90 of the cabinet top cover mounted portion. The latch stop 81 has a downwardly facing ramp 88, as shown in FIG. 8, which allows the latch stop 81 to override the latch catch 90 by sliding to the right in the slots 82 to allow closing of the access door 23 should the cabinet latch catch 90 be in a locking position as in FIG. 4.
The cabinet top mounted latch portion consists of three elements: a mounting element, a bell crank shaped latch member, and a biasing spring. The mounting element 83 is secured to the cabinet top 29 through a pair of legs 84 and includes a concavely radiused pivot point 85 and an angularly extending arm 86. The bell crank shaped latch member 99 includes a transversely extending round shaft 89 mating with the concavely radiused pivot point 85 of the mounting element 83 and further includes two arms disposed generally at right angles to each other. The first of the two arms defines a latch catch 90 and extends through a slot 91 in the cabinet top 29 engage with the latch stop 81. The second arm 93 provides a connecting point 94 for the second looped cable end and provides a connecting point 95 for a hook end of the biasing spring 96 to control movement of the latch member 99. The biasing spring 96 is hooked between the second arm 93 of the latch member 99 and the extending arm 86 of the latch mounting element 83. This biasing spring 96 serves to maintain the latch catch 90 in the non-locking position as in FIG. 5 when the clothes basket is not spinning.
In normal operation when the sequence control device 13 enters a portion of the predetermined series of operations that requires the clothes basket to spin at high speed, the upper portion 56 of the latch actuator 55 climbs the cam surface 54 to a position shown generally in FIG. 6 which forces the upper portion 56 radially outward. At the same time, the lower portion 59 moves inward, or to the left in FIG. 6, pulling the attached cable 61 which moves relative to the pulley-like guide 73 and places tension on the cable system. The cable pulls the second arm 93 of the bell crank shaped latch member 99, as in FIG. 5, causing it to pivot clockwise and move latch catch of the first arm 90 into the locking position as in FIG. 4 and to thereby place added tension on the biasing spring 96. After the high speed spin operation the latch actuator 55 drops off the cam surface 54, releasing the cable tension, and allowing the biasing spring 96 of the latch member to restore the latch member to the non-locking position of FIG. 5.
If during the high speed spinning, a predetermined unbalance condition causes the tub assembly 15 to excessively gyrate, the bumper 19 mounted on the tub cover 16 is moved so as to engage the depending lever 43 of the unbalance mechanism 26 and pivot the actuator 39 to the position of FIG. 3 so that the rear end 40 of the actuator 39 is moved downwardly. This motion releases plunger 46, causes de-energization of the apparatus, and effectively latches the rear end 40 of the actuator under the switch plunger 46. The downward movement of the actuator 39 also causes the unbalance-sensitive latch release member 64 to pivot counterclockwise through engagement with arm 65 for moving the second arm 70 toward the machine center line. The pivot action causes the cable 61 that is passed around the pulley-like guide 73 portion of the second arm 70 to lose tension, and thereby enable the biasing spring 96 of the cabinet mounted latch member to move the latch element 90 into an unlocked position, as in FIG. 5. The lid is thus unlocked to permit access to the clothes basket for manual redistribution of the clothes within the basket to eliminate the conditions causing the unbalance.
The apparatus will be maintained de-energized until the unbalance mechanism 26 is reset. The resetting is accomplished automatically upon the opening of the access door 23 by the operator which is a natural part of the redistribution of the clothing. Opening of the access door 23 releases the plunger 31 so that the plunger 31 and actuator 39 move axially to the left under biasing force of the spring 45 to position the plunger 31 in its forward position and to position the actuator rear end 40 in substantial alignment with the switch plunger 46. The unbalance mechanism 26 is now operable for re-energizing the extractor apparatus upon closing of the access door 23. As the unbalance mechanism 26 is reset, the spring biased first arm 65 of the unbalance-sensitive latch release member 64 moves with the actuator 39 as it moves upwardly into alignment with plunger 46. Cable tension is thus restored and the latch catch 90 is returned to the locked position.
It is therefore seen that the instant invention provides clear and distinct advantages over latch mechanisms shown in the prior art. Latching is automatically and positively achieved when the clothes basket is spinning. Also, access to the clothes basket in case of an unbalance condition is provided without any physical requirements on the part of the operator.
In the drawings and specification there has been set forth a preferred embodiment of the invention and although specific terms are employed these are used in a generic and descriptive sense only and not for purposes of limitation. Changes in form and the proportion of parts, as well as the substitution of equivalents are contemplated, as circumstances may suggest or render expedient, without departing from the spirit or scope of this invention as defined in the following claims.
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A selectively operable latch mechanism for the access door of an apparatus having a rotatable member provides a positive latching of the access door when the rotatable member is operating. An associated unbalance-responsive mechanism will unlatch said access door when an unbalance condition has occurred and will stop the rotation of said rotatable member.
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FIELD OF THE INVENTION
[0001] This invention relates to decorative finishes and more particularly to a process for creating a plated plastic article having a decorative relief pattern.
BACKGROUND OF THE INVENTION
[0002] Decorative chrome finishes on plastic components have long been popular in automotive, appliances, teletronics, and household applications. While chrome plated plastic articles having decorative relief patterns are known and desired, it is expected that the demand for more delicately textured or patterned chrome finishes will increase in the near future. A textured chrome finish on a plastic component can be achieved by applying a chrome plating over a pre-textured molded plastic component. However, this practice is not economically acceptable in the initial marketing phase of potential products, and is unacceptable for certain low volume or specialty products, because pre-textured molds are relatively expensive. Further, it is extremely difficult to consistently produce delicate and/or intricate textured patterns in a plastic molding process. In addition, because of the thicknesses of the multiple layers required for chrome plating a plastic substrate, much of the original detail in the molded relief pattern may be lost during the plating process.
[0003] U.S. Pat. Nos. 3,843,763 and 3,869,535 disclose methods for modifying embossing rollers, plates or dies by subjecting machine engraved or electroformed roller to a combination of plating steps. The embossed roller is first subjected to a bright metal plating step with a metal characterized by a high or medium leveling effect to produce a combined brightening and smoothing effect on the roller. This step is followed by a second plating step used as a finishing coating for the roller. The second plating is suitably achieved using a metal having a relatively lower leveling effect such as chromium or nickel. The second plating step provides a hard coating surface which is resistant to corrosion and erosion while at the same time enhancing the textured pattern of the end desired product. The disclosed process starts with a substrate having the desired relief pattern.
[0004] U.S. Pat. No. 4,278,739 discloses a method of metallizing materials by coating a substrate material with a hydrophilic composite material, electrolessly metal plating the hydrophilic composite material with a metal to render the surface conductive, and electroplating a metal onto the conductive surface. The method is said to be useful for producing metallized forms, embossing plates for reproduction of grains and textures, and decorative coatings for substrate materials.
[0005] U.S. Pat. No. 4,600,480 discloses a method for plating selected surfaces of a plastic substrate without plating other selected surfaces. The disclosed method involves electrolessly plating the substrate to provide an electroless metal layer over all of the first selected surfaces and at least a portion of second selected surfaces, mounting the substrate on an electroplating rack so that the current density at the second selected surfaces is lower during electroplating than at the first selected surfaces, whereby the substrate is electroplated to provide intermediate metal layers which extend over at least all of the first selected surfaces, and then electroplating with a final metal different from the metals of the electroless and intermediate layers at a voltage whereby the final metal deposits over the first selected surfaces but not over the second selected surfaces. The electroplated substrate is then immersed in a stripping solution which dissolves the electroless and intermediate metals but not the final metal.
[0006] U.S. Pat. No. 4,820,553 discloses a process for conditioning surfaces of a polyester or polyamide material for electroless plating. The method comprises exposing surfaces of the polyester and/or polyamide material to a composition which comprises a solvent system containing water, a water-soluble organic solvent and solvated hydroxyl ions to etch the surface of the substrate to improve adhesion of a metal coating with the substrate.
[0007] U.S. Pat. No. 6,489,034 discloses a method of applying a metal onto a copper layer by steps of stabilizing a surface of a copper layer by applying an oxide layer to the copper layer, and vapor depositing a metal, such as chromium, directly onto the oxide surface of the copper layer.
[0008] There remains a need for improved processes for preparing textured decorative plastic components, especially techniques that allow preparation of delicately, textured patterned finishes which have fine, crisp, clean lines and intricate details. Especially needed is a process of this type which is relatively inexpensive and/or provides greater flexibility in the preparation of low cost plastic articles having a textured finish.
SUMMARY OF THE INVENTION
[0009] The invention provides an economically acceptable process for making plastic components having delicately textured or patterned finishes, and provides a flexible technology for producing decorative patterns having fine, crisp, clean lines and intricate details on a variety of plastic parts having a metal layer. The process includes steps of electroplating a layer of etchable metal on a surface of a plastic article; typically preventing the etchable metal surface from tarnishing; etching a desired relief pattern on the layer of etchable metal; typically cleaning and activating the surface of the relief patterned etched metal layer; and depositing a finish layer on the relief patterned etched metal layer.
[0010] These and other features, advantages and objects of the present invention will be further understood and appreciated by those skilled in the art by reference to the following specification and claims.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
[0011] In accordance with an embodiment of the invention, a process for preparing a plastic article having a desired relief pattern in a plated surface generally involves depositing a relatively thick layer of etchable metal on a surface of the article; forming the desired relief pattern on an exposed surface of the etchable metal layer; and depositing a finish layer over the relief pattern.
[0012] Generally, there are several preparation steps prior to the step of electroplating a layer of etchable metal on the surface of the article. Typically, an electrically conductive electroless coating is provided prior to electroplating of the layer of etchable metal. Electroless coating generally involves steps of cleaning and etching the substrate, neutralizing the etched surface, catalyzing the neutralized surface (e.g. in a solution that contains palladium chloride, stannous chloride and hydrochloric acid), followed by immersion in an accelerator solution (which is either an acid or a base), and forming a metallic coating on the activated substrate. The surface of the substrate is typically conditioned by cleaning with a detergent solution and etched by dipping the substrate in an etchant (e.g., a mixed solution of chromic acid and sulfuric acid). The metallic coating may be deposited on the activated substrate by immersing the substrate in a chemical plating bath containing nickel or copper ions and deposing the metal thereon from the bath by means of the chemical reduction of the metallic ions. The resulting metallic coating is useful for subsequent electroplating because of its electrical conductivity. It is also conventional to wash the substrate with water after each of the above steps. Other suitable techniques for pretreating a plastic substrate to provide an electrically conductive coating to render the substrate receptive to electroplating operations are well known in the art, and may be employed prior to electroplating a layer of etchable metal on a surface of the article in accordance with the principles of this invention.
[0013] Typical plastic materials that have been rendered receptive to electroplating, and which may be subsequently electroplated include acrylonitrile-butadiene styrene (ABS) resins, polyesters, polyethers, polyacrylics, polycarbonates, polyamides, polyolefins, polyvinylchloride, polycarbonate (PC) resins/ABS alloy polymers and phenol-formaldehyde polymers. The process of this invention may be applied to these and other plastics.
[0014] After electroless plating or coating of the substrate with an electrically conductive material, the layer of etchable metal is electroplated onto the article. In order to provide a visually perceivable and aesthetically acceptable relief pattern, a relatively thick layer of etchable metal is electroplated onto the treated surface of the plastic article. A suitable thickness of the etchable metal layer is typically from about 50 to about 500 micrometers. A thinner layer may be utilized, although this may limit the ability to provide a visually discernible, aesthetically acceptable relief pattern. Greater thicknesses may also be used, but are generally unnecessary to achieve an aesthetically acceptable textured or graphical relief pattern. While various metals may be used for electroplating a suitable etchable metal layer, including nickel, tin, zinc, cobalt, etc., a copper electroplate is preferred because of its relatively low cost and excellent etchability properties. Specifically, it is possible to chemically, mechanically (e.g., such as with sand blasting), or ablatively (e.g., such as with a laser) etch a desired relief pattern into a copper surface to produce relatively sharp, precise relief structures.
[0015] While it is not necessary, the layer of etchable metal that is subsequently etched to form the desired relief pattern may be electroplated over any number of previous layers. Accordingly, as used herein, electroplating a layer of etchable metal on the article may be achieved by either electroplating directly on the plastic article treated with an electroless coating, or on one or more layers of material deposited on the surface of the plastic article.
[0016] Before etching the relief pattern into the layer of etchable metal, it is desirable to first activate the exposed surface of the etchable metal layer in order to form a thin layer of preservative film on the etchable metal surface. This may be achieved by contacting the exposed surface of the etchable metal layer with an activating solution comprising from about 1% to about 10% by weight hydrogen peroxide (H 2 O 2 ) and from about 5 to about 20% by volume of sulfuric acid (H 2 SO 4 ). A suitable contact time is from about 5 seconds to about 60 seconds, and contacting of the exposed surface of the etchable metal layer with the activating solution may be performed at ambient conditions (e.g., normal atmosphere pressure and normal facility or room temperatures). Before etching the etchable metal layer, it may be desirable to contact the exposed surface of the etchable metal layer with an aqueous corrosion inhibiting solution to prevent the etchable metal surface from tarnishing. The expression “contacting” as used herein, unless otherwise indicated, refers to immersion, spraying or any other treatment that provides appropriate contact of the surface with a liquid treatment composition. A suitable contact time of the exposed surface of the etchable metal layer with the corrosion inhibitor solution is from about 1 second to about 10 minutes. Examples of corrosion inhibiting agents that may be employed in an aqueous corrosion inhibitor include benzotriazole, 2-mercaptobenzimidazole, 2-mercapatobenzothiazole, 2-mercaptobenzoxazole, their derivatives, or a combination of these corrosion inhibiting agents. Such agents are typically present in the aqueous corrosion inhibitor solution at a concentration of at least 10 mg/L.
[0017] Any of various etching techniques that are well known may be employed for etching the desired relief pattern into the surface of the etchable metal layer. In the case of chemical etching, the exposed surface of the etchable metal layer is coated with a material (typically a synthetic polymer material) that is either chemically resistant to the etchant used for etching the metal, or which can be rendered chemically resistant, such as by cross-linking. Any of various masking techniques known in the art may be employed, including wax masking, etchable film masking, brush-coat masking, spray-coat masking, immersion-coat masking, UV cure photoresist masking, etc. After the coating has been applied to the exposed surface of the etchable metal layer, sections of the coating are removed to expose sections of the underlying etchable metal layer. The patterned coating or mask and the exposed sections of the surface of the etchable metal layer are contacted with a chemical etchant that removes (e.g., dissolves) metal at the surface of the etchable metal layer, thereby forming a relief pattern into the metal that corresponds with the mask pattern. Conventional photoresist materials may be used for preparing the patterned coatings or masks. Typically, precise patterns can be formed into the photoresist materials by selective exposure of the photoresist material to ultraviolet radiation. Typically ultraviolet radiation is used to either decompose the exposed areas of the photoresist resin coating or to cross link the exposed areas of the photoresist resin coating. In the case where the ultraviolet radiation decomposes sections of the photoresist coating, the decomposed areas are removed, typically by contacting these areas with a solvent, and the remaining portions, which constitute the mask, are chemically resistant to the etchant. In the case where the ultraviolet radiation cross links the exposed sections of the photoresist material, the cross-linked sections are rendered chemically resistant to the etchant, and the unexposed sections are removed (such as with a solvent) to form the mask.
[0018] Suitable etchants for etching the surface of a metal layer, such as copper, include various acid solutions. Specific examples of metal (e.g., copper) etchants include a solution comprising from 50 g/L to 500 g/L ferric chloride (FeCl 3 ); a solution comprising from about 5% to about 20% by weight of hydrogen peroxide plus from about 15% to about 30% by volume of sulfuric acid (H 2 S 4 ); a solution comprising from about 15% to about 25% by weight of ammonium persulfate plus from about 15% to about 30% by volume of sulfuric acid; a solution comprising from 250 g/L to 380 g/L nitric acid, and a solution comprising from about 150 to about 350 g/L CrO 3 plus from about 200 to about 400 g/L of sulfuric acid (H 2 SO 4 ). Typically, contacting of the exposed surface of the etchable metal layer with the etchant solution is performed at ambient temperature (e.g., from about 50° F. to about 90° F.) for a period of from about 30 seconds to about 2 minutes to produce an etch depth of from about 20 to about 400 micrometers. After the exposed areas of the etchable metal layer have been contacted with an etchant for a suitable period of time to achieve a desired etch depth, the etch material is immediately contacted with water to remove the etchant and stop the etching process.
[0019] The etching process can cause stains at the etch surfaces. In order to remove such stains the etched surfaces may be exposed to a hydrochloric acid solution (e.g., 25-50% HCl by volume) at ambient temperature for a relatively short period of time (e.g., from about 1 second to 60 seconds) to remove the stains. Immediately thereafter, the surfaces are rinsed with water and dried (e.g., with compressed oil-free air). Thereafter, the remainder of the photoresist material (mask) is removed with an organic stripping solvent, such as denatured alcohol, heptane, etc. The chemical etching process may be repeated a plurality of times using different mask patterns, different depths, etc. to prepare various textured patterns, graphical designs, text, etc.
[0020] As an alternative to chemical etching, sand blasting or other mechanical techniques may be employed, or laser or other ablative techniques may be employed.
[0021] Because the etching process may leave invisible masking material and etching agent residue on surfaces of the etched metal layer, it is usually necessary to further clean and activate the surfaces of the etched metal layer for subsequent electroplating. Cleaning solutions useful for removing residues from the surface of the etched metal layer generally contain at least one organic solvent and at least one surfactant. An example of a preferred cleaning solution contains 20-35% by weight ethyl ethanol, 10-40% by weight heptane, 2-10% by weight triethanolamine, 1-3% by weight non-ionic surfactant (such as butyl or hexyl cellosolve), 10-50% by weight p-mentha-1,8-diene, and up to 10% by weight isopropanol. The cleaning process is typically carried out at a temperature of from about 70° F. to about 110° F. Contacting of the etched metal layer with a cleaning solution may be accompanied with mechanical agitation or ultrasonic agitation for at least about 1 minute. Soft brushing may also be helpful to eliminate heavy contaminants on the surface of the etched metal layer. After cleaning masking and etchant residues from the surface with the cleaning solution, the cleaning solution is rinsed from the etched surface with a water-soluble solvent, such as ethanol, 1-propanol, 2-propanol, or mixtures of these solvents. Thereafter, the water-soluble solvents are immediately rinsed from the surface of the etched metal layer with water. In some cases, it may be desirable to further remove inorganic contaminants from the textured (etched) metal layer by immersion in or spraying with a 5-10% commercial alkaline cleaner, such as Polyprep Cleaner 2202 (Henkel), Gardoclean S 5206 (Oakite), etc. at a temperature of from about 140° F. to about 180° F. for at least 30 seconds, and immediately thereafter rinsing with water. After the cleaning and rinsing steps, it may be necessary to remove corrosion or tarnish stains by immersion in an acid solution, such as a 20-50% by volume hydrochloric acid solution, or a 15-30% by volume sulfuric acid solution, etc., at ambient temperature for a period of from about 10 seconds to about 120 seconds, and immediately thereafter rinsing the acid from the textured (etched) metal layer with demineralized water, and drying (such as with compressed, oil-free air).
[0022] The surface of the textured (etched) metal layer may be activated by contact with an activating solution prior to subsequent electroplating. For example, a suitable activating solution for subsequent acid copper electroplating is a solution comprising from about 1% to about 15% by weight hydrogen peroxide (H 2 O 2 ) and from about 10% to about 30% by volume sulfuric acid (H 2 SO 4 ). A suitable contact time with the activation solution is about 5 seconds to about 60 seconds at room temperature, followed by rinsing with water.
[0023] Before the finish layer is deposited on the surface of the plastic component, it may be desirable to electroplate one or more layers over the textured metal layer having the desired relief pattern. Specifically, it may be desirable to utilize a conventional acid copper electroplating process to level or fill light scratches left on the etched surface during prior texturing and cleaning operations. It may also be desirable to electroplate one or more layers of other metals, particularly nickel, on the relief patterned layer before depositing a finish layer on the relief patterned layer. For example, a semi-bright nickel layer may be electroplated onto the textured metal layer prior to electroplating chrome onto the component. In addition, or alternatively, a bright nickel layer may also be electroplated onto the textured metal layer prior to electroplating a chrome finish layer. In addition, or alternatively, a microporous nickel layer may be electroplated onto the plastic article between the textured metal layer and the finish layer in order to retard corrosion. Accordingly, the expression “depositing a finish layer over the patterned metal layer” refers to either depositing a finish layer directly on the etched or patterned metal layer, or depositing a finish layer on one or more layers previously applied to the etched metal layer.
[0024] The finish layer may comprise a relatively thin chrome or other metal (e.g., nickel) layer deposited over the etched metal layer using known electroplating techniques. Other suitable finish layers include metals such as rhodium, gold, palladium, platinum, silver, black nickel, nickel, or other metals deposited over etched metal layer using any of various metal plating techniques, including vacuum deposition, physical vapor deposition, chemical vapor deposition, etc. A non-metallic material may be used as the finish layer, or may be applied over a metal finish layer. Examples of non-metallic finish or overcoat layers include clear or tinted organic (e.g., polymer) coating compositions, electrophoretic coatings, opaque paints, etc.
[0025] To facilitate different processing steps at different facilities, it may be desirable to apply a corrosion inhibitor to the surface of the relief patterned metal layer after cleaning the surface of the relief patterned layer. This facilitates storage and/or transportation of the article to another facility for subsequent processing. The corrosion inhibitor may be removed, such as with cleaning solvents or the like, prior to subsequent processing.
[0026] The above description is considered that of the preferred embodiments only. Modifications of the invention will occur to those skilled in the art and to those who make or use the invention. Therefore, it is understood that the embodiments shown in the drawings and described above are merely for illustrative purposes and not intended to limit the scope of the invention, which is defined by the following claims as interpreted according to the principles of patent law, including the doctrine of equivalents.
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A relatively inexpensive process for making plastic components having textured chrome finishes that may have fine, crisp, clean lines and intricate details includes steps of electroplating a layer of etchable metal on a surface of a plastic article, typically preserving the surface of the etchable metal, etching a desired relief pattern on the layer of etchable metal, typically cleaning and activating the surface of the relief patterned etched metal layer, and electroplating a layer of decorative metal on the relief patterned etched metal layer.
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FIELD OF THE INVENTION
The present invention relates to methods of displaying digital images and to computer systems therefor.
BACKGROUND TO THE INVENTION
Static digital images can now be produced from a wide variety of sources, including digital cameras and scanners. The ease of production, and relative ease of storage, of such images means that there can be many of them available. This has led to the recognition of the growing problem of holding the viewers attention when viewing an image. In an attempt to address this problem, it has been proposed to use so-called “rostrum camera” techniques, which produce a series of images from a static image by zooming in on a part of the image, zooming out to the original image and then zooming in on a different part of the original image.
A method of automating rostrum camera techniques for static digital images has been proposed in our co-pending United Kingdom patent application number GB 0104589.7 the content of which is incorporated herein by reference. The method disclosed therein is used automatically to determine areas of interest in the image to avoid the requirement for a manual selection thereof by the user. It is concerned with viewing a single image by producing a moving sequence of images thereover. It can pan, zoom or fade between images, all of which are forms of moving viewpoints. This is referred to as a rostrum path, whether produced manually or automatically.
However, a viewer often wishes to view a plurality of separate digital images. In this case, as shown in FIG. 1 of the drawings that follow, from a first static digital image 2 , an object 4 (here a person's face)is selected (whether manually or automatically) on which to zoom and a first zoomed image 6 is displayed by the system zooming in on the object 4 . The zoomed image 6 thus shows a part (not being the whole) of the first static digital image 2 . To move to a second static digital image 8 , the method is first to zoom out from the first zoomed image 6 to first static digital image 2 (shown as 10 in FIG. 1 to illustrate the sequence though it is identical to image 2 ), to replace first static digital image 2 with second digital static image 8 . The view may then zoom in to a part of the second static digital image 8 as a second zoomed image 12 on an object (house 14 ) selected manually or by an automatic process.
Such a transition between images can be arbitrary, aesthetically unappealing and slow. The transition from image 6 to image 12 is via two full-view images ( 8 and 10 ) and the two zoomed images are unconnected conceptually and visually.
SUMMARY OF THE INVENTION
According to the present invention in a first aspect, there is provided a method of displaying digital images comprising the steps of using a processor to determine an extent of similarity between a first image part and a second image part, displaying a first image part from a viewpoint and transitioning to displaying a second image part from a viewpoint, the second image part being selected at least partly based on a determined extent of similarity between the first image part and the second image part, in which the viewpoint of an image part is moved during the transition.
According to the present invention in a second aspect, there is provided a method of displaying digital images comprising the steps of using a processor to determine an extent of similarity between a first image part and a second image part, displaying a first image part from a viewpoint and transitioning to displaying a second image part from a viewpoint, the second image part being selected at least partly based on a determined extent of similarity between the first image part and the second image part, in which the viewpoint of the second image part is moved after the transition takes place.
Suitably, the transition is one or more of a dissolve, a wipe, a blind, a random dissolve or a morphing between images.
Suitably, the determination of an extent of similarity requires a substantial match between an object in a first image part and an object in a second image part before a transition is effected.
Suitably, an extent of similarity is determined between at least three image parts, which image parts are displayed in an order based at least in part on maximising the extent of similarity therebetween.
Suitably, a predetermined first image part is selected against which to determine an extent of similarity of a second image part.
Suitably, the predetermined first image part is the final image part of a rostrum path.
Suitably, the determination of the extent of similarity is uses image matching.
Suitably, a viewpoint is positioned to maximise the overlap between the first image part and the second image part.
Suitably, an extent of similarity is determined between faces in the first and second image parts.
Suitably, the first image part and the second image part each have a corresponding frame size and the respective frame size is determined to maximise the overlap between an object in the first image part and an object in the second image part.
Suitably, the first image part and second image part are from the same image.
Suitably, the first image part is from a first image and the second image part is from a second image.
Suitably, a rostrum path is determined in the first image having a first image part start and first image part finish.
Suitably, the first image part is the first image part finish.
Suitably, a rostrum path is determined in the second image having a second image part start and second image part finish.
Suitably, the second image part is the second image part start.
Suitably, the rostrum path of the first image and the rostrum path of the second image are determined whereby the first image part finish is the most similar image part determined in a comparison of the first image rostrum path and the second image rostrum path and the second image part start is the corresponding most similar image part of the second image.
Suitably, the or each rostrum path is determined using the processor to perform an analysis of image data from the first and second images to identify characteristics of the image content; and generating, in the processor, a set of video data for output to a display, the video data representing displayable motion over the image and being generated in accordance with the image content characteristics.
According to the present invention in a third aspect, there is provided a computer system comprising a processor, a data input port and a display device, the processor being arranged to receive image data from the data input port, and to determine an extent of similarity between a first image part of the image data and a second image part of the image data and to display a transition between a viewpoint of the first image part and a viewpoint of the second image part selected from a plurality of image parts, the selection being based at least partly on the determined extent of similarity between the first image part and the second image part, and in which the viewpoint of an image is moved during the transition.
According to the present invention in a fourth aspect, there is provided a computer system comprising a processor, a data input port and a display device, the processor being arranged to receive image data from the data input port, and to determine an extent of similarity between a first image part of the image data and a second image part of the image data and to display a transition between a viewpoint of the first image part and a viewpoint of the second image part selected from a plurality of image parts, the selection being based at least partly on the determined extent of similarity between the first image part and the second image part and in which the viewpoint of the second image part is moved after the transition takes place.
The view point is a 3-parameter quantity, namely x and y position and z zoom factor, relative to the image.
DESCRIPTION OF THE DRAWINGS
The present invention will now be described, by way of example only, with reference to the drawings that follow; in which:
FIG. 1 is a diagrammatic illustration of the image transitions of a prior art rostrum camera method.
FIG. 2 is a schematic illustration of a computer system according to an embodiment of the present invention.
FIG. 3 is a diagrammatic illustration of image transitions of an embodiment of the present invention.
FIG. 4 is a functional flow diagram illustrating a method corresponding to FIG. 3 .
FIG. 5 is a diagrammatic illustration of image transitions of another embodiment of the present invention.
DESCRIPTION OF PREFERRED EMBODIMENTS
An embodiment of the present invention is shown in FIG. 2 of the drawings that follow. Referring to FIG. 1 , a computer system 20 comprises a processor 22 connected to a memory 24 , which processor 22 outputs data to a display device 26 , such as a monitor. The computer system 20 further comprises a data input port 28 for receiving image data from a digital image data source 30 , such as a scanner, digital camera, data carrier or an image download.
Memory 24 stores a computer program for operating the computer system 20 according to an embodiment of the present invention.
Referring to FIGS. 3 and 4 of the drawings that follow, the method of this embodiment of the present invention is now described.
It is desired to transition from a first static digital image 2 (the same as the first image in FIG. 1 ) to a second static digital image 9 via a zoomed image of first static digital image 2 . In order to do so, processor 22 determines the similarity of parts of first and second static digital images 2 , 9 respectively (step 400 in FIG. 4 ). There are many different techniques for making an assessment of similarity (region matching) between parts of two images using machine-vision techniques. Generally these techniques use a combination of colour, texture and gradient information.
For instance general techniques used for image database indexing Rowley-Baluja-Kanade.. Neural Network based face detection. IEEE PAMI, 20(1):23-38 del Bimbo, A, Pala, P., Shape Indexing by Multi-Scale Representation, IVC Journal (17), No. ¾ March 1999, pp. 243-259, Latecki, L. J. [L. Jan], Lak,,mper, R., Shape Similarity Measure Based on Correspondence of Visual Parts, PAMI(22), No. 10, October 2000, pp.1185 use region colour, shape and texture-based similarity metrics to find similar part of different images and could be uses to generate candidates for our purpose. If there are the same objects in two images other techniques can be used, such as active shape models [Cootes, T. F., Taylor, C. J., Lanitis, A., Multi-Resolution Search with Active Shape Models, ICPR Conference 1994 (vol App610-612) that seek to match similar shapes by deforming according to image characteristics. Faces are excellent candidate features for match-dissolving and techniques that locate faces and which can identify them as well Rowley-Baluja-Kanade. Neural Network based face detection. IEEE PAMI, 20(1):23-38, Brunelli, R., Falavigna, D., Person Identification Using Multiple Cues, IEEE PAMI(17), No. 10, October 1995, pp. 955-966 and can be used for extracting candidate face locations, matching scores etc.
In each case an assessment is made of the similarity between parts of the first static digital image 2 and parts of the second static digital image 10 . From each technique a quantitative determination is made of the similarity of parts of image 2 with parts of image 8 . The frame size of each image part may be selected manually or automatically and may be adaptively determined to maximise the overlap between objects in the respective images. This determination can be used in a number of ways, some of which are detailed below, to transition between the first static digital image 2 to the second static digital image 10 .
It is noted that the “objects” may be single or multiple items and may be part or the whole of something. Any object may be a person, a face, a chair, a tree, a building, a part of scenery etc.
From each technique a quantitative determination is made of the similarity of parts of image 2 with parts of image 9 .
The first option is for the transition to occur between the parts of the two images 2 , 10 that have the highest quantitative determination of similarity.
Another option is for the transition to occur only for faces or even only if two individual faces are found that, according to the determination, belong to the same individual. Alternatively, after an initial determination of similarity, a weighting may be applied for items likely to be of interest (eg skin tones).
It may be pre-set that for the image transition according to embodiments of the present invention to occur, a given similarity threshold must be determined between at least a part of the first image and a part of the second image or identity may be required, though an allowance may be made for movement of an object between images.
Other possibilities exist. For instance a random selection may be made from any image part pair that exceed a predetermined similarity.
The determination of the object types the transition is to be between may be made automatically or manually (step 402 in FIG. 4 ).
A determination is then made (step 404 in FIG. 4 ) of the transition type to be used. Again, this can be an automatic or manual selection.
Many transitions can be used, including the following:
a) dissolve b) wiping c) blinds d) random dissolve e) morphing f) cut
Other possible transitions exist. These may be used singly or in combination.
The selection of which transition type to use can be made adaptively, in which case an automatic determination is made of the most appropriate transition to use, or randomly.
Referring again now to FIG. 3 , it is determined in this example that the two most similar parts are the objects 4 , 30 being the faces, of the individuals in the images 2 , 9 . The term “objects” is used in its widest sense. For instance it may include a mountain scene, a tree or even an arbitrary object such as a shape (see FIG. 5 ). The image then zooms to first zoomed image 6 (step 406 in FIG. 4 ). The view then transitions (indicated at 32 ) from the zoom on the object 4 on first image 2 to the zoomed image 30 of second image 9 (step 408 in FIG. 4 ), and may then zoom out to the full second image 9 (step 410 in FIG. 4 ). Thus, instead of transitioning between the images 2 , 9 from full image to full image, the transition is from a zoomed image of one image to a zoomed image of another image.
In an alternative embodiment a selection of a part of first image 2 may be made before a determination of similarity is carried out. In such an embodiment a manual or automatic selection is made of a part of the first image of interest, say the face 4 in the first image 2 and then a determination of similarity is made between this image part and parts of the second image 9 . Therefore the view may zoom to a part of the first image before any similarity determination is made.
It is preferable to position the viewpoint of both image parts so as to maximise the overlap therebetween. That is the veiwpoint is adjusted so that the position and dimensions of an object in the second image part match, to the maximum extent possible, the position and dimensions of the similarity based object in the first image part. So, if a face is determined as an object in the first image part and there is a face in the second image part to which a transition is to be made, if the first face is to the left and takes up half the image space, the viewpoint for the second image part is positioned so the second face is positioned correspondingly to the left and to take up substantially the same image area
Embodiments of the present invention can, therefore, be used to produce slide shows from a plurality of static digital images.
Referring to FIG. 5 of the drawings that follow, a further embodiment of the present invention is illustrated in which only a single original digital image 50 is analysed for similar image parts. In this case a sufficient similarity is found between first object 52 (a circle) and a second object 54 (an oval). Accordingly, a first zoomed image 56 of first object 52 is displayed, followed by a transition (as described above) to a second zoomed image 58 of second object 54 . Optionally the displayed image may zoom out to the original image 50 .
As with the FIGS. 3 and 4 embodiment, initial selection of an object/image part may be manual or automatic and a variety of part matches and transition types can be available.
The first and second image parts may be part of a rostrum path, in which case the rostrum path may be manually or automatically generated. A rostrum path extends for a plurality of image parts from an image part start to an image part finish. To create the best slide show, it is generally best if the final image of a first rostrum path is transitioned to the first image of a second rostrum path, the final and start images being determined as being the most similar.
Whether there is one image or two, a further refinement to the present invention is for three or more image parts to be assessed against each other for an assessment of similarity therebetween. The image parts can then be displayed in an order that has the lowest overall discrepancy between image parts.
If a first rostrum path has been determined, a transition to an image part, that may be the start image part of a second rostrum path, can be based on an assessment of similarity between the finish image part of the first rostrum path and part of the image which a transition is to be made, to maximise the similarity therebetween. In this case the first image part is fixed and the system and method seek a best matching second image part that may be the start of a second rostrum path.
The determination of extent of similarity may use image matching techniques that match object to object in one image part to an object or objects in a second image part (generally, but not necessarily, this will be between two distinct images). These techniques make allowance for temporal and/or spatial displacement between the two images. One such technique uses active shape models (see Cootes, T. F., Taylor, C. J., Lanitis, A., Multi-resolution Search with Active Shape Models, ICPR Conference 1994 (vol A: pp 610-612)). If a match is found it is preferred for a morphing transition to be used.
The reader's attention is directed to all papers and documents which are filed concurrently with or previous to this specification in connection with this application and which are open to public inspection with this specification, and the contents of all such papers and documents are incorporated herein by reference.
All of the features disclosed in this specification (including any accompanying claims, abstract and drawings), and/or all of the steps of any method or process so disclosed, may be combined in any combination, except combinations where at least some of such features and/or steps are mutually exclusive.
Each feature disclosed in this specification (including any accompanying claims, 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.
The invention is not restricted to the details of the foregoing embodiment(s). The invention extend to any novel one, or any novel combination, of the features disclosed in this specification (including any accompanying claims, abstract and drawings), or to any novel one, or any novel combination, of the steps of any method or process so disclosed.
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A method of displaying digital images comprises the steps of using a processor to determine an extent of similarity between a first image part and a second image part, displaying a first image part from a viewpoint and transitioning to displaying a second image part from a viewpoint, the second image part being selected at least partly based on a determined extent of similarity between the first image part and the second image part, in which the viewpoint of an image part is moved either during the transition or after the transition takes place. An appropriate system is provided.
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BACKGROUND AND SUMMARY OF THE INVENTION
This invention pertains to a current supply circuit, and more particularly, to such a circuit which includes changeable-level voltage source for the supply of current, the level of which source is varied in accordance with the impedance of a load connected to the circuit. For the purpose of illustration herein, a preferred embodiment of the circuit is described in connection with transcutaneous stimulation which is used for pain relief purposes. In such apparatus, the instant invention has been found to have particular utility.
Speaking in very general terms, a conventional current supply circuit includes a current source connected in series with what is known as a compliance voltage source. These two devices are connected in series between a pair of output terminals adapted for connection to a load. Typically, the compliance voltage source operates at a particular maximum voltage, which voltage is divided between the current source and the output terminals directly in accordance with the impedance of any load connected to the output terminals. The larger the impedance value of a connected load, the more of the compliance voltage which appears across the load and the less of it which appears across the current source. The lower the impedance value of a load, the smaller the voltage across the load and the larger the voltage across the current source. The sum of the voltages across the load and the current source always substantially equals the maximum voltage level of the compliance voltage source.
While there are applications where this kind of an arrangement is entirely satisfactory, there are many others where it is desirable to reduce and limit the maximum voltage which can appear across output terminals in such a supply circuit. One of these applications concerns devices known as transcutaneous stimulators which, essentially, are pulsed current supply circuits intended for connection through electrodes to a person's skin for the purpose of creating electrical current nerve stimulation. Such a device is used quite frequently for pain relief. However, it is known that it is possible for too high a voltage between output electrodes to cause skin damage. Further, if too high a voltage exists between such electrodes in their open-circuited condition, then, if a stimulator, while turned on, is connected to a person's skin, a substantial shock can occur.
A general object of the present invention is to provide a current supply circuit which includes a changeable-level compliance voltage source whose voltage output level is modified in accordance with the impedance of a load connected to the circuit.
More particularly, the present invention proposes a circuit wherein, so long as the value of the impedance of a connected load is below a predetermined maximum value, the overall circuit performs essentially like an ordinary current supply circuit of the type generally described above. However, on the connected load exceeding this predetermined maximum impedance value, a control subcircuit, which is included in the circuit, responds to this condition quickly to shut down the level of the voltage in the compliance voltage source to an acceptable minimal level, which level remains until the impedance value of any connected load is again below the predetermined maximum impedance value.
With this kind of arrangement, the open-circuit voltage which exists between output terminals in such a supply circuit when the same is turned on, is the minimum voltage level just mentioned, and there is no likelihood of a shock occurring when electrodes are connected to a person. Further, if, when electrodes are connected, the skin impedance between the electrodes exceeds the predetermined maximum impedance value, the compliance voltage level is held at the minimum voltage level so that no skin damage can occur.
These and other objects and advantages which are attained by the invention will become more fully apparent as the description which now follows is read in conjunction with the accompanying single drawing figure.
DESCRIPTION OF THE DRAWING
The single drawing figure is a schematic diagram, partly in block form, illustrating the construction of a portion of a transcutaneous stimulator including a current supply circuit constructed in accordance with the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Turning now to the drawing, indicated at 10 is a portion of a transcutaneous stimulator including a current supply circuit made in accordance with the present invention. Shown at 12 is a changeable-level compliance voltage source, including a conventional voltage generator, indicated in block form at 14, and a conventional voltage doubler and storage circuit, indicated in block form at 16. Generator 14 takes the form herein of a changeable-amplitude high-frequency oscillator which produces high-frequency AC between output terminals 14a, 14b. An amplitude-change control terminal 14c is provided for the generator. Changes in voltage on terminal 14c effect changes in the amplitude of the AC voltage developed between terminals 14a, 14b. More specifically, the higher the voltage on terminal 14c, the higher the voltage between terminals 14a, 14b, up to a maximum of about one-hundred volts AC, peak-to-peak. When terminal 14c is grounded, the voltage between terminals 14a, 14b drops to about ten volts AC, peak-to-peak. The output terminals of the voltage generator are connected to the input terminals doubler and storage circuit 16. This circuit produces, between terminals 16a, 16b, a changeable-level DC output voltage that ranges between about ten volts DC and about one-hundred volts DC. Such voltage is referred to herein as a compliance voltage.
Indicated by a dashed block 18 is a changeable-level constant current source which is also of conventional construction. Shown within block 18, schematically, are symbols representing two current generators 20, 22, wherein arrows are used to indicate the respective orientations for producing current flow in opposite directions. A solid arrow is used in generator 20, and a dashed arrow in generator 22. When generator 20 is switched on, as will be explained, it couples to output terminals 18a, 18b in block 18. Similarly, when generator 22 is switched on, it couples to output terminals 18c, 18d.
It should be understood that while source 18 has just been described as one including a pair of oppositely directed current generators, such an arrangement would typically be constructed using a single generator, with appropriate switching circuitry provided which effectively changes the direction in which current flows at output terminals connected to the source. There are many ways of constructing such a source, and none of them forms any part of the present invention.
Control terminals 18e, 18f are provided for block 18. With a certain positive voltage existing on terminal 18e, and a substantially zero voltage existing on terminal 18f, generator 20 operates. With essentially the same certain positive voltage existing on terminal 18f, and a substantially zero voltage existing on terminal 18e, generator 22 operates. Under other circumstances, there is no current flow through source 18.
As was previously mentioned, another aspect of current source 18 is that its level can be changed. For example, it is contemplated in the construction shown that an output current level for this source is infinitely selectable in the range from about zero to about thirty milliamperes. This is a range of currents which has been found to be particularly suitable for the usual transcutaneous stimulation procedure. A suitable means (not shown) is provided for selecting such a current level.
Further included in circuit 10 are two output terminals 24, 26. Terminal 24 is connected to a terminal 28a in a switching circuit 28, the function of which will be explained shortly. Terminal 26 is connected to each of terminals 18b, 18d in the current source. Terminals 18a, 18c in the current source are connected through a conductor 30 to another terminal 28b in switching circuit 28. Terminals 24, 26 herein are adapted for connection, through suitable body-contacting electrodes, to a persons's skin, represented in the figure by block 32 designated "LOAD".
Contained in circuit 10, in accordance with the invention, is a voltage-level control means which functions, as will be explained, to change the level of the compliance voltage produced by source 12. This voltage-level control means is designated generally at 34, and includes a transistor 36. The emitter of transistor 36 is connected to the circuit ground (represented by a triangle), and the collector is connected through a conductor 38 to previously mentioned control terminal 14c in generator 14. The base of transistor 36 connects with a conductor 40 which connects through a resistor 42 and a diode 44 to output terminal 16b in block 16. The anode of diode 44 connects to the circuit ground through a capacitor 46, and the cathode of the diode connects to the circuit ground through a resistor 48.
Terminal 16a in block 16 connects through a conductor 50 to a terminal 28c in switching circuit 28. A resistor 52 interconnects conductors 40, 50. A conductor 54 connects yet another terminal, 28d, in circuit 28 to the circuit ground.
In the setting of transcutaneous stimulation, it has been found to be desirable to supply current to a patient in pulses at a rate of around 100-pulses-per-second. More specifically, it has been found to be desirable to apply, first, a pulse of one polarity for a selected time duration, such as about 0.2-milliseconds, followed immediately by an equal current pulse in the opposite direction for substantially the same duration -- with such "bidirectional" pulses applied at the above-mentioned rate. It will be obvious that other kinds of current supplies for other applications will not require this pulsing technique. However, in the circuit shown in the drawing there is provided a pulse generator 56 including output terminals 56a, 56b, 56c which function, as will be described, to generate pulses like those just discussed. Terminal 56a connects with previously mentioned conductor 40. Terminal 56b connects through a conductor 58 with a terminal 28e in switching circuit 28, and through conductor 58 and a conductor 60 with previously mentioned terminal 18f. Terminal 56c connects through a conductor 62 with a terminal 28f in circuit 28, and through conductor 62 and a conductor 64 with previously mentioned terminal 18e.
Pulse generator 56 is of conventional construction. When it operates, it produces at terminal 56a, positive-going square-wave pulses lasting about 0.4-milliseconds, at a rate of about 100-pulses-per-second. On terminal 56b it produces similar positive-going square-wave pulses, approximately 0.2-milliseconds long, and corresponding in time to the first 0.2-millisecond portions of the pulses produced on terminal 56a. On terminal 56c the pulse generator produces positive-going square-wave pulses, each also lasting about 0.2-millisecond, and each corresponding in time to the latter 0.2-millisecond portions of the pulses produced on terminal 56a.
Explaining generally how the pulse generator cooperates with other elements in circuit 10, each pulse on terminal 56a turns on transistor 36, and thereby causes grounding, through the transistor, of conductor 38, and hence of control terminal 14c in generator 14. Each pulse on terminal 56b produces switching in circuit 28 whereby flow can take place through this circuit as indicated by the dashed arrows in block 28. Also, each such pulse acts through terminal 18f to cause current flow through source 18 as indicated by generator 22. Each pulse on terminal 56c causes switching in 28 whereby flow can take place therethrough as indicated by the solid arrows in block 28. Also, each such pulse on terminal 56c acts through terminal 18e to cause current flow through source 18 as indicated by generator 22.
As was previously mentioned, source 18 is infinitely variable to select output current levels within the range of about zero to about thirty milliamperes. This range has been selected as the one most suitable for the usual transcutaneous stimulation procedure. Different specific levels are, of course, selected for different stimulation situations. Further, generator 14 and circuit 16 have been constructed herein to produce a compliance voltage between output terminals 16a, 16b of up to about one-hundred volts DC. This has been found to be a desirable maximum level. Whenever transistor 36 is in a nonconducting state, substantially the full maximum amount of this compliance voltage appears between terminals 16a, 16b. However, whenever the transistor conducts and grounds terminal 14c, the output level of voltage generator 14 is reduced, as will be explained, to lower the available compliance voltage.
Under circumstances with no load connected to terminals 24, 26, and with circuit 10 operating, transistor 36 is biased to a stage of conduction, by virtue of the voltage made available at its base, which maintains generator 14 operating at a sufficient level to produce a compliance voltage between terminals 16a, 16b also of about ten volts DC. Substantially this same voltage appears periodically between terminals 24, 26 with operation of pulse generator 56. Thus, the open-circuit voltage appearing between terminals 24, 26 is relatively low.
According to an important feature of the invention, so long as the impedance value of a load connected between terminals 24, 26 is less than about 3000-ohms, circuit 10 always functions to create a compliance voltage level related to the amount of current flowing through the load, which acts as if there is a constant fixed impedance of 3000-ohms connected between conductors 40, 50. In other words, so long as the connected load does not exceed the value just mentioned, and with a particular level of current selected from source 18, the compliance voltage produced by source 12 will be automatically adjusted to a value whereby the ratio of this voltage and the selected current equals 3000-ohms.
Let us take a typical operation for example. With circuit 10 operating, let us assume that electrodes connected to terminals 24, 26 are attached to a person's skin, and that the impedance between these electrodes (through the skin) is 1000-ohms. Let us assume further that source 18 has been adjusted to provide a maximum current of ten milliamperes. Initially, and because of a certain minimum voltage required to keep the current source operating, only a portion of the original open-circuit ten volts appears across the load, and this portion produces a current which, it will be recalled, can only flow during the time that a pulse exists either on terminal 56b or on terminal 56c. Assuming that initial flow is as produced by current generator 20, this flow is into conductor 30 through switching circuit 28 and conductor 54 to the circuit ground. From circuit ground, current flows through resistor 48, through voltage source 12 to conductor 50, back through switching circuit 28, and through the load back to the current generator.
The consequence of this activity is that a negative voltage builds up at the junction between capacitor 46 and resistor 42, which voltage tends to hold transistor 36 in a nonconducting state. It should be pointed out that whenever a pulse exists on pulse generator terminal 56a, the transistor is held in a conducting state, which situation results in the output voltage of generator 14 being held down. However, and considering the time that no pulse exists on terminal 56a, the voltage at the base of the transistor which is effective to control whether it is turned on or off depends upon the voltages existing at the junction just mentioned between resistor 42 and capacitor 46, and that existing at the junction between resistor 52 and conductor 50. With some negative voltage applied to the base sufficient to hold the transistor in a nonconductive state, generator 14 operates to build up the voltage between terminals 16a, 16b, which results in a slightly greater current flow occurring through the load with the next set of control pulses from terminals 56b, 56c.
So long as current through the load is building up to the ten milliampere setting mentioned earlier, a sufficiently negative voltage is maintained on the base of the transistor, during times that no pulse exists on terminal 56a, to allow the voltage of source 12 to build up. When the full ten milliampere current can flow and is flowing, the compliance voltage which exists between terminals 16a, 16b is thirty volts. This results in the previously mentioned constant impedance of 3000-ohms which the circuit "assumes" is connected between conductors 40, 50. Without any change occurring in load resistance, or in the setting of current source 18, this situation remains unchanged. As a consequence, and in repeated cycles, a 0.2-millisecond positive-going current pulse, at the level of ten milliamperes, is delivered to the person, followed immediately by a negative-going pulse of the same duration and level, followed by a period of 9.6-milliseconds with no current so delivered. It might be pointed out that this manner of delivering pulses has been found to be the most effective for nerve stimulating and the least damaging to skin tissue.
Should the load impedance change at any time during this operation, and so long as it does not exceed 3000-ohms, current continues to be delivered in the manner just described and at the ten milliampere level called for. All that takes place is that the division of compliance voltage between the current source and the load changes. The sum of the voltages across the current source and across the load will, under these circumstances, always equal the full value of the compliance voltage which is then being used. In the case now being illustrated this value is thirty volts.
The fact that load current flows through resistor 48 causes this resistor to act as a monitoring resistor which, in effect, and inasmuch as the current level is constant, provides a direct indication of load impedance. As was discussed above, an equilibrium condition is reached whereby the negative voltage at the junction between resistor 42 and capacitor 46 balances with voltage on conductor 50 so as to produce a control voltage on the base of transistor 36 sufficient to maintain the compliance voltage at thirty volts.
If the setting of the current source is changed, for example to twenty milliamperes, load current builds in the manner described previously, and a new equilibrium condition is reached whereby transistor 36 controls source 12 so as to produce a compliance voltage of sixty volts. With the full level of current selected, i.e., thirty milliamperes, the compliance voltage builds up to ninety volts.
Should the load impedance exceed 3000-ohms, then what will occur is that the current source, at the compliance voltage level then called for by the particular current level setting, will not be able to supply the full level of called-for current. As a consequence, a slightly lower value of current than the setting value will flow in the circuit, and this will result in the base voltage of the transistor rising. This will increase conduction in the transistor, and effect a lowering of the compliance voltage. With a drop in compliance voltage level, yet a smaller current flows, and this process continues in a regenerative fashion until the compliance voltage has been reduced to the minimum level of about ten volts. As a consequence, a potential damage situation does not occur in the person's skin.
It will thus be apparent that resistor 48 acts as a means for monitoring load current, and ultimately load impedance. The negative voltage which exists across this resistor is stored in capacitor 46, and is applied through resistor 42 to the base of transistor 36, tending to turn the transistor off. Also acting on the transistor's base, and tending to turn the transistor on, is a positive voltage derived directly from the compliance voltage, and applied through resistor 52. The larger the negative voltage across resistor 48, the larger is the compliance voltage; and the ratio of the resistance values of resistors 42, 52 determines what level of compliance voltage will develop with respect to a given negative voltage across resistor 48. Herein, this ratio is selected to produce a compliance voltage which, when divided by the current flowing in the load, equals 3000-ohms. Those skilled in the art will readily appreciate how such a ratio may be changed to handle other circumstances.
There is thus provided by the invention a unique current supply circuit in which control occurs automatically for the level of compliance voltage, so that the voltage which is applied to any connected load is not only limited to a predetermined maximum level, but is in fact shut down when a too-high load impedance tends to call for an excessive voltage. This same control also insures that open-circuit voltage is low.
It is appreciated that the circuit of the invention may be used in a number of applications other than in the setting of a transcutaneous stimulator. For example, it can certainly be used in a variety of current supply circuits which are neither pulse nor bidirectional.
Thus, while a preferred embodiment of the invention has been described herein, it is appreciated that variations and modifications may be made without departing from the spirit of the invention.
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A constant current supply circuit including a changeable-level compliance voltage source whose output voltage is automatically reduced whenever the impedance of a load connected to the circuit exceeds a predetermined value. A sampling resistor is provided in the path for load current, and this resistor, with load current flowing, develops a related voltage whose level is employed directly to affect the operating level of the compliance voltage source.
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RELATED APPLICATIONS
This application is a continuation of U.S. patent application Ser. No. 13/949,507, filed 24 Jul. 2013, now U.S. Pat. No. 8,642,814. This application claims priority to U.S. Provisional Application No. 61/675,221 filed 24 Jul. 2012.
INTRODUCTION
Currently, most chemical production is based on petrochemical feedstocks (also known as fossil fuels). These feedstocks are obtained from carbon sources that have been buried underground for millions of years. These petrochemical feedstocks are being extracted from their underground repositories and converted into a myriad of chemicals for uses ranging from fuel to plastics to commodity chemicals to high value compounds such as fragrances. Although techniques for modifying petrochemical feedstocks are very well developed, there are serious drawbacks from petrochemical-based technologies including declining supplies of petrochemicals and environmental hazards in extracting the petrochemicals from underground repositories. In addition, much of the carbon from the petrochemicals ends up in the atmosphere in the form of carbon monoxide (CO) and carbon dioxide (CO 2 ) which are implicated in global warming.
To ameliorate the problems with petrochemicals, great efforts have been expended in developing alternatives to petrochemical-based technologies. One such alternative to petrochemical feedstocks are carbon-containing compounds extracted from recently-living organisms. As organisms such as algae and plants grow, they extract CO 2 from the atmosphere, thus providing a major advantage over fossil fuel technology. A challenge with using these organisms to replace fossil fuels is the relative cost of growing them and making useful products from these organisms. Thus, there has been a long-standing problem of increasing the value of products obtained from living or recently-living organisms such as algae and plants. This invention provides new techniques for making high-value products from mixtures of palmitoleic acid esters and oleic acid esters that are derived from biological materials.
As described in greater detail below, the invention provides a new route to civetone and olefinic co-products. Civetone is a macrocyclic ketone which is used as an ingredient in perfume and fragrance products. In nature, civetone is a pheromone produced by the African Civet. Due to the limited natural supply, methods of synthesizing civetone have been developed. Known sources of starting materials for synthesizing civetone include compositions high in oleic acid (C18:1; C 18 H 34 O 2 ), such as palm oil, and compositions high in aleuritic acid (C 16 H 32 O 5 ), such as shellac. The current methods for synthesizing civetone have not achieved a high efficiency, with the overall isolated yields for known methods of synthesizing civetone from oleic acid ranging from 23-74% in lab settings and yields from aleuritic acid being even lower. The ability to get higher overall yields of selected products is an advantage of some preferred embodiments of the invention.
Civetone can be synthesized from Omega-7 rich oil, such as, but not limited to, the commonly known sources sea buckthorn and macadamia nut oil. The monounsaturated fatty composition (C16:1 and C18:1) for Sea buckthorn is around 50% (Yang & Kallio, 2001) and for Macadamia nut oil (Maguire, O'Sullivan, Galvin, O'Connor, & O'Brien, 2004) it is approximately 80%. In the present invention, ethyl esters of Palmitoleic acid (C16:1) and Oleic acid (C18:1) obtained from Omega-7 rich oil sources can be used as precursors for synthesis of civetone.
Synthesis of ethyl esters is known for the enrichment of Omega-3 fatty acids. Transesterification of Omega-7 fatty acids to produce ethyl esters can be done using multiple catalyst/conditions, such as the following catalyst/conditions:
a) enzymatic (Fjerbaek, Christensen, & Norddahl, 2009)(Modi, Reddy, Rao, & Prasad, 2007)(Mata, Sousa, Vieira, & Caetano, 2012);
b) acid/base catalyzed (Rodri & Tejedor, 2002)(Alamu, Waheed, & Jekayinfa, 2008); or
c) heterogeneous catalyst (Zabeti, Wan Daud, & Aroua, 2009)(Liu, He, Wang, Zhu, & Piao, 2008).
As shown in FIG. 1 , ethyl esters of Omega-7 oil can be separated using one or more separation techniques, such as, but not limited to, molecular distillation. Molecular distillation is a separation technique used for separation of fatty acid methyl esters (FAME) in biodiesel production process. Ethyl esters from Omega-7 rich oil can be separated into three fractions (Rossi, Pramparo, Gaich, Grosso, & Nepote, 2011)(Tenllado, Reglero, & Torres, 2011):
1) Fuel (such as C10 to C16)
2) Omega-7 (such as C16:1 and C18:1)
3) Omega-3 fractions (such as C20:5 and C22:6).
After molecular distillation, the fuel fraction can provide feed to a hydrotreater for synthesis of high cetane diesel through hydrodeoxygenation treatments known in the art. The high cetane diesel produced may be isomerized, using methods known in the art, to give jet fuel. The omega-7 fraction (mono-saturated fatty acids), composed of Palmitoleic acid (C16:1) and Oleic acid (C18:1), is a commercial product with many potential uses in the health industry. Omega-7 (Palmitoleic acid) is found in human skin sebum and is known to decline with age (Wille & Kydonieus, 2003). Omega 7 supplements comprising sea buckthorn oil are currently available in the market as a health product for skin and hair (contains approximately 30% Omega 7)(Yang & Kallio, 2001). Omega 7 ethyl esters can substitute for sea buckthorn oil in products, and provide an advantage due to the fact that esters can provide a higher purity not currently available in the market (Rüsch gen. Klaas & Meurer, 2004). In preferred embodiments of the present invention, the Omega-7 rich fraction is used for synthesis of civetone by olefin metathesis.
PRIOR ART
Prior Art: Known method of synthesizing civetone from palm oil
In 1994 (Choo, Ooi, & Ooi, 1994), synthesis of Civetone was reported from Palm oil. In this process Oleic acid (C18:1) was obtained from Palm oil by hydrolytic splitting with 99% purity. See FIG. 2 . The pure Oleic acid was esterified under acidic conditions using concentrated sulfuric acid at 110° C. Self-metathesis of ethyl oleate was performed using WCl 6 and SnMe 4 to give two products, 9-Octadecene and Diethyl 9-Octadecenedioate, with almost quantitative yields of 97 and 99% respectively. Silica-gel chromatography was used to separate the two products. The Diethyl 9-Octadecenedioate was cyclized using base catalyzed Dieckmann Condensation under inert conditions. Dieckmann Condensation was carried out under argon using potassium hydride (KH) in dry THF at 55° C. for 3 hours to give 2-ethoxycarbonyl-9-cycloheptadecenone with 63% yield which was purified by silica-gel chromatography. Civetone was synthesized by hydrolysis followed by decarboxylation of 2-ethoxycarbonyl-9-cycloheptadecenone using 5% NaOH/THF/Ethanol with 93% yield which was also purified by silica-gel chromatography.
Prior Art: Known methods of ethenolysis of methyl oleate and synthesis of civetone using methyl 9-decenoate
Ethenolysis of Methyl Oleate
In 2011, ethenolysis of methyl oleate (Thomas, Keitz, Champagne, & Grubbs, 2011) was performed using N-Aryl, N-alkyl N-heterocyclic carbene (NHC) ruthenium metathesis catalysts with 95% selectivity for terminal olefins.
Ethenolysis of methyl oleate can be performed using First Generation Grubb's catalyst (Burdett et al., 2004) or in a microbial system (Park, Van Wingerden, Han, Kim, & Grubbs, 2011) to give 1-Decene and Methyl 9-Decenoate as products. See FIG. 3 .
Synthesis of Civetone Using Methyl 9-Decenoate
In 2000, Ti-Claisen condensation of Methyl 9-Decenoate followed by an intramolecular metathesis reaction was used for synthesis of civetone (Hamasaki, Funakoshi, Misaki, & Tanabe, 2000). See FIG. 4 .
Ti-Claisen condensation of Methyl 9-Decenoate was carried using TiCl 4 and Bu 3 N at 0-5° C. for 1 hour to give β-ketoester as a product with 93% yield. The β-ketoester was then allowed to undergo intramolecular metathesis using Grubb's reagent at 110° C. to give 2-methoxycarbonyl-9-cycloheptadecenone with 84% yield. The intermediate 2-methoxycarbonyl-9-cycloheptadecenone gives Civetone after hydrolysis followed by decarboxylation with 95% yield.
SUMMARY
The invention describes certain naturally-derived (bio-based) products and systems and methods for synthesizing civetone and other products from an omega-7 containing composition. The term “bio-based” or “naturally-derived” means that the compounds are synthesized from recently-living biological materials rather than petrochemical feedstocks. In this way, the compounds and methods offer a significant advantage over petro-based components in that they remove carbon from the atmosphere. Practically, bio-based materials can be distinguished from petrochemical-based materials by the well known techniques of 14 C dating. Bio-based materials will have significant levels of 14 C that are typical of biological material that was living within the past few hundred years. In contrast, petro-based compounds will have essentially zero 14 C.
In a first aspect (see FIG. 5 ), the invention provides a method of converting a mixture comprising derivatives of palmitoleic acid and oleic acid to useful products including olefinic hydrocarbons, comprising: reacting a composition comprising an ester of palmitoleic acid and an ester of oleic acid in a metathesis reaction to produce a first reaction mixture; reacting at least a portion of the first reaction mixture, or derivatives thereof, in a cyclization reaction to produce a second reaction mixture; hydrolyzing and decarboxylating at least a portion of the second reaction mixture, or derivatives thereof, to produce a third reaction mixture comprising civetone. The phrase “or derivatives thereof” means that the reaction mixtures can be modified by treatments, such as transesterifications, that do not have a significant deleterious effect on subsequent synthesis steps. This method yields civetone along with at least one olefinic compound selected from the group of Olefin D (C 14 H 28 see FIG. 6 ), and Olefin C (C 16 H 32 see FIG. 6 ), and 1-Octene (C 8 H 16 ). In practice, of course, any of the reaction co-products can be separated or used as intermediates in further reactions—products that are separated or consumed as intermediates in a further reaction are still included in calculations of yield and selectivity.
The “esters” referred to are generally made by esterification or transesterification of precursor composition comprising palmitoleic acid and oleic acid. A preferred precursor composition comprises a mixture of palmitoleic acid C16:1 (C 16 H 30 O 2 ) and oleic acid C18:1 (C 18 H 34 O 2 ), which is a mixture that can be obtained in an extract from sources such as algae, sea buckthorn, and macademia. In one preferred embodiment, the precursor composition is derived from algae.
In some preferred embodiments, the esters are produced by esterification or transesterification in the presence of a catalyst such as an enzymatic, acidic, basic, and/or heterogeneous catalyst. In some embodiments the esters comprise methyl esters or ethyl esters.
In some of the inventive aspects, the invention can be further characterized one or more of any of the following: the palmitoleic acid and oleic acid are present in the precursor composition in at least 50 mass % as a percentage of the total mass of unsaturated fatty acids, in some embodiments, at least 80%, and in some embodiments at least 90% as a percentage of the total mass of unsaturated fatty acids. Likewise, the composition of esters preferably contains at least 50 mass % (in some embodiments at least 80%, or at least 90%) of C16 palmitoleic-acid-derived esters and C18 oleic-acid-derived esters as a mass percentage of all fatty acid esters present in the composition. The mass percent of palmitoleic acid (or the corresponding esters) as a percent of the sum of palmitoleic acid plus oleic acid (or the corresponding esters) is preferably in the range of 20 to 80%, in some embodiments 30 to 70%, in some embodiments 40 to 60%, in some embodiments, 20 to 50%, in some embodiments 50 to 80%. These characteristics can be present individually or in combination.
In some embodiments, the precursor composition or composition comprises about equal parts palmitoleic acid and oleic acid or (in the composition) their corresponding fatty acid esters (i.e., each is within the range of 45 to 55% of their total mass). In some embodiments, the precursor composition or composition comprises a greater portion of palmitoleic acid (or esters) than oleic acid (or esters). In some embodiments, the composition comprises a greater portion of oleic acid ester(s) than palmitoleic acid ester(s). In some preferred embodiments, the C16 and C18 fatty acids or corresponding esters in the precursor composition or composition comprises at least 50 mass % (absolute) of the total mass of the precursor composition or composition, in some embodiments at least 70% or at least 80%, and in some embodiments up to 99% or 100%.
At any stage of the method, selected products can be separated or purified by known methods; for example, silica gel chromatography or HPLC. The invention includes any of the products or reaction mixtures in purified form. For example, any of the chemical compounds can be obtained in forms that are at least 50 mass % pure (i.e., no more than 50 mass % of components other than those listed in a claim). For example, if a mixture is described as “comprising 1-octene, 1-decene, and ethyl 9-decenoate,” then the invention also includes (in more specific embodiments) a mixture comprising at least 50 mass % of 1-octene, 1-decene, and ethyl 9-decenoate. Likewise, the invention includes compositions comprising at least 50 mass % of any of the specific products and intermediates described herein, since it is contemplated that any of the products or intermediates can be isolated. In some preferred embodiments, any of the compounds or mixtures are at least 80% (by mass) pure, in some embodiments at least 99% pure.
In some embodiments, the metathesis reaction is a self-metathesis reaction producing a reaction mixture comprising C 18 H 36 , C 14 H 28 , and C 22 H 40 O 4 . In some embodiments, the metathesis reaction is a cross-metathesis reaction producing a reaction mixture comprising C 16 H 32 and C 22 H 40 O 4 . In some embodiments, the metathesis reaction comprises a catalytic system selected from the group consisting of: WCl 6 /Me 4 Sn; Heterogeneous Re 2 O 7 /Al 2 O 3 (rhenium oxide on alumina); Heterogeneous Re 2 O 7 /SiO 2 .Al 2 O 3 /SnBu4; W(O-2,6-C 6 H 3 X 2 )2Cl 4 (X=Cl, Ph) precatalysts promoted with Me 4 Sn; B 2 O 3 .Re 2 O 7 /Al 2 O 3 .SiO 2 /SnBu 4 ; WCl 6 and WOCl 4 , as primary catalysts and SnMe 4 , PbMe 4 , Cp 2 TiMe 2 , and Cp 2 ZrMe 2 , as cocatalysts; Ruthenium based catalyst; Grubb's catalyst first generation; Grubbs catalyst second generation; and Hoveyda-Grubbs catalyst. In some preferred embodiments, the metathesis catalyst comprises rhenium oxide, preferably supported on alumina or an aluminosilicate.
In some embodiments, the cyclization reaction comprises Dieckmann condensation. In some embodiments, the cyclization reaction is carried out with metal hydrides under inert conditions. In some embodiments, the cyclization reaction is carried out with TiO 2 doped with alkali or alkaline earth metal oxides in gaseous phase reaction. In some embodiments, the cyclization reaction comprises Ti-Dieckmann or Ti-Claisen condensation.
In some embodiments, civetone is extracted from the product mixture using ether. In further embodiments, the extracted civetone can be further purified, for example, by using silica-gel chromatography. In some embodiments, the Ti-Dieckmann cyclization forms a reaction mixture comprising 34-membered macrocyclic ketones. In some embodiments, the method includes a hydrogenation reaction of the C 22 H 40 O 4 to produce a reaction mixture and followed by a cyclization step to produce dihydrocivetone (cycloheptadecanone).
In another embodiment, fatty acid esters of palmitoleic acid and oleic acid are reacted with ethene to produce a reaction mixture; and subsequently reacting at least a portion of this reaction mixture (or a derivative thereof) in a condensation reaction; and then conducting a second metathesis reaction, followed by hydrolysis and decarboxylation to produce civetone and 1-Octene (C 8 H 16 ).
In some embodiments, the metathesis reaction with ethene produces a mixture comprising 1-Octene (C 8 H 16 ), 1-Decene (C 10 H 20 ), and ethyl 9-decenoate (C 12 H 22 O 2 ). In some embodiments the condensation reaction is a Ti-Claisen condensation with a catalysis system selected from the group consisting of: TiCl 4 —Bu 3 N, Pentafluorophenylammonium Triflate, and MgBr 2 .OEt 2 in DIPEA. In some embodiments, the metathesis reaction of the condensation produces ethene and a macrocyclic compound. In some embodiments, the macrocylcic compound is 2-ethoxycarbonyl-9-cycloheptadecenone. In some preferred embodiments, the ethene produced is recycled to the step of reacting the esters in a metathesis reaction with ethene. In some embodiments, the condensation product comprises a beta-ketoester. In further embodiments, the beta-ketoester can be purified, for example by extraction ether and optional additional steps such as chromatography, for example, silica-gel chromatography.
In further aspects of the invention, the invention provides a method of producing olefins. In this method, fatty acid esters of the unsaturated fatty acids C16:1 (C 16 H 30 O 2 ) and C18:1 (C 18 H 34 O 2 ) are reacted in a metathesis reaction to produce a reaction mixture comprising C 18 H 36 , C 14 H 28 , C 16 H 32 and C 22 H 40 O 4 . The invention also includes compositions that comprise a mixture of the biobased olefins Olefin E (C 18 H 36 see FIG. 6 ), Olefin D (C 14 H 28 see FIG. 6 ), and Olefin C (C 16 H 32 see FIG. 6 ). The invention further includes compositions comprising the individual biobased Olefin C, Olefin D and mixtures thereof, made by methods of the present invention. In some preferred embodiments the composition comprises at least 10% of Olefin C or Olefin D as a percentage of all olefins in a composition; in some embodiments at least and 10% of Olefin C and at least 10% Olefin D; in some embodiments at least 20% of Olefin C or Olefin D; at least 20% of Olefin C and at least 20% of Olefin D; in some embodiments, 5% to 50% of Olefin C; in some embodiments 5% to 50% of Olefin D; all as a percentage of the total mass of olefins in the composition. In some preferred embodiments, the composition comprises at least 5 mass % of olefins; at least 10 mass % olefins; at least 20 mass % olefins; or at least 50 mass % based on total mass of the composition. In each case, the olefins are biobased which is a significant advantage over petrochemical derived olefins. The compositions can be used in the synthesis of polymers or chemical compounds, and can be used as a fuel additive, for example, to increase octane rating.
In any of its aspects, the invention may also be characterized by yields. In each case, yield is calculated based on carbon in the selected product or intermediate and in the monounsaturated fatty acid esters present in a starting material composition. In the reactions carried out using metathesis of the palmitoleic and oleic acid esters, the yield of Diester F (see FIG. 6 below) is preferably greater than 20%, more preferably at least 30%, in some embodiments in the range of 30 to about 60%, and in some embodiments 40 to 55%. In the reactions carried out using metathesis of the palmitoleic and oleic acid esters, the yield of the sum of Olefins C, D, and E (see FIG. 6 below) is preferably at least 20%, more preferably at least 30%, in some embodiments 30 to 44%, in some embodiments 35 to 43%, and in some embodiments 38 to 43%. In some embodiments, the yield of Olefin C is at least 5%, in some embodiments at least 10%, in some embodiments, at least 15%, in some embodiments in the range of 10% to 20%. In some embodiments, the yield of Olefin D is at least 5%, in some embodiments at least 10%, in some embodiments, at least 15%, in some embodiments at least 20%, in some embodiments at least 25%, in some embodiments in the range of 10% to about 38%, in some embodiments in the range of 10% to 30%, in some embodiments in the range of 15% to 25%. Note that, using the above definition of yield, in the noninventive case of pure oleic acid ester as the starting material, the maximum theoretical yields of Diester F and Olefin E would be 55 and 45%, respectively. For the cyclization of Diester F, the yield of cyclized intermediate is preferably at least 60%, in some embodiments in the range of 60 to 95%. For the combined steps of hydrolysis and decarboxylation the yield of civetone is preferably at least 60%, in some embodiments in the range of 60 to 95%.
In the reactions carried out using metathesis with ethene, the yield of ethyl 9-decenoate is preferably at least 30%, more preferably at least 40%, in some embodiments in the range of 30 to about 65%, in some embodiments 35 to 60% (carbon in ethyl 9-decenoate divided by carbon in starting materials. Note that, using the present carbon-based definition, for the noninventive case of pure oleic acid the maximum theoretical yield of ethyl 9-decenoate is 55%. The yield of 1-octene is preferably at least 5%, in some embodiments at least 10%, in some embodiments at least 15%, in some embodiments at least 20%, in some embodiments in the range of 10 to 40%, in some embodiments 10 to 35%, in some embodiments 15 to 30%. The yield of 1-decene is preferably at least 5%, in some embodiments at least 10%, in some embodiments at least 15%, in some embodiments at least 20%, in some embodiments in the range of 10 to 40%, in some embodiments 10 to 35%, in some embodiments 15 to 30%. The yield of the condensation of ethyl 9-decenoate is preferably at least 60%, in some embodiments 60 to 95%. The yield of the cyclized compound from metathesis of the beta-ketoester is civetone is preferably at least 60%, in some embodiments in the range of 60 to 95%. For the combined steps of hydrolysis and decarboxylation the yield of civetone is preferably at least 60%, in some embodiments in the range of 60 to 95%.
In preferred embodiments, the invention has an overall yield, based on carbon in the products (civetone plus olefinic hydrocarbons) divided by the sum of carbon in the palmitoleic acid ester and oleic acid ester starting materials of greater than 25%, preferably greater than 50%, preferably greater than 60%, in some embodiments in the range of 40% to 80%, in some embodiments greater than 60% to 95%, in some embodiments greater than 60% to 85%, in some embodiments at least 70%, in some embodiments 75 to 90%.
In another aspect, the invention provides a method of producing α-olefins, comprising: producing esters from an composition comprising at least 50 mass % of palmitoleic acid and oleic acid; and reacting at least a portion of the esters in a metathesis reaction with ethene to produce a reaction mixture comprising 1-Octene (C 8 H 16 ), 1-Decene (C 10 H 20 ), and ethyl 9-decenoate (C 12 H 22 O 2 ).
In yet another aspect, the invention provides a method of synthesizing dihydrocivetone. In this method, civetone is made as described herein and then hydrogenated to produce dihydrocivetone.
In yet another aspect, the invention provides a method of synthesizing cyclopropanated civetone. In this method, civetone is made as described herein and then reacted in a Simmons-Smith reaction using ZnCu and CH 2 I 2 to produce cyclopropanated civetone.
In still further embodiments, certain melanin production inhibitors (described herein) are produced. In some embodiments, an acyloin condensation of diethyl 9-octadecenedioate produces a 2-hydroxy macrocyclic ketones which is subsequently converted to melanin production inhibitors. In some embodiments, reducing civetone produces melanin production inhibitors. The reduction may include hydrogenation to make civetol.
In various embodiments, the invention can provide advantages such as: the production of civetone and other high value products from algae-derived products; greater efficiency in fully utilizing starting materials; the ability to make valuable products such as olefins, polyolefins, and precursors for lubricants, olefins, polymers, and plasticizers; and the synthesis of environmentally-friendly, biobased olefins.
As is standard patent terminology, the term “comprising” means “including” and permits the presence of additional components. Where the invention is characterized as “comprising” it should be understand that the invention, in narrower embodiments, can alternatively be characterized as “consisting essentially of” or “consisting of” in place of “comprising.” Such language limits the invention to the named components plus components that do not materially degrade the properties of the invention, or narrow the invention to only the stated components, respectively. In the descriptions of the invention, the phrase “such as” should be understood as not limiting but only providing some non-limiting examples.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 illustrates examples of synthesis of esters from oil and separation into fractions based on fatty acid chain length.
FIG. 2 illustrates a known method of synthesizing civetone from palm oil.
FIG. 3 illustrates a known method for the ethenolysis of methyl oleate.
FIG. 4 illustrates a known method of synthesizing civetone from methyl 9-decenoate.
FIG. 5 illustrates a method for synthesizing civetone
FIG. 6 illustrates products produced in the Metathesis of Palmitoleic acid and Oleic acid.
FIG. 7 is a side-by-side comparison of metathesis stage of a prior art process of synthesizing civetone from palm oil (left) and the invention method (1) of synthesizing civetone and new polyolefin products from Omega-7 rich oil (right).
FIG. 8 illustrates ethenolysis of a mixture of ethyl esters of Palmitoleic acid (C16:1) and Oleic acid (C18:1).
FIG. 9 illustrates metathesis, hydrolyzation, and decarboxylation to make civetone.
FIG. 10 illustrates products from metathesis reactions of Omega-7 fraction in invention method 1.
FIG. 11 illustrates alkylation of civetone macrocycle.
FIG. 12 illustrates the synthesis of melanin-production-inhibiting products from the acyloin condensation of civetone.
DETAILED DESCRIPTION
In some preferred embodiments, a mixture comprising Palmitoleic acid (C16:1) and Oleic acid (C18:1) is used as a precursor for synthesis of Civetone. Preferably, the mixture of palmitoleic acid and oleic acid is obtained by transesterification of an Omega-7 rich oil followed by molecular distillation and is termed “the Omega-7 rich fraction”.
Metathesis of Palmitoleic Acid and Oleic Acid:
Methathesis:
A fraction of fatty acids that can be obtained from biomaterials such as algae or plants is a mixture of ethyl esters Palmitoleic acid (C16:1) and Oleic acid (C18:1). The metathesis of this composition will produce a unique mixture of products, not available through prior art methods. Referring to FIG. 6 , the Omega 7 fraction self-metathesis of the Palmitoleic acid ester (A) will yield olefin (D), and Diethyl ester (F) as products. The products will also include self-metathesis products of the Oleic acid esters (B), which are olefin (E) and Diethyl ester (F). The Omega 7 fraction will also undergo a cross metathesis reaction between the Palmitoleic acid ester (A) and the Oleic acid ester (B) to give olefin (C), a product not available through prior art methods, and Diethyl ester (F).
The Palmitoleic acid of the Omega-7 rich fraction is derived from sources such as sea buckthorn and macadamia oil, but not palm oil. Therefore the olefin metathesis reaction of the Omega-7 rich oil will give unique products which are not obtainable by the prior art methods comprising olefin metathesis of ethyl oleate obtained from palm oil, as shown in FIG. 7 .
Cyclization:
The diethyl ester (product F in FIG. 6 ) produced from the metathesis stage can be cyclized using Dieckmann condensation or its variant.
Hydrolysis and Decarboxylation:
The cyclized compound can be hydrolyzed and decarboxylated to form civetone.
Ethenolysis:
Ethenolysis comprises a cross-metathesis reaction involving ethene. According to some preferred embodiments of the invention, a mixture of ethyl esters of Palmitoleic acid (C16:1) and Oleic acid (C18:1) are subjected to conditions of ethenolysis to yield a mixture of α-olefins (1-Octene and 1-Decene) and Methyl 9-Decenoate. See FIG. 8 . The 1-Octene is a product unique to ethenolysis of Palmitoleic acid (C16:1). In the inventive method, Ethyl 9-Decenoate and 1-Decene will also form from the mixture of Palmitoleic and Oleic acid ethyl esters. Prior art methods using Oleic acid esters (Methyl Oleate) as the starting material only produce Methyl 9-Decenoate and 1-Decene.
Condensation:
The Ethyl 9-Decanoate (see above) can be subjected to a Claisen condensation.
Intramolecular Metathesis:
The product of the condensation stage can be subjected to an intramolecular metathesis reaction to produce ethane gas and a macrocyclic compound, such as 2-ethoxycarbonyl-9-cycloheptadecenone. The ethene gas can be recycled to the ethenolysis step for use in the ethenolysis reaction.
Hydrolyization and Decarboxylation:
The macrocyclic beta-ketoester compound can be hydrolyzed and decarboxylated to form civetone.
Examples
Contemplated
Invention Embodiment 1 Example
Metathesis of Omega-7 Fraction
The 2 nd generation ruthenium catalyst (IMesH 2 )(PCy 3 )(Cl) 2 Ru═CHPh where IMesH 2 is 1,3-dimesityl-4,5-di-hydroimidazol-2-ylidene with its bulky N-heterocyclic carbine (NHC) ligand (Dinger & Mol, 2002) is known to perform with high turnover numbers and gives the product with high selectivity and can be an ideal catalyst for metathesis of Omega-7 fraction. The reaction will be carried out in inert atmosphere at about 55° C. The products Diethyl 9-Octadecenedioate and mixture of olefins formed in this reaction will be purified by silica-gel chromatography. See FIG. 10 .
Metathesis Catalysts:
In oleochemistry, olefin metathesis is well known and it includes self-metathesis (SM), cross-metathesis (CM), ring closing metathesis (RCM), ring-opening metathesis (ROM) and ROM polymerization (ROMP) as well as acyclic diene metathesis polymerization (ADMET) reactions. A variety of catalytic systems can be utilized for metathesis of Omega-7 fraction to achieve selectivity and high turnover numbers, such as:
WCl 6 /Heterogeneous Re 2 O 7 /A l2O3 Heterogeneous Re 2 O 7 /SiO 2 .Al 2 O 3 /SnBu 4 W(O-2,6-C 6 H 3 X 2 )2Cl 4 (X=Cl, Ph) precatalysts promoted with Me 4 Sn B 2 O 3 .Re 2 O 7 /Al 2 O 3 .SiO 2 /SnBu 4 WCl 6 and WOCl 4 , as primary catalysts and SnMe 4 , PbMe 4 , Cp 2 TiMe 2 , and Cp 2 ZrMe 2 , as cocatalysts, Ruthenium based catalysts (Grubb's catalyst first, second generation and Hoveyda-Grubbs catalyst).
Table 1 illustrates examples of catalysts which can be used to perform metathesis of the omega-7 fraction (Mol, 2002).
TABLE 1
Examples of catalyst system for metathesis of (m)ethyl oleate
Catalyst
Ester/metal atom a
T/° C.
t b /h
TON c
Ref.
Homogeneous systems
WCl 4 /Me 4 Sn
75
110
2
38
26
W(OC 6 H 3 Cl 2 -2,6) 2 Cl 4 /Bu 4 Pb
50
85
0.5
25
30
W(═CHCMe 3 )NpCl(OAr) 2 (OEt 2 ) d
100
85
1
32
31
[W]═CHCMe 3 (see formula I)
300
25
2-3
150
32
[W]═CHCMe 3 (see formula II)
500
25
1
250
33
Ru(═CH—CH═CPh 2 )Cl 2 (PCy 3 ) 2
2 000
20
96
960
34
Ru(═CHPh)Cl 2 (PCy 3 ) 2
5 500
20
48
2 500
35
[Ru 2 ]═CHPh(III, R′ = CF 3 )
550
40
1
225
36
Ru(═CHPh)Cl 2 (H 2 IMes)(PCy 3 ) (IV) c
987 000
55
6
440 000
48
Heterogeneous systems
Re 2 O 7 /Al 2 O 3 /Et 4 Sn
60
20
2
3
18
Re 2 O 7 /MoO 3 /Al 2 O 3 /Et 4 Sn
60
20
2
30
18
Re 2 O 7 /B 2 O 3 /Al 2 O 3 /Bu 4 Sn
120
20
2
50
37
Re 2 O 7 /SiO 2 —Al 2 O 3 /Bu 4 Sn
240
40
2
120
10
Re 2 O 7 /B 2 O 3 /SiO 2 —Al 2 O 3 /Bu 4 Sn f
480
20
2
160
38
Re 2 O 7 /B 2 O 3 /SiO 2 —Al 2 O 3 /Bu 4 Sn g
200
80
2
99
39
CH 3 ReO 3 /SiO 2 —Al 2 O 3
100
25
2
27
40
MoO 3 /SiO 2 /(CO, hv)/cyclopropane
250
50
0.17
25
41
MoO 3 /SiO 2 /(CO, laser)/cyclopropane
1 250
40
3
500
10
a Molar ratio.
b t = Time to reach the highest conversion.
c TON = Moles of substrate converted per mol of W, Ru, Re or Mo into reaction products.
d Ar = C 6 H 3 Ph 2 -2,6; Np = CH 2 CMe 3 .
e No solvent.
f Silica-alumina containing ~25 wt % Al 2 O 3 .
g Silica-alumina containing 60 wt % Al 2 O 3 .
Dieckmann Condensation (Macrocyclization):
Ti-Dieckmann (intramolecular Ti-Claisen) condensation (Hamasaki et al., 2000; Tanabe, Makita, Funakoshi, Hamasaki, & Kawakusu, 2002a; “U.S. Pat. No. 6,861,551.pdf,” n.d.) (TiCl 4 /amine) will be used to cyclize Diethyl 9-Octadecenedioate. The reaction will be carried out at around 0-5° C. for about 1 hour to give the cyclized product 2-ethoxycarbonyl-9-cycloheptadecenone which can be purified by silica-gel chromatography. The same macro cyclization (Dieckmann condensation) can be carried out in different conditions:
KH or NaH (metal hydrides) under inert conditions. TiO 2 doped with alkali or alkaline earth metal oxides (Na 2 O or K 2 O) in gaseous phase reaction. ZrCl 4 /Bu 3 N similar to Ti-Dieckmann condensation.
Hydrolysis and Decarboxylation:
2-ethoxycarbonyl-9-cycloheptadecenone will be refluxed with about 10% NaOH in methanol for about 1 hour to give civetone. After completion of the reaction, the reaction mixture will be neutralized using about 10% sulfuric acid. The product will be extracted using ether and can be purified using silica-gel chromatography.
Hydrolysis and Decarboxylation to Form Civetone
Invention Embodiment 2 Example
Ethenolysis of Omega-7 Fraction
Ethenolysis Reaction of Omega 7 Fraction
Catalysts for Use in Ethenolysis Reaction of Omega 7 Fraction
Ethenolysis of the Omega-7 fraction will be carried out under inert atmosphere with ethylene under conditions of about 150 psi pressure and about 40° C. (Thomas et al., 2011). N-Aryl,N-alkyl N-heterocyclic carbene (NHC) ruthenium metathesis catalysts are highly selective toward the ethenolysis of methyl oleate. The catalysts shown in FIG. 16 , (A) and (B), give more kinetic selectivity when catalyst loading was ≈500 ppm due to their sterically demanding ligands. Catalyst A-88% selectivity with 78% yield while catalyst B with 88% selectivity and 77% yield. The products will be separated using silica gel chromatography.
Similar to the Invention embodiment 1 example, a metathesis reaction can be performed by selecting a catalyst from a variety of metathesis catalysts (Table 1).
Ti-Claisen Condensation of Ethyl-9-Decenoate:
Ti-Claisen condensation (Hamasaki et al., 2000) will be performed by adding TiCl4 to mixture of Bu 3 N and Ethyl decenoate at around 0-5° C. The reaction mixture will be stirred for approximately 1 hour and then will be quenched by the addition of water. The product β-ketoester will be extracted using ether and will be purified by silica-gel chromatography.
Intramolecular Metathesis Reaction, Hydrolysis and Decarboxylation:
The intramolecular metathesis reaction will be similar to the Invention embodiment 1 example metathesis reaction of an Omega-7 fraction. The metathesis reaction can be carried out with a selected catalyst as described above. The hydrolysis and decarboxylation will be carried out as described above.
Additional Embodiments
Potential Products from Invention Methods of Synthesizing Civetone Relevant to Perfume Industry (Macrocyclic Ketone)
The Invention methods disclosed above for synthesizing civetone will give geometrical isomers of the final product which are Cis-Civetone and Trans-Civetone.
Invention embodiment 1 cyclization mediated Ti-Dieckmann conditions (Tanabe, Makita, Funakoshi, Hamasaki, & Kawakusu, 2002a) will predominately give Z-isomer of Civetone with approximately 50% yield. Invention embodiment 2 intramolecular metathesis will give a mixture of E:Z (3:1) isomers of Civetone with 90% yield (Hamasaki et al., 2000).
Ti-Dieckmann cyclization conditions may lead to the formation of 34-membered macrocyclic ketones, which have potential uses in the perfume industry. The 34-membered macrocycle can be formed using TiCl 4 -Et 3 N, with approximately 14% yield (Tanabe, Makita, Funakoshi, Hamasaki, & Kawakusu, 2002b).
Dihydrocivetone (Cycloheptadecanone) is another macrocyclic ketone with musk fragrance and can be synthesized by hydrogenation of the final product (Civetone) or by hydrogenation of Diethyl 9-Octadecenedioate followed by cyclization.
In 2011 International Flavors & Fragrances Inc. introduced a new class of chemical entities cyclopropanated macrocycles (see U.S. Pat. No. 7,943,560) as flavors and fragrances. Civetone (both geometrical isomers) can undergo Simmons-Smith reaction using ZnCu and CH 2 I 2 to give cyclopropanated Civetone.
Alkylation:
Muscone (3-Methyl cyclopentadecanone) is methylated macrocycle with musk fragrance. Civetone macrocycle can be alkylated (methylated) to give 2-methyl 9-Cycloheptadecen-1-one which can be potential product for perfume industry. Alkylation reaction can be done using Stork enamine conditions to substitute the macrocycles with different alkyl groups. See FIG. 11 .
Macrocycles with Potential Melanin Production Inhibition Activity which can be Used in Skin Care Products (“Melanin Production Inhibitors,” n.d.):
Diethyl 9-Octadecenedioate product from Invention embodiment 1 can undergo Acyloin condensation to give 2-hydroxy macrocyclic ketones, which can inhibit Melanin production, as shown in FIG. 12 . Civetone can be reduced to give product C, which is a potential melanin production inhibitor, and hydrogenation of Product C gives Civetol D.
LITERATURE
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The invention describes methods and systems for making particular organic compounds from unsaturated fatty acids derived from biological materials. Particular embodiments describe synthesizing civetone and olefins from a mixture of palmitoleic and oleic unsaturated fatty acid esters. The inventive methods use reaction steps such as metathesis, cyclization, hydrolysis, and/or decarboxylation.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] The present application is a continuation of International Application PCT/EP02/02326 filed Mar. 4, 2002, the entire content of which is expressly incorporated herein by reference thereto.
BACKGROUND
[0002] The present invention pertains to novel strains of lactic acid bacteria capable of reducing an individual's tendency to develop allergic reactions. In particular, the present invention relates to recombinant strains of lactic acid bacteria expressing surface polypeptides which include small and larger peptides acting as mimics for at least a part of the F c region of immunoglobulin E (IgE)-molecules. The invention also pertains to food or pharmaceutical compositions containing said micro-organisrns or active fractions thereof.
[0003] The immune system is a complex and multifactorial defense system that protects the body from any invasive biological or chemical agent, such as viruses, bacteria, parasites and fungi or simply larger chemical substances. Although being indispensable for maintaining the body's integrity, the immune system may in certain cases be the cause of the illness itself, such as in autoimmune diseases, inflammation or allergies.
[0004] Allergies are inappropriate reactions of the immune system to a variety of substances (allergens). Generally, individuals do not generate a significant immune reaction against substances regularly encountered in the environment, such as pollen or food material, which non-reactivity is deemed to be mainly due to a suppressing mechanism of the immune system itself However, in an impaired condition the immune system does not fulfil said suppressing activity resulting in a specific immune reaction against the allergen—the allergic reaction.
[0005] A generally established mechanism of allergic reactions involves a sequence of events beginning with the uptake of the allergen which needs to pass the epithelial barrier to reach and activate effector cells, located in the lamina propria or epithelium below the level of the tight junctions. The clinical symptoms associated with allergic reactions are basically the result of an early specific immune response and a late inflammatory reaction. During the early phase immunoglobulines E (IgE) against the allergenic substance are produced by the host's immune system, which are subsequently bound via a receptor protein to e.g. mast cells and basophils. Upon binding and crosslinking the IgE molecules on their surface the cells release histamine and cytokines, which then mediate the late phase by recruiting inflammatory cells into the nasal and upper respiratory tract passages. The influx of eosinophils, macrophages, lymphocytes, neutrophils and platelets subsequently starts the inflammatory cycle amplifying the initial immune response which in turn triggers the release of more inflammatory cells.
[0006] In the past, the number of individuals suffering from allergy has increased, which is frequently attributed to an ever increasing atmospheric pollution caused by e.g. exhaust gases. Also, an extended consumption of proteinaceous material is deemed to contribute to said development, in particular to the growing occurrence of food allergy. Further, the deficit in microbial infections encountered in developed countries has also been suggested as another possible cause for the increase of atopic diseases.
[0007] Therefore, there exists a need in the art to treat allergy, for which different approaches have been proposed so far.
[0008] As for the treatment of food allergy some methods rely on modifying the food material itself such that its allergenic potential is reduced. This may be achieved by altering the chemical structure thereof, or by limiting or banning the food material or components thereof, respectively, which would be the cause of such trouble. Yet, a problem involved often resides in that the specific allergenic substance in the respective food material is frequently not known so that in most cases it is not clear which component should be selectively removed or altered.
[0009] A different approach of treating food allergy and food intolerance is directed to restoring and maintaining the intestine's integrity such that food allergens essentially may not pass. In this respect, U.S. Pat. No. 5,192,750 describes the use of N-acetyl glucosamine to enable the mucosa to form the necessary barrier to transmission of food allergens and to maintain normal function.
[0010] A most general approach of treating allergy is an immunotherapy which involves repeated injection of the allergen, over a period of several years, to desensitize a patient to the allergen. Proceeding accordingly is, however, time consuming, involves years of treatment, and often fails to achieve its goal of desensitizing the patient.
[0011] According to a more recent approach, vaccination of individuals against IgE molecules is suggested which inhibits triggering of mast cells and basophils. To this end, WO 97/31948 proposes specific peptides for vaccination that resemble in their three dimensional conformation parts of the IgE molecule, i.e. the immunoglobulines involved in the release of mediators, that play a part in the regulation of allergic and inflammatory reactions. It is conceived that the individual's own immune system will eventually form antibodies directed to said IgE molecules such that said IgE immunoglobulines are scavenged.
[0012] However, said method harbours the disadvantage common to normal vaccination procedures in that the biologically active substance has to be administered by invasive methods, such as e.g. by intraveneous injection, which route of administration is generically disliked by patients. On the other hand, when choosing the oral route, suitable galenic formulas have to be designed to allow the biologically active substance to pass the gastro-intestinal tract without getting destroyed. Another problem encountered in this method resides in that the mimotopes are, in most of the cases, short length peptides, that on their own will not elicit a substantial immune response so that apart from carriers and excipients adjuvantia have to be included in the composition.
[0013] Therefore, there is a need in the art to provide improved means for treating allergy. In particular, an object of the present invention resides in providing means that allow treatment of allergy in an efficient, easy and cost effective manner preferably without requiring a physician and without bringing about the negative associations linked with such treatments.
SUMMARY OF THE INVENTION
[0014] The present invention now resolves these problems by providing novel lactic acid bacteria strains that express on their surface a polypeptide containing at least one peptide sequence mimicking at least part of a conformational epitope (mimotope) of an IgE molecule. The bacterial strain is preferably selected from Lactobacillus group or Bifidobacterium group or Lactococcus group, and is more preferably derived from the groups of L. acidophilus, L. johnsonii, L. gasseri, L. casei, L. paracasei or L. reuteri.
[0015] Preferably, the bacterial strain is included in a food composition, such as a milk, yoghurt, curd, cheese, fermented milks, milk based fermented products, ice cream, fermented cereal based products, milk based powders, infant formulae or pet food, wherein the bacterial strain is contained therein in an amount ranging from 10 7 to 10 12 cfu (colony formation unit) per dosage form.
[0016] The invention also relates to a method of making an ingestible carrier for the treatment of allergy or prevention of the onset of allergic reactions which comprises adding a bacterial strain as described herein to a suitable carrier. In particular, the suitable carrier is a food composition such as one of those mentioned herein.
[0017] Yet another embodiment of the invention relates to a method for the treatment of allergy or prevention of the onset of allergic reactions which comprises administering to a subject in need of such treatment one of the ingestible carriers or food compositions disclosed herein. The subjects are typically mammals such as humans or animals.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] The accompanying drawings, which are incorporated in and form a part of the specifications, illustrate the preferred embodiments of the present invention, and together with the description serve to explain the principles of the invention. In the drawing figures,
[0019] [0019]FIG. 1 shows a protein stain and Immunoblot analysis of Lactobacillus johnsonii recombinants. (A) Protein stain of La1 wild type (lane 1), La1 carrying pMD112TT (La1TT, lane 2) or pMD112ε4 (La1ε4, lane 3). (B) Expression of proteinase PrtB (SEQ ID NO:2) on La1TT (lane 2) and La1ε4 (lane 3). Approximately 10 8 bacteria were analyzed by immunoblot using anti-PrtB serum diluted 1:2000. Wild type La1 was loaded as a negative control (lane 1). Binding antibodies were detected with horseradish peroxidase conjugated goat anti-rabbit IgG (Fc) antibodies. (C) Expression of tetanus mimotope on the surface of La1TT (lane 2). Approximately 10 8 bacteria per slot were analyzed by immunoblot using anti-TT serum diluted 1:1000. La1 (lane 1) and La1ε4 (lane 3) were used as negative controls. Binding antibodies were detected with horseradish peroxidase conjugated goat anti-rabbit IgG (Fc) antibodies. (D) Expression of ε4 mimotope on the surface of La1ε4 (lane 3). Approximately 108 bacteria per slot were analyzed by immunoblot using anti-E4 serum (SDS280) at a concentration of 10 μg/ml. La1 (lane 1) and La1TT (lane 2) were used as negative controls. Binding antibodies were detected with horseradish peroxidase conjugated goat anti-rabbit IgG (Fc) antibodies. The arrow indicates the height of the proteinase band seen in A-D.
[0020] [0020]FIG. 2 shows the result of an binding assay of anti TT IgG to surface displayed epsilon mimotopes on lactic acid bacteria in ELISA.
[0021] [0021]FIG. 3 shows the result of an binding assay of anti-ε4 IgG to surface displayed epsilon mimotopes on lactic acid bacteria in ELISA.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0022] In the studies leading to the present invention it has now been found that by providing a lactic acid bacterium containing a recombinant surface polypeptide comprising a peptide sequence as defined above a specific immunization of an individual against IgE may be obtained, with the result that allergic reactions of said individuals to essentially all antigens are suppressed.
[0023] Without wishing to be bound to any theory it is presently envisaged that the lactic acid bacteria, that upon ingestion remain in the gastro-intestinal tract for a period of time, are capable of presenting the antigen to an individual's immune system such that an effective immune reaction takes place leading to the formation of anti-IgE antibodies in the individual. This fact is all the more surprising, since it could not be predicted, whether administration of a bacterium to an individual, which is effected via the gastro-intestinal route, containing such a surface protein, would eventually present the corresponding antigen—the mimotope—to the individual's immune system such that the immune system will be capable of recognizing the antigen and elicit an immune response thereto. What is more, the biological environment, wherein the mimotope is presented to the immune system is such that the use of adjuvantia for eliciting an immune response against the antigen is not required.
[0024] According to a preferred embodiment the lactic acid bacterium containing a surface polypeptide containing the mimotope belongs to the Lactobacillus group or Bifidobacterium group or Lactococcus group, and is more preferably derived from the groups of L. acidophilus, L. johnsonii, L. gasseri, L. casei, L. paracasei or L. reuteri , all of human or animal origin. According to a more preferred embodiment the lactic acid bacterium is a probiotic lactic acid bacterium. As probiotics micro-organisms shall be understood capable to pass the gastro-intestinal tract in an essentially viable and live form and optionally also be capable of stimulating the host's immune system. According to a most preferred embodiment the lactic acid bacteria is Lactobacillus johnsonii.
[0025] The nature of the surface polypeptide is not crucial with the proviso that the “mimotope peptide sequence” may be inserted such that it is accessible for the immune system. According to a preferred embodiment the surface polypeptide/protein, into which a sequence mimicking a conformational epitope of an IgE immuno-globuline is inserted, is the cell surface anchored protease of Lactobacillus bulgaricus the sequence of which was published in Gilbert et al., (1996) J. Bacteriol, 178, 3059-3065. This protein was characterized as a 2000 amino acids protein, being composed of a leader peptide of 33 amino acids (pre-region) responsible for cell export of the enzyme, followed by a series of 154 amino acids (pro-region) which is responsible, upon cleavage, for the activation of the proteolytic activity of the enzyme and 700-800 amino acids for the active site. The subsequent region (around 1000 amino acids) has been suggested to play a role in the specificity of cleavage and transport in the cell of the generated peptides and to also span the cell wall. The protease is cell wall anchored by its carboxyl end with the last 200 amino acids being responsible for the specific covalent binding to the cell wall peptidoglycan structure.
[0026] The polypeptide may be expressed in the lactic acid bacterium according to methods well known in the art. For example the commercially available vectors pNZ124 (Platteuw et al., (1994) Appl. Env. Microbiol. 60, 587), pGKI2 (Walke et al., (1996) FEMS Microbiol. 138, 233,) or pG+host9 (Maguin et al., (1996) J. Bacteriol 178, 931) may be used for episomal expression. Yet, having in mind the superior stability of chromosome integration, this way of doing could be preferred for the recombinant gene coding for the respective polypeptide. For integration into the chromosome homologous recombination may be applied by e.g. using an recombinant gene from lactic acid bacteria, containing the tolerogenic peptide and replacing the endogenous gene. Yet, methods for introducing recombinant genes into a host's chromosome are well within the skilled person's skill.
[0027] The peptide sequences (SEQ ID NOS: 1-17) and the anti-idiotypic VH and VL sequence (SEQ ID NOS: 18-19) mimicking a conformational epitope of an IgE may be found by screening random peptide and human Fab antibodies phage display libraries with an antibody directed to the Fc part of IgE. Preferred mimotope and anti-idiotypic Fab sequences are selected from the group consisting of:
Ile-Asn-His-Arg-Gly-Tyr-Trp-Val, (A) (SEQ ID NO:1) Arg-Asn-His-Arg-Gly-Tyr-Trp-Val, (B) (SEQ ID NO:2) Arg-Ser-Arg-Ser-Gly-Gly-Tyr-Trp-Leu-Trp, (C) (SEQ ID NO:3) Val-Asn-Leu-Thr-Trp-Ser-Arg-Ala-Ser-Gly, (D) (SEQ ID NO:4) Val-Asn-Leu-Pro-Trp-Ser-Arg-Ala-Ser-Gly, (E) (SEQ ID NO:5) Val-Asn-Leu-Thr-Trp-Ser-Phe-Gly-Leu-Glu, (F) (SEQ ID NO:6) Val-Asn-Leu-Pro-Trp-Ser-Phe-Gly-Leu-Glu, (G) (SEQ ID NO:7) Val-Asn-Arg-Pro-Trp-Ser-Phe-Gly-Leu-Glu, (H) (SEQ ID NO:8) Val-Lys-Leu-Pro-Trp-Arg-Phe-Tyr-Gln-Val, (I) (SEQ ID NO:9) Val-Trp-Thr-Ala-Cys-Gly-Tyr-Gly-Arg-Met, (J) (SEQ ID NO:10) Gly-Thr-Val-Ser-Thr-Leu-Ser, (K) (SEQ ID NO:11) Leu-Leu-Asp-Ser-Arg-Tyr-Trp, (L) (SEQ ID NO:12) Gln-Pro-Ala-His-Ser-Leu-Gly, (M) (SEQ ID NO:13) Leu-Trp-Gly-Met-Gln-Gly-Arg (N) (SEQ ID NO:14) Leu-Thr-Leu-Ser-His-Pro-His-Trp-Val-Leu- (O) (SEQ ID NO:15) Asn-His-Phe-Val-Ser, Ser-Met-Gly-Pro-Asp-Gln-Thr-Leu-Arg, (P) (SEQ ID NO:16) Val-Asn-Leu-Thr-Trp-Ser, (Q) (SEQ ID NO:17) Gln-Val-Lys-Leu-Leu-Glu-Ser-Gly-Pro-Gly- (R) (SEQ ID NO:18) Leu-Val-Lys-Pro-Ser-Glu-Thr-Leu-Ser-Leu- Thr-Cys-Thr-Val-Ser-Gly-Gly-Ser-Ile-Ser- Ser-Gly-Gly-Tyr-Tyr-Trp-Thr-Trp-Ile-Arg- Gln-Arg-Pro-Gly-Lys-Gly-Leu-Glu-Trp-Ile- Gly-Tyr-Ile-Tyr-Tyr-Ser-Gly-Ser-Thr-Ser- Tyr-Asn-Pro-Ser-Leu-Lys-Ser-Arg-Val-Thr- Met-Ser-Val-Asp-Thr-Ser-Lys-Asn-Gln-Phe- Ser-Leu-Arg-Leu-Thr-Ser-Val-Thr-Ala-Ala- Asp-Thr-Ala-Val-Tyr-Tyr-Cys-Ala-Arg-Glu- Arg-Gly-Glu-Thr-Gly-Leu-Tyr-Tyr-Pro-Tyr- Tyr-Tyr-Ile-Asp-Val-Trp-Gly-Thr-Gly-Thr- Thr-Val-Thr-Val-Ser-Ser Glu-Leu-Val-Val-Thr-Gln-Pro-Ala-Ser-Val- (S) (SEQ ID NO: 19) Ser-Gly-Ser-Pro-Gly-Gln-Ser-Ile-Thr-Ile- Ser-Cys-Thr-Gly-Thr-Arg-Ser-Asp-Val-Gly- Gly-Tyr-Asn-Tyr-Val-Ser-Trp-Tyr-Gln-Gln- His-Pro-Gly-Lys-Ala-Pro-Lys-Leu-Met-Ile- Tyr-Asp-Val-Ser-Asn-Arg-Pro-Ser-Gly-Val- Ser-Asn-Arg-Phe-Ser-Gly-Ser-Lys-Ser-Gly- Asn-Thr-Ala-Ser-Leu-Thr-Ile-Ser-Gly-Leu- Gln-Ala-Glu-Asp-Glu-Ala-Asp-Tyr-Tyr-Cys- Ser-Ser-Tyr-Thr-Ser-Ser-Ser-Thr-Leu-Gly- Val-Phe-Gly-Gly-Gly-Thr-Lys-Leu-Thr-Val- Leu-Gly
[0028] For more detailed information regarding the isolation and/or preparation of peptide and anti-idiotypic VH and VL sequences mimicking part of an IgE constant region in general, reference is made to WO 97/31948, the teaching of which is expressly incorporated herein by reference thereto.
[0029] The present invention also relates to a food and pharmaceutical composition, in particular vaccines, containing at least one such lactic acid bacterium as described above.
[0030] The bacterial strain may be included in the composition in an amount ranging from 10 5 to 10 12 cfu/g of the material. The food composition may be milk, yoghurt, curd, cheese, fermented milks, milk based fermented products, ice cream, fermented cereal based products, milk based powders, infant formulae or, in case of animals, pet food and the pharmaceutical composition may be in the form of tablets, liquid bacterial suspensions, dried oral supplements, wet oral supplements, dry tube feeding or wet tube-feeding.
[0031] The lactic acid bacterium and the food/pharmaceutical composition of the present invention may be used for treating any disease condition associated with allergic reactions, wherein an immune reaction involving IgE antibodies are involved, such as e.g. rhinitis, atopic dermatitits, erythema etc. Likewise, it will be appreciated that the bacteria/compositions of the present invention are well suited for being used as a “vaccination agent”, preventing the onset of allergy in an individual in general. This may easily be accomplished by simply feeding the person in need of a treatment against allergy with a food composition or a pharmaceutical composition according to the present invention. Upon ingestion the bacteria will colonize the intestine for a certain period of time so that depending on the amount of bacterial cell counts and the time period during which the compositions of the present invention are administered, the mimotope is presented to he individual, so that he may form an immune response against the mimotope(s). It will be appreciated that in addition to the lactic acid bacterium contained in the compositions of the present invention agents known to stimulate the immune system may be administered as well, so as to improve the immune response against the mimotope.
EXAMPLES
[0032] The following examples further illustrate the invention without limiting it thereto.
Example 1
Construction of Recombinant Polypeptide
[0033] Two peptides were fused with the cell surface anchored protease of L. bulgaricus to be displayed on the surface of the bacterium La1, i.e. the peptide s4 and another peptide (used as a control) derived from Tetanus Toxin (termed TT in the following sequence, see below).
[0034] The mimotope (ε4) was fused in frame to the cell surface proteinase (PrtB) from Lactobacillus bulgaricus (Gilbert et al., (1996) J. Bacteriol, 178, 3059-3065).
[0035] The protease gene was first amplified with its promoter by using the following two primers:
5′-TTTTGTGGATCCTTAACTTCATAGCACG-3′ (SEQ ID NO:20) (upstream the promoter of the gene, carrying a BamHI site) 5′-ATATTATCTAGAATTGAATAGATTGCC-3′ (SEQ ID NO:21) (downstream the rho-independent terminator of the gene, carrying a XbaI site)
[0036] The amplification product was cleaved with BamHI and XbaI and cloned in the lactic acid bacteria vector pNZ124, that had been digested with the same restriction enzymes, and eventually introduced by electroporation into plasmid-free (beta-galactosidase and protease negative) Lactococcus lactis.
[0037] The region of the active site of the cloned protease was replaced by the sequence of the TT and the ε4 peptides flanked by two cysteines residues at both ends. The cysteine residues were added becauses these two peptides were isolated from phage display libraries as circular peptides flanked by two cysteine residues. As these peptides do not represent the natural epitopes but rather mimic them, they are called mimotopes:
9 18 27 5′TGC ATT AAT CAT AGA GGA TAT TGG GTT TGC 3′ (SEQ ID NO:22) --- --- --- --- --- --- --- --- --- --- ε4 Cys Ile Asn His Arg Gly Tyr Trp Val Cys (SEQ ID NO:23) 9 18 27 5′TGC ACA GAT CCT TCT GGA GCA TCT GCA CCT TGC 3′ (SEQ ID NO:24) --- --- --- --- --- --- --- --- --- --- --- TT Cys Thr Asp Pro Ser Gly Ala Ser Ala Pro Cys (SEQ ID NO:25)
[0038] To achieve this, the cloned protease was cleaved with NheI which is located 50 bp downstream the sequence of the cleavage site of the leader peptide and PvuI, 800 bp further downstream. The DNA sequence coding for the peptide of interest (supra) was inserted between the two restriction sites as two oligonucleotides, which were designed such as to generate the two restriction sites at their ends once they are hybridized. The design of the oligonucleotides took into account that upon ligation to the protease gene the reading frame of the recombinant protein remains open.
[0039] The amplification product was cleaved with the restriction enzymes. In both cases the DNA fragments were ligated to the protease gene and introduced by electroporation into Lactobacillus johnsonii.
Example 2
Transformation of Lactobacillus johnsonii
[0040] For transformation purposes Lactobacillus johnsonii strain La1 (available from the Institute Pasteur under the accession no. CNCM I-1225) was grown overnight in MRS broth at 37° C. in anaerobic conditions. An aliquot of this culture was used to inoculate (1:10) another culture broth (MRS) containing 0.5M sucrose. After an additional re-inoculation at 2% into 200 ml MRS+0.5M sucrose the culture was grown to an OD 595 of 0.6. The cells were collected by centrifuging at 5000 rpm at 4° C. for 10 minutes, the pellet was washed twice with ½ volume of a solution containing 1M sucrose and 2.5 mM CaCl 2 , once with ¼ volume of a solution containing 1M sucrose, 2.5 mM CaCl 2 ) and the pellet obtained after centrifugation was resuspended in 3.5 ml of a solution of IM sucrose, 2.5 mM CaCl 2 +0.459 ml 87% glycerol (10% final concentration). The cells were either directly used for transformation or frozen at −80° C.
[0041] For the electroporation 40 εμl of cells were mixed with 10-100 ng of DNA (in <5 μl volume) and transferred into an ice-cold 0.2 cm electroporation cuvette. Pulses at 200 Ω, 25 μF, 2.5 kV in ice-cold 0.2 cm electroporation cuvette were applied. To the cuvette 1 ml of MRS+20 mM MgCl 2 , 2 mM CaCl 2 was added and the suspension was incubated for 2-3 hours at 37° C. 10 μl and 100 μl aliquots, respectively, were plated on MRS agar plates containing the appropriate antibiotic. The plates were incubated anaerobically for 24-48 hours at the same temperature as above. As a selection medium MRS with chloramphenicol (10 μg/ml) was used.
Example 3
Generation of Antisera Against the Proteinase PrtB
[0042] To generate antisera against the PrtB rabbits were immunized subcutaneously with Lactobacillus delbrueckii subsp. bulgaricus strain ATCC11842 expressing proteinase B (PrtB). Bacteria were grown overnight in MRS broth at 42° C. in a GasPak anaerobic system. An aliquot of this culture was used to inoculate another culture broth (MRS) containing 0.5M sucrose and the culture was grown for 5 hours at 42° C. until an OD 595 of 0.6. The cells were collected by centrifuging at 5000 rpm at 4° C. for 10 minutes, the pellet was washed twice with 10 ml PBS and then resuspended in 2 ml PBS. Rabbits were immunized three times at two weeks intervals with 1.5 ml PBS resuspended cells and seven days after the last feeding rabbits were bled. Serum was purified six times on 2×10 9 Lactobacillus johnsonii (La1).
Example 4
Generation of Antisera Against the TT and the ε4 Mimotopes
[0043] To generate sera against the TT and the ε4 mimotopes rabbits were immunised subcutaneously with either polyoxime-TT mimotope construct or with ε4 mimotope conjugated with keyhole limpet hemocyanin (KLH). Rabbits were immunized four times at two weeks intervals and animals were bled seven days after the last injection. The antiε4 serum was purified by immunoaffinity chromatography on CH-Sepharose 4B coupled to ε4 mimotope.
Example 5
Detection of Mimotope-PrtB Fusion Proteins by Antibodies
[0044] In order to determine, whether the lactic acid bacteria express the mimotopes in a manner so as to be accessible by and recognized by antibodies, bacteria either containing the PrtB gene without any modification, or containing the recombinant gene (coding either for the ε4 or the TT mimotope respectively) were grown in 25 ml medium containing 10 μg/ml chloramphenicol. Bacterial cells were harvested by centrifugation at 3000×g for 15 minutes at 4° C., washed with 5 ml TBS and recentrifuged. Finally the bacterial pellet was resuspended in 450 μl Tris-buffered saline (TBS: 25 mM Tris/HCl pH 7.5, 0.8% NaCl, 0.02% KCl) and 150 μl 4×non-reducing sample buffer (80 mM Tris/HCl pH 6.8, 2.5% SDS, 0.15% glycerol, 0.05% bromophenol blue). 20 μl aliquots were separated by SDS-polyacrylamide gel electrophoresis (SDS-PAGE) (6% acrylamide-Bis, 0.5M Tris-HCl pH 8.8) and run in a 25 mM Tris, 192 mM glycine buffer (pH 8.3) at 100V for 60 minutes. The gels were stained with BM Fast stain (Boehringer Mannheim, Germany) or transferred electrophoretically onto nitrocellulose membranes (Protran BA 83, Schleicher & Schuell, Dassel, Germany). After transfer the membranes were blocked with PBS/5% BSA for 2 hours at RT. Immunoblots were incubated with either rabbit anti-TT serum (1:1000) or anti-PrtB serum (1:2000) overnight at RT and incubated for 3 hours at RT with a 1:1000 dilution of horseradish peroxidase conjugated goat anti-rabbit IgG. Immunoblots were developed with 4-chloro-1-naphtol for 2 minutes.
[0045] As shown in FIG. 1, it could be observed that recombinant Lactobacillus johnsonii showed specific bands using the appropriate antibodies for detection, indicating that the ε4 and the TT mimotopes as well as the proteinase PrtB was produced by the recombinant bacteria in the correct conformation.
Example 6
ELISA to Detect Surface Antigen Expression on Lactobacillus johnsonii (La1)
[0046] Transformed bacteria were grown overnight in 50 ml medium containing 10 μg/ml chloramphenicol. Bacterial cells were harvested by centrifugation at 3000×g for 15 minutes at 4° C., washed with 5 ml TBS and recentrifuged. Finally the bacterial pellet was resuspended in 900 μl TBS and 100 μl 0.5M bicarbonate buffer pH9.6. Costar EIA/RIA half-well plates (Costar, Cambridge, Mass.) were coated overnight at 37° C. with 50 μl bacterial solution per well (approximately 10 8 bacteria). Coating efficiency was assessed using TTd at a concentration of 10 μg/ml as coating antigen. Plates were extensively washed with PBS/0.1% Tween-20 until no bacteria were left. Wells were blocked in PBS/5% BSA for 2 hours at 37° C. and incubated with 50 μl of either rabbit anti-TT serum or affinity purified rabbit anti-ε4 serum IgG antibodies at a concentration of 10 μg/ml for 4 hours at 37° C. After washing six times with PBS/0.1% Tween-20 plates were incubated 1.5 hours at 37° C. with a 1:1000 dilution of horseradish peroxidase conjugated goat anti-rabbit IgG. Plates were washed six times with PBS/0.1% Tween-20 and developed with tetramethylbenzidine (TMB; Fluka Chemie AG, Buchs, Switzerland). The reaction was stopped with 1 M H 2 SO 4 and absorbance values were measured at 450 nm using an ELISA reader (Molecular devices, Basel, Switzerland).
[0047] As are illustrated in FIGS. 2 and 3 anti-TT and anti-ε4 antibodies specifically recognized the live recombinant La1 expressing TT and ε4 mimotopes indicating that the two mimotopes were expressed and displayed on the cell surface of the bacteria.
1
25
1
8
PRT
Homo sapiens
1
Ile Asn His Arg Gly Tyr Trp Val
1 5
2
8
PRT
Homo sapiens
2
Arg Asn His Arg Gly Tyr Trp Val
1 5
3
10
PRT
Homo sapiens
3
Arg Ser Arg Ser Gly Gly Tyr Trp Leu Trp
1 5 10
4
10
PRT
Homo sapiens
4
Val Asn Leu Thr Trp Ser Arg Ala Ser Gly
1 5 10
5
10
PRT
Homo sapiens
5
Val Asn Leu Pro Trp Ser Arg Ala Ser Gly
1 5 10
6
10
PRT
Homo sapiens
6
Val Asn Leu Thr Trp Ser Phe Gly Leu Glu
1 5 10
7
10
PRT
Homo sapiens
7
Val Asn Leu Pro Trp Ser Phe Gly Leu Glu
1 5 10
8
10
PRT
Homo sapiens
8
Val Asn Arg Pro Trp Ser Phe Gly Leu Glu
1 5 10
9
10
PRT
Homo sapiens
9
Val Lys Leu Pro Trp Arg Phe Tyr Gln Val
1 5 10
10
10
PRT
Homo sapiens
10
Val Trp Thr Ala Cys Gly Tyr Gly Arg Met
1 5 10
11
7
PRT
Homo sapiens
11
Gly Thr Val Ser Thr Leu Ser
1 5
12
7
PRT
Homo sapiens
12
Leu Leu Asp Ser Arg Tyr Trp
1 5
13
7
PRT
Homo sapiens
13
Gln Pro Ala His Ser Leu Gly
1 5
14
7
PRT
Homo sapiens
14
Leu Trp Gly Met Gln Gly Arg
1 5
15
15
PRT
Homo sapiens
15
Leu Thr Leu Ser His Pro His Trp Val Leu Asn His Phe Val Ser
1 5 10 15
16
9
PRT
Homo sapiens
16
Ser Met Gly Pro Asp Gln Thr Leu Arg
1 5
17
6
PRT
Homo sapiens
17
Val Asn Leu Thr Trp Ser
1 5
18
126
PRT
Homo sapiens
18
Gln Val Lys Leu Leu Glu Ser Gly Pro Gly Leu Val Lys Pro Ser Glu
1 5 10 15
Thr Leu Ser Leu Thr Cys Thr Val Ser Gly Gly Ser Ile Ser Ser Gly
20 25 30
Gly Tyr Tyr Trp Thr Trp Ile Arg Gln Arg Pro Gly Lys Gly Leu Glu
35 40 45
Trp Ile Gly Tyr Ile Tyr Tyr Ser Gly Ser Thr Ser Tyr Asn Pro Ser
50 55 60
Leu Lys Ser Arg Val Thr Met Ser Val Asp Thr Ser Lys Asn Gln Phe
65 70 75 80
Ser Leu Arg Leu Thr Ser Val Thr Ala Ala Asp Thr Ala Val Tyr Tyr
85 90 95
Cys Ala Arg Glu Arg Gly Glu Thr Gly Leu Tyr Tyr Pro Tyr Tyr Tyr
100 105 110
Ile Asp Val Trp Gly Thr Gly Thr Thr Val Thr Val Ser Ser
115 120 125
19
112
PRT
Homo sapiens
19
Glu Leu Val Val Thr Gln Pro Ala Ser Val Ser Gly Ser Pro Gly Gln
1 5 10 15
Ser Ile Thr Ile Ser Cys Thr Gly Thr Arg Ser Asp Val Gly Gly Tyr
20 25 30
Asn Tyr Val Ser Trp Tyr Gln Gln His Pro Gly Lys Ala Pro Lys Leu
35 40 45
Met Ile Tyr Asp Val Ser Asn Arg Pro Ser Gly Val Ser Asn Arg Phe
50 55 60
Ser Gly Ser Lys Ser Gly Asn Thr Ala Ser Leu Thr Ile Ser Gly Leu
65 70 75 80
Gln Ala Glu Asp Glu Ala Asp Tyr Tyr Cys Ser Ser Tyr Thr Ser Ser
85 90 95
Ser Thr Leu Gly Val Phe Gly Gly Gly Thr Lys Leu Thr Val Leu Gly
100 105 110
20
28
DNA
Artificial
Primer for the promoter of protease gene of
Lactobacillus bulgaricus
20
ttttgtggat ccttaacttc atagcacg 28
21
27
DNA
Artificial
Primer for the promoter of protease gene of
Lactobacillus bulgaricus
21
atattatcta gaattgaata gattgcc 27
22
30
DNA
Homo sapiens
22
tgcattaatc atagaggata ttgggtttgc 30
23
10
PRT
Homo sapiens
23
Cys Ile Asn His Arg Gly Tyr Trp Val Cys
1 5 10
24
33
DNA
Homo sapiens
24
tgcacagatc cttctggagc atctgcacct tgc 33
25
11
PRT
Homo sapiens
25
Cys Thr Asp Pro Ser Gly Ala Ser Ala Pro Cys
1 5 10
|
The present invention pertains to novel strains of lactic acid bacteria capable of reducing an individual's tendency to react allergic against a variety of different allergens. In particular, the present invention relates to recombinant strains of lactic acid bacteria that express surface polypeptides which include peptides or antibody fragments acting as mimic for at least a part of the F c region of IgE-molecules. The invention also pertains to food or pharmaceutical compositions containing said micro-organisms or active fractions thereof.
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FIELD OF THE INVENTION
This invention relates to a method and apparatus for controlling the head pressure in refrigeration and air conditioning systems. More specifically, this invention is intended to control the condenser capacity in such a way as to maintain the condensing pressure or discharge line pressure approximately equivalent to the internal compressor discharge pressure.
BACKGROUND OF THE INVENTION
Screw compressors are commonly used in air conditioning and refrigeration systems. It is well known that screw compressors, along with rotary vane compressors and the more recently introduced scroll compressors, are constant volume ratio compressors. For screw compressors, the internal volume ratio, V i , is defined as the volume of uncompressed vapor in one groove of the compressor before compression begins divided by the volume of the compressed vapor in the groove just prior to the uncovering of the discharge port. This ratio is fixed during the manufacture of the machine by the size of the compressor grooves and the location of the suction and discharge ports of the compressor.
Since screw compressors are constant volume ratio machines, they are also constant pressure ratio, P i , machines. Assuming isentropic compression, the volume ratio is related to the pressure ratio by the following equation: ##EQU1## where: k=the isentropic exponent of the refrigerant being used
P d =the internal discharge pressure of the screw compressor
P s =the suction pressure of the screw compressor
As can be seen from the above relationship, for a given refrigerant, the screw compressor internal discharge pressure, P d , is dependant only on the built in volume ratio, V i and suction pressure, P s . Thus, in systems utilizing a compressor with a constant internal volume ratio and where the suction pressure is held constant, the internal discharge pressure will also remain constant.
It is important to note that while the relationship shown above for V 1 and P i is correct for isentropic compression, it is recognized that screw compressors do not perform in a pure isentropic fashion. The vapor being compressed within the grooves of the compressor is cooled to some degree by the oil injected injected into the compressor. In addition, the grooves of the compressor are not perfectly sealed which allows a small portion of the refrigerant to blow-through, or leak out of, the grooves during compression. As a result, the ideal pressure ratio is not achieved. This change of pressure can be determined from the adiabatic compressor efficiency of the compressor and a correction factor applied to obtain the "ideal" pressure ratio.
It is well known that for the most economical operation, the internal discharge pressure of the screw compressor should equal the pressure of the refrigerant within the line into which the screw compressor discharges. This is referred to as ideal compression. However, in many cases where the internal discharge pressure remains relatively constant, ideal compression is not achieved due to changes in the condensing pressure and hence, the discharge line pressure. The discharge line pressure can be considered equal to the condensing pressure in most applications because the only difference in these two pressures is the relatively small pressure loss which occurs in the line between the outlet of the compressor and the inlet of the condenser. As a result, the discharge line pressure will vary directly with the condensing pressure.
The condensing pressure at which a condenser will operate depends upon a number of factors such as the design conditions for which the condenser was selected, the actual conditions at which the condenser is operating, and whether the condenser is operating at full or partial capacity. In many cases, condenser operations in refrigeration and air conditioning systems are operated at full capacity at all times. In these situations, the pressure at which the condenser operates will fluctuate as changes occur in the ambient conditions such as outside air temperature or humidity. Because of these condensing pressure fluctuations, refrigeration or air conditioning systems utilizing screw compressors typically operate where the internal discharge pressure of the compressor does not equal the condensing or discharge line pressure resulting in a condition of either "over-compression" or "under-compression".
In the under-compression case, the internal discharge pressure is less than the discharge line pressure. Energy is wasted because the compressor must work against this higher pressure from the time the discharge port is uncovered until all gas is pushed out of the cavity. In the over-compression case, the internal discharge pressure is greater than the discharge line pressure. Energy is wasted in this case when the condenser needlessly operates at full capacity, thereby keeping the discharge line pressure low, when operation at less than full capacity would be sufficient.
PRIOR ART
In the past, screw compressors were selected with an internal volume ratio that would most closely match the expected system evaporating and condensing pressures. In many applications, the evaporator load and suction pressure would remain relatively constant but a fluctuation would occur in the ambient conditions such as outside air temperature or outside air relative humidity. Typically, condensing capacity was maintained at the maximum and the condensing pressure was allowed to fluctuate with the ambient conditions. This would result in the discharge line pressure varying while the internal discharge pressure remained constant; which, in turn would cause the over or under compression conditions described above.
U.S. Pat. No. 4,516,914 disclosed an apparatus to change the internal volume ratio of the screw compressor while the compressor is operating. This change in the internal volume ratio was effected by relocating the discharge port of the compressor during operation. Since the internal discharge pressure is directly related to the internal volume ratio, by changing the internal volume ratio, this system could control the internal discharge pressure of the compressor during operation to allow it to match the discharge line pressure. This system came to be known to those skilled in the art as "Variable Volume Ratio Control."
In systems utilizing a compressor supplied with variable volume ratio control, the condenser operations are typically run at full capacity and the discharge line pressure is allowed to fluctuate with ambient conditions. However, the internal discharge pressure of the compressor is controlled to match the current discharge line pressure. The condensing capacity is normally not reduced until the discharge line pressure reaches the minimum allowable for the system, which minimum is usually based upon what is required for proper liquid feed or oil circulation.
The variable volume ratio control system saves energy by matching the internal discharge pressure to the discharge line pressure, thereby minimizing the conditions of over and under-compression. In addition, it allows the same compressor to be efficiently used as a "swing" machine on different systems. However, there is still significant room for improvement in this area.
For example, the lowest internal volume ratio that the variable volume ratio control system can provide is not small enough in many applications where the ambient or outdoor temperature, and thus discharge line pressure, can approach very low levels. In these applications, the internal discharge pressure can not be reduced enough by the variable volume ratio control system to allow it to match the low discharge line pressure. This results in over-compression which is energy wasteful.
Also, the variable volume ratio system can only be provided on new machines because the system must be built into the compressor. The fact that the variable volume ratio control system can not be retrofit on any existing screw compressor machines severely restricts the usefulness of this system.
Further, the variable volume ratio system is complex and results in the addition of many more mechanical parts to the screw compressor machine.
SUMMARY OF THE INVENTION
The present invention provides a method and apparatus for controlling the discharge line pressure in an air conditioning or refrigeration system.
It is an object of the present invention to provide a method and apparatus to control the capacity of the condenser operations in air conditioning or refrigeration systems such that the discharge line pressure and the compressor internal discharge pressure are maintained substantially equal.
Briefly stated, the present invention operates by measuring the suction pressure of the working fluid just prior to its entrance into the compressor. The internal discharge pressure of the compressor is then calculated from this suction pressure and from the internal pressure ratio of the compressor. The discharge line pressure is then measured and compared to the internal discharge pressure of the compressor. If the discharge line pressure and the internal discharge pressure of the compressor are substantially equal, no changes are made to the system. However, if these pressures are not equal, the condenser capacity is either increased or decreased depending upon whether the internal discharge pressure of the compressor is greater than or less than the discharge line pressure.
If the internal discharge pressure is greater than the discharge line pressure, a condition of over-compression exists and the present invention saves condenser energy by decreasing the capacity of the condenser until the discharge line pressure increases to match the internal discharge pressure of the compressor. If the internal discharge pressure of the compressor is less than the discharge line pressure, a condition of under-compression exists and the present invention saves compressor energy by increasing the condensing capacity until the discharge line pressure decreases to match the internal discharge pressure of the compressor. The amount of energy saved at the compressor in the under-compression case will be greater than that required to increase the condensing capacity. Thus, the present invention provides energy savings when the compressor is either operating at an over- or under-compression condition by changing the discharge line pressure to have it be substantially equal to the internal discharge pressure.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a flow chart block diagram illustrating the control logic of the present invention,
FIG. 2 is a schematic diagram showing the configuration of a typical air conditioning or refrigeration system utilizing the present invention,
FIG. 3 is a schematic diagram showing one configuration of a two stage compressor refrigeration system utilizing the present invention,
FIG. 4 is a schematic diagram showing an alternative configuration of a two stage compressor refrigeration system utilizing the present invention,
FIG. 5 is a flow chart block diagram illustrating the operation of the control logic of the present invention for the case of ideal compression,
FIG. 6 is a flow chart block diagram illustrating the operation of the control logic of the present invention for the case of under-compression, and
FIG. 7 is a flow chart block diagram illustrating the operation of the control logic of the present invention for the case of over-compression.
DETAILED DESCRIPTION
Referring now to FIG. 1, there is shown a flow chart block diagram displaying the preferred embodiment of the control logic of the present invention. The control logic start point 10 signifies the beginning of the control sequence. In block 12, the suction pressure, Ps, is measured. In block 14, the internal discharge pressure is calculated by multiplying the suction pressure by the internal pressure ratio. The condensing pressure, or discharge line pressure, Pc is measured in block 16. In block 18, the difference between the internal discharge pressure and the discharge line pressure is calculated and is shown as ΔP. Block 20 is a decision block wherein a comparison is made between the absolute value of ΔP and a pre-set tolerance that has been manually inputted to and stored in the controller. If the absolute value of ΔP is less than the tolerance, the logic follows path 22 which leads to block 24 in which no change to the condenser capacity is made. The logic then follows path 38 back to the start 10 of the control sequence.
If in block 20, the absolute value of ΔP is greater than the tolerance, then the logic follows path 26 which leads to a second decision block 28. In decision block 28, a determination is made as to whether the difference between the internal discharge pressure and discharge line pressure, ΔP, is greater than zero. If the answer is no, a condition of under-compression exists and the logic follows path 30 to block 32 wherein the condenser capacity is increased. Upon leaving block 32 the logic follows path 38 back to the start 10 of the control sequence. If, however, in decision block 28, the answer is yes and ΔP is greater than zero, a condition of over-compression exists and the logic follows path 34 to block 36 wherein the condenser capacity is decreased. Upon leaving block 36, the logic follows path 38 back to the start 10 of the control sequence.
The apparatus required in the present invention is show schematically in FIG. 2. The typical refrigeration or air conditioning system consists of a compressor 100, which could be a screw, rotary vane or scroll compressor. Compressor 100 has an outlet which is connected via conduit 102 to the inlet of condenser 104. The condenser 104 could be an evaporative condenser, a water cooled condenser with cooling water supplied by a cooling tower, an air cooled condenser, or other condensing device. Condenser 104 has an outlet which is connected via conduit 106 to an expansion device 108, which usually is a thermostatic expansion valve but which could be an alternative expansion device such as an orifice, capillary tubes or other type of expansion device. Expansion device 108 has an outlet which is connected via conduit 110 to the inlet of evaporator 112. The outlet of evaporator 112 is connected via conduit 114 to the inlet of compressor 100 thereby completing the circuit. A working fluid, most typically a gaseous refrigerant, is contained in and flows through this circuit.
In addition to the basic refrigeration or air conditioning system described above, the present invention also requires the use of two pressure sensing devices 116 and 122 and a controller 128. Pressure sensing devices 116 and 122 are typically pressure transducers which function to hydraulically or pneumatically sense the pressure of a fluid, transduce this physical pressure measurement into an electrical signal and transmit this electrical signal, representing the sensed pressure, to a suitable receiving device such as controller 128.
In the present invention, pressure sensing device 116 measures the working fluid suction pressure at location 118 and transmits an electrical signal representing this pressure measurement to controller 128 via line 120. The second pressure sensing device 122 measures the discharge line pressure at location 124 and transmits an electrical signal representing this pressure measurement to controller 128 via line 126
Depending upon the signals received from pressure sensing devices 116 and 122 and the calculated internal discharge pressure of the compressor, controller 128 may output a signal via line 130 to condenser 104 to either increase or decrease the capacity of condenser 104. This change in condensing capacity could be achieved in several different ways such as increasing or decreasing the condenser o cooling tower fan motor speed, cycling the condenser or cooling tower fans on and off, cycling the evaporative condenser spray water pump on and off, adjusting the position of the condenser or cooling tower fan dampers, cycling off entire condenser units in a multiple cell installation or combinations of the above.
One of the many possible applications for the present invention would be for controlling the head pressure of a refrigeration system which is used to provide cooling to a process. These refrigeration systems often used multiple stage, twin screw, axial flow screw compressors and multiple cell evaporative condensers with various means to control condensing capacity as described above. In many cases the refrigeration load remains relatively constant but the ambient conditions, and hence the condensing pressure and discharge line pressure, vary throughout the day.
The present invention could be used to control the discharge line pressure in a two, or multiple, stage compressor refrigeration system. FIG. 3 is a schematic diagram of a two stage compressor refrigeration system utilizing the present invention. Note that the compressor means 100 illustrated in FIG. 2, has been replaced in the system shown in FIG. 3 by a first stage compressor 101', an intercooler 103', and a second stage compressor 100', which are all connected in series. In this two stage system, the present invention is used to control the discharge line pressure of the working fluid in line 102' by treating the two compressors, 101' and 100', as a single compressor. Pressure sensing device 116' measures the suction pressure of the working fluid at location 118' just prior to the working fluid entering the first stage compressor 101'. Pressure sensing device 122' measures the discharge line pressure of the working fluid at location 124', just after the outlet of compressor 100'. In this two stage system, the present invention would operate in the same manner as has been previously described, except that the internal pressure ratio which must be inputted to and stored in the controller would be the product of the internal pressure ratios for the first and second stage compressors.
However, it is not required in the operation of the present invention in a two, or multiple stage compressor refrigeration system that the operation of the two or more compressors be combined and treated as one. Rather, the present invention can be used in a multiple stage compressor refrigeration system to control the discharge line pressure based only on the operation of the last stage compressor as illustrated in the schematic diagram of FIG. 4. In this diagram, the compressor means is shown to consist of first stage compressor 101", intercooler 103", and second stage compressor 100", all of which are connected in series. However, in this system, pressure measuring device 116" measures the suction pressure of the working fluid at location 118", which is just prior to the inlet of the second stage compressor 100", and pressure sensing device 122" measures the discharge line pressure at location 124", just after the outlet of the second stage compressor 100". In this case, the present invention would operate in the same manner as described previously except that the internal pressure ratio which is inputted and stored in the controller 128" would be the pressure ratio for only the second stage compressor.
The operation of the preferred embodiment of the present invention can best be illustrated by the following example. In this example, the operation of the present invention will be illustrated for use in a two stage screw compressor system with multiple cell condensers. Both compressor will be combined for the purposes of this example and treated as one. Further, it will be assumed that the first stage compressor has an internal pressure ratio of 2.6 and the second stage compressor has an internal pressure ratio of 2.8. As a result, the total pressure ratio for the compressor system would be equal to 2.6×2.8=7.3. In addition, it will be assumed that the suction pressure remains constant and equal to 29.0 psia.
Referring now to FIG. 5, the operation of the present invention will be explained for the ideal compression case which occurs when the discharge line pressure is within the pre-set tolerance of the internal discharge pressure. As shown by block 52, the first step in the control sequence of the present invention is to measure the suction pressure of the refrigerant which is shown to be 29.0 psia. Next, the controller in block 54 calculates the internal discharge pressure of the compressor, P d , by multiplying the suction pressure by the internal pressure ratio, P i , which is shown in the figure as 29.0 psia×7.3=211.7 psia.
The discharge line pressure is then measured as shown by block 56. To illustrate the operation of the present control device in this first mode, it will be assumed that the ambient conditions are close to the design conditions for the system and that at these conditions, the discharge line pressure is equal to 210 psia as indicated. In block 58, the controller then subtracts this discharge line pressure, P c , from the internal discharge pressure, P d , to determine the difference between these pressures, ΔP, which is shown to be equal to 211.7-210=1.7 psia. The controller then compares the absolute value of this 1.7 psia pressure difference to the preset tolerance of the system in decision block 60 to determine if the pressure difference is less than this tolerance. In this example, assume that the tolerance is 3 psia. As a result, the pressure difference is less than the tolerance and the controller then follows path 62 to block 64 in which no signal is sent to the condenser to change the capacity. The controller then follows path 78 back to the start of the controller logic sequence 50 and begins the control sequence over again.
Referring now to FIG. 6, the operation of the present invention will be explained for the case where under-compression exists, that is, when the discharge line pressure is greater than the internal discharge pressure of the compressor. This situation could commonly arise during the morning hours when the ambient temperature is relatively low. During these low ambient temperature operating times, the system will not require its full condensing capacity to maintain the discharge line pressure close to the internal discharge pressure of the compressor. However, as the ambient temperature increases, the condensing pressure and discharge line pressure will also increase causing a condition of under-compression. This condition will continue until additional condensing capacity is brought on-line to reduce the discharge line pressure.
For the purposes of this example, it will be assumed that the suction pressure is still 29 psia as shown in block 52'. Accordingly, since the internal pressure ratio remains constant, the calculated internal discharge pressure is still equal to 211.7 psia as shown in block 54'. However, since the ambient temperature has now increasing from a relatively low level, the discharge line pressure has also increased and in fact, is shown as 220 psia in block 56'. The calculated ΔP in block 58' is now equal to -8.3 psia. As a result, in decision block 60', the absolute value of ΔP is greater than the pre-set tolerance of 3 psia so the controller follows path 66' to the second decision block 68'. In this decision block 68', it is determined that -8.3 is less than zero such that the controller follows path 70', which is the under-compression path, to block 72' wherein the controller outputs a signal to the condenser to increase the capacity in order to lower the discharge line pressure and bring it within the preset tolerance. Upon leaving decision block 72', the controller follows path 78' back to start block 50'.
Referring now to FIG. 7, the operation of the present invention will be explained for the case where over-compression exists, that is, when the discharge line pressure is less than the internal discharge pressure of the compressor. This situation could arise during the evening hours as the ambient temperatures begin to fall from their peak, mid-day levels. During the time when the ambient temperature is at its highest level for the day, the refrigeration system could require the maximum available condensing capacity to maintain the discharge line pressure close to the internal discharge pressure of the condenser. However, as the ambient temperatures begin to fall, the condensing pressure and the discharge line pressure will also fall, assuming the refrigeration load remains constant. This drop in discharge line pressure could cause the condition of over-compression which will continue until the condensing capacity is reduced in order to effect an increase in the discharge line pressure.
As before, it will be assumed that the suction pressure has remained constant and, therefore, is still shown as 29 psia in block 52". Accordingly, since the internal pressure ratio remains constant, the calculated internal discharge pressure is still equal to 211.7 psia as shown in block 54". However, since the ambient temperature has fallen from its previous high levels, the discharge line pressure has also fallen and, in fact, is shown as 200 psia in block 56". The calculated ΔP in block 58" is now equal to 11.7 psia. As a result, in decision block 60", the absolute value of ΔP is greater than the pre-set tolerance of 3 psia so the controller follows path 66"to the second decision block 60". In this decision block 60", it is determined that 11.7 is greater than zero such that the controller follows path 74', which is the over-compression path, to block 76' wherein the controller outputs a signal to the condenser to decrease the capacity. This decrease in condenser capacity will effect an increase in the discharge line pressure such that the discharge line pressure is brought within the pre-set tolerance. This condenser capacity decrease could be easily achieved as described previously by slowing down the fan motors, turning off some fans, or closing the fan dampers. Upon leaving decision block 76', the controller follows path 78' back to start block 50'.
While the operation of the present invention has been described when used with a screw compressor refrigeration system, it should be obvious to those skilled in the art that the present invention could find application on any refrigeration or air conditioning system which utilizes fixed or variable volume ratio compressors. Further, the present invention would be able to provide energy savings with any type of condenser operation that has multiple control steps which can be used to reduce energy input as capacity is decreased. Various modifications may be made without departing from the scope and intent of the invention which is defined in the following claims.
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The present invention describes a method of controlling the head pressure in a refrigeration or air conditioning system in order to maintain the internal discharge pressure and discharge line pressure substantially equal. The method consists of the steps of measuring the suction pressure of the working fluid, calculating the internal discharge pressure of the working lfuid by multiplying the suction pressure by the internal pressure ratio of the compressor, measuring the discharge line pressure of the working fluid and then comparing the internal discharge pressure to the discharge line pressure. If the difference between the internal discharge pressure and discharge line pressure is greater than some allowable tolerance, the capacity of the condenser is adjusted to equalize these two pressures.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This present invention relates to the deployment of objects in the nature of projectiles and in particular, although not exclusively, to the formation of a predetermined pattern of deployed sub-projectiles by a parent projectile and to a projectile launching method for masking the launch location of a projectile.
[0003] 2. Discussion of the Background Art
[0004] Projectiles that incorporate explosive charges have been used as fragmentation devices to deploy a plurality of fragments. In a simple form the casing of such a projectile fragments on detonation of the explosive charge such that individual fragments of the casing are deployed radially to form a fragmentation pattern roughly in the shape of the surface of a sphere.
[0005] In other configurations, the shape of the charge and the configuration of the casing may be varied to control the fragmentation pattern. However, such fragmenting projectiles produce a relatively thin, shell like fragment casing pattern. It is desirable that the depth of the fragmentation be able to be increased or controlled.
[0006] Such projectiles may be particularly suited to defending a designated area whilst avoiding rending the area dangerous after a threat situation has diminished, such as occurs with conventional minefields.
[0007] Existing defences to attacks typically include systems for acquiring and monitoring the trajectory of objects, including flying objects such as rockets and missiles. Examples of trajectory acquisition and monitoring systems are described in U.S. Pat. No. 4,622,458 to Boeck et al and U.S. Pat. No. 5,960,097 to Pfeiffer et al.
[0008] More recently, sophisticated defences to threats which include rounds launched at relatively high angles so as to be thrown or hurled at a target, such as characteristic of mortars, are capable of calculating the source of an attack by deriving the location of a projectile launching apparatus from the trajectory of the projectiles.
SUMMARY OF THE INVENTION
OBJECT OF THE INVENTION
[0009] It is an object of certain embodiments of the invention to provide a projectile that may be used to deploy sub-projectiles in a predetermined pattern that addresses the problems of the prior art, by providing increased or controlled fragmentation, or at least provides a useful choice for defence purposes.
[0010] It is a further object of certain embodiments of the invention to provide a defence system that has improved control over deployment of projectiles and does not render the defended area unsafe for later civilian use.
[0011] It is an object of other embodiments of the invention to provide a defence system capable of masking the location of a projectile launching apparatus by diverting projectile in flight whereby the location of the projectile launching apparatus is unable, or at least more difficult, to derive.
DISCLOSURE OF THE INVENTION
[0012] According to a first form of the present invention, there is provided a projectile including a multiplicity of barrel assemblies radially disposed from the centre of mass of the projectile, wherein each of said multiplicity of barrel assemblies includes a plurality of sub-projectiles axially disposed within a barrel, wherein each of said sub-projectiles are associated with a discrete propellent charges for propelling a respective sub-projectile from the barrel, and wherein said projectile is capable of selectively firing sub-projectiles to provide a predetermined pattern of deployed sub-projectiles.
[0013] Preferably the projectiles of the present invention are particularly adapted for deployment by firing from the barrel of a gun, rather than self-propelled missiles or rockets that are launched from a tube or gantry. In other embodiments the projectiles of the invention may be deployed by dropping from a mobile platform, such as an aircraft or ship, utilising gravity for delivery or, alternatively, adapted for throwing by a soldier or protective services officer in a similar fashion to a conventional manually delivered grenade.
[0014] The projectiles of the invention suited to firing from a barrel may, in a first aspect, be used for intercepting and destroying incoming missiles, particularly of the high altitude ballistic type. In a second aspect, the present invention provides a method of intercepting a missile including the steps of determining the path of the missile, firing a projectile of the type herein described into the path of said missile, and firing selected sub-projectiles to form a predetermined pattern of sub-projectiles in and adjacent to the determined path of the missile.
[0015] The projectiles of the present invention may be used for vehicle self defence. A vehicle coming under attack, in particular from close range, may fire a projectile of the type herein described towards the attackers and deploy the sub-projectiles in a predetermined pattern amongst the attackers. In a third aspect, the present invention provides a self defence method for a vehicle from an attacking force including the steps of determining the location of the attacking force, firing a projectile of the type herein described adjacent to the determined location of the attacking force, and firing selected sub-projectiles to form a predetermined pattern of sub-projectiles in and adjacent to the determined location of the attacking force.
[0016] The projectiles of the present invention may be used for repelling an infantry advance. In a fourth aspect, the present invention provides a method of repelling an infantry including the steps of determining the location of the infantry, firing at least one projectile of the type herein described adjacent to the determined location of the infantry, and- firing selected sub-projectiles to form a predetermined pattern of sub-projectiles in and adjacent to the determined location of the infantry.
[0017] The projectiles of the present invention may be used for forming airborne images, such as fireworks. In a fifth aspect, the present invention provides a method of forming airborne images including the steps of firing a projectile of the type herein described into the air, and firing selected sub-projectiles including image forming matter to form a predetermined pattern of image forming matter in the air.
[0018] The projectiles of the present invention may be used for fire fighting. In a sixth aspect, the present invention provides a method of fire fighting including the steps of determining the location of the fire, firing at least one projectile of the type herein described adjacent to the determined location of the fire, firing selected sub-projectiles to form a predetermined pattern of sub-projectiles in and adjacent to the determined location of the fire, and deploying from the fired sub-projectiles a fire retardant.
[0019] The projectiles of the present invention may be used for generating a fuel-air explosion. In a seventh aspect, the present invention provides a method of generating a fuel-air explosion including the steps of selecting the desired location of the fuel-air explosion, firing at least one projectile of the type herein described adjacent to the desired location of the fuel-air explosion, firing selected sub-projectiles including a fuel to form a predetermined pattern of sub-projectiles, deploying the fuel from the fired sub-projectiles, firing selected sub-projectiles including detonators to form a predetermined pattern of sub-projectiles, detonating said detonators to generate a fuel-air explosion.
[0020] The projectiles of the present invention may be used for deploying a variety of payloads. In a eighth aspect, the present invention provides a method of deploying a payload including the steps of selecting a desired location for the delivery of a payload, firing at least one projectile of the type herein described adjacent to the desired location of the payload, firing selected sub-projectiles including said payload to form a predetermined pattern of sub-projectiles, and deploying said payload from the fired sub-projectiles.
[0021] The projectiles of the present invention may be used for defending a designated area. In a ninth aspect, the invention resides broadly in defence system for defending a designated area, said defence system including:
[0022] at least one monitor for monitoring the designated area to detect any zone therein in which a new presence appears;
[0023] defence means capable of debilitating personnel present anywhere in a remote designated area wherein said defence means includes a weapon capable of firing projectiles wherein the projectiles include an array of barrel assemblies disposed radially from the centre of mass of the projectile, each barrel assembly having a plurality of secondary or sub-projectiles axially disposed within a barrel, which sub-projectiles are associated with discrete propellant charges for propelling said sub-projectiles sequentially from the barrel, wherein said array of barrel assemblies is capable of selectively firing the sub-projectiles from selected barrels whereby said projectile may deploy a predetermined pattern of sub-projectiles; and
[0024] communication means providing communication between the monitor and the defence for triggering selective activation of the defence for delivering a debilitating attack to the detected zone.
[0025] The monitors include one or more on-site sensors deployed in the designated area or remote-sensing means deployed remote from the designated area. Alternatively the monitoring means may include both on-site and remote sensing means.
[0026] The monitoring means may also provide a visual display of the monitored designated zone so that manual override means may be actuated, if desired, to enable manual control of the set defence means.
[0027] A number of secondary or sub-projectiles can be fired simultaneously from a plurality of barrels or in quick succession from the one barrel. In such arrangements the electrical signal may be carried externally of the barrel or it may be carried through the superimposed secondary projectiles which may clip on to one another to continue the electrical circuit through the barrel, or abut in electrical contact with one another. The sub-projectiles may carry the control circuit or they may form a circuit with the barrel.
[0028] The array of barrel assemblies may be arranged adjacent the leading end or the trailing end of the projectile for effecting changes in attitude of the projectile or medially for displacing laterally displacing the projectile. Alternatively the directional control system may include an array of barrel assemblies adjacent both leading and trailing ends of the projectile.
[0029] The or each array of barrel assemblies may fire a sub-projectile in a direction having a longitudinal component in order to provide a consequent addition to the kinetic energy of the projectile or a component in a direction tangential to the longitudinal axis of the missile in order to impart or change projectile rotation about its longitudinal axis. The barrel assembly may fire secondary projectiles across flight surfaces such as a wing to induce a further steering effect to the projectile. Alternatively barrel assemblies may extend through the aerofoil surfaces so as to fire in both directions. This may add structural strength to the aerodynamic design.
[0030] If desired, a separate array or opposing arrays of barrel assemblies may be provided to control projectile rotation about the longitudinal axis of the projectile. The configuration of the arrays may include opposing pairs of barrel assemblies that are fired simultaneously to effect changes in rotation about the longitudinal axis of the projectile only. The sub-projectiles may be selectively actuated before and/or after firing secondary projectiles form the directional control system to negate or utilise the effects on the projectile of such rotation about its longitudinal axis.
[0031] In certain embodiments of the present invention energy required to change attitude and/or the flight direction of the parent projectile may be provided by the firing of sub-projectiles from one or more selected barrel assemblies.
[0032] According to a second form of the present invention, there is provided a method of masking the launch location of a projectile launching apparatus is provided. The method includes the steps of discharging at least one projectile from a barrel assembly, said barrel assembly having a barrel, a plurality of projectiles axially disposed within the barrel for operative sealing engagement with the bore of the barrel, and discrete propellant charges for propelling respective projectiles sequentially through the muzzle of the barrel and, whilst said at least one projectile is in flight, firing at least one sub-projectile from an array of divert propulsion assemblies incorporated therein, each divert propulsion assembly having a plurality of sub-projectiles axially disposed within a divert propulsion barrel, which sub-projectiles are associated with secondary discrete propellant charges for propelling said sub-projectiles sequentially from the divert propulsion barrel, wherein said array of divert propulsion barrel assemblies is capable of selectively firing the sub-projectiles from selected divert propulsion barrels whereby said projectile is accelerated by the reactionary force generated by said firing of sub-projectiles.
[0033] The overall shape of the sub-projectile is not narrowly critical as the sub-projectile is a mass against which the secondary propellant acts and exerts a reactionary force on the breech of the divert propulsion barrel. In the context of the present form of the invention, the breech may be formed by subsequent sub-projectiles remaining in the barrel in sealing engagement with the bore of the divert propulsion barrel. The reactionary force is transferred from the breech of the secondary or divert propulsion barrel to the projectile and results in an acceleration of the projectile.
[0034] The array of barrel assemblies may be disposed radially from the centre of mass of the projectile. Such configurations of barrel assemblies are particularly suited to objects that do not incorporate an in flight propulsion system, ie. rockets and missiles. The firing of sub-projectiles simply displaces the projectile and the projectile continues upon its trajectory, save for the displacement, the apparent trajectory.
[0035] The present invention has particular application to area denial systems wherein the area is subject to shelling by projectiles launched from a pod, such as a mortar box. It will of course be understood that the present invention also has application to disguising the firing location of other projectile launching or firing systems.
[0036] In a preferred embodiment the apparent trajectory may be selected to draw fire from the launch apparatus to other enemy positions.
[0037] The projectiles of the present invention advantageously employ barrel assemblies of the type described in International Patent Application Nos. PCT/AU94/00124 and PCT/AU96/00459. Such barrel assemblies include a barrel;
[0038] a plurality of sub-projectiles axially disposed within the barrel for operative sealing engagement with the bore of the barrel, and discrete propellant charges for propelling respective sub-projectiles sequentially through the muzzle of the barrel.
[0039] The sub-projectiles may be round, conventionally shaped or dart-like and the fins thereof may be off-set to generate a stabilising spin as the dart is propelled from a barrel which may be a smooth-bored barrel. If required, the projectiles carrying the sub-projectiles may be substantially cylindrical, ovoid or spherical in shape.
[0040] The propellant charge may be form as a solid block to operatively space the sub-projectiles in the barrel or the propellant charge may be encased in metal or other rigid case which may include an embedded primer having external contact means adapted for contacting an pre-positioned electrical contact associated with the barrel. For example the primer could be provided with a sprung contact which may be retracted to enable insertion of the cased charge into the barrel and to spring out into a barrel aperture upon alignment with that aperture for operative contact with its mating barrel contact. If desired the outer case may be consumable or may chemically assist the propellant burn. Furthermore an assembly of stacked and bonded or separate cased charges and sub-projectiles may be provided for reloading a barrel.
[0041] Each sub-projectile may include a head and extension means for at least partly defining a propellant space. The extension means may include a spacer assembly that extends rearwardly from the head and abuts an adjacent sub-projectiles assembly.
[0042] The spacer assembly may extend through the propellant space and the head whereby compressive loads are transmitted directly through abutting adjacent spacer assemblies. In such configurations, the spacer assembly may add support to the extension means that may be a thin cylindrical rear portion of the head. Furthermore the extension means may form an operative sealing contact with the bore of the barrel to prevent burn leakage past the sub-projectile.
[0043] The spacer assembly may include a rigid collar which extends outwardly to engage a thin cylindrical rear portion of a malleable head inoperative sealing contact with the bore of the barrel such that axially compressive loads are transmitted directly between spacer assemblies thereby avoiding deformation of the malleable head. Complementary wedging surfaces may be disposed on the spacer assembly and head respectively whereby the head is urged into engagement with the bore of the barrel in response to relative axial compression between the spacer means and the head. In such arrangement the head and spacer assembly may be loaded into the barrel and there after an axial displacement is caused to ensure good sealing between the sub-projectile and barrel. Suitably the extension means is urged into engagement with the bore of the barrel.
[0044] The head may define a tapered aperture at its rearward end into which is received a complementary tapered spigot disposed on the leading end of the spacer assembly, wherein relative axial movement between the head and the complementary tapered spigot causes a radially expanding force to be applied to the sub-projectile.
[0045] The barrel may be non-metallic and the bore of the barrel may include recesses that may fully or partly accommodate the ignition means. In this configuration the barrel houses electrical conductors that facilitate electrical communication between the control means and ignition means. This configuration may be utilised for disposable barrel assemblies that have a limited firing life and the ignition means and control wire or wires therefore can be integrally manufactured with the barrel.
[0046] A barrel assembly may alternatively include ignition apertures in the barrel and the ignition means are disposed outside the barrel and adjacent the apertures. A non-metallic outer barrel that may include recesses adapted to accommodate the ignition means may surround the barrel. The outer barrel may also house electrical conductors that facilitate electrical communication between the control means and ignition means. The outer barrel may be formed as a laminated plastics barrel that may include a printed circuit laminate for the ignition means.
[0047] The barrel assembly may have adjacent sub-projectiles that are separated from one another and maintained in spaced apart relationship by locating means separate from the sub-projectiles, and each sub-projectile may include an expandable sealing means for forming an operative seal with the bore of the barrel. The locating means may be the propellant charge between adjacent sub-projectiles and the sealing means suitably includes a skirt portion on each sub-projectile that expands outwardly when subject to an in-barrel load. The in-barrel load may be applied during installation of the sub-projectiles or after loading such as by tamping to consolidate the column of sub-projectiles and propellant charges or may result from the firing of an outer sub-projectile and particularly the adjacent outer sub-projectile.
[0048] The rear end of the sub-projectile may include a skirt about an inwardly reducing recess such as a conical recess or a part-spherical recess or the like into which the propellant charge portion extends and about which rearward movement of the sub-projectile will result in radial expansion of the sub-projectile skirt. This rearward movement may occur by way of compression resulting from a rearward wedging movement of the sub-projectile along the leading portion of the propellant charge it may occur as a result of metal flow from the relatively massive leading part of the sub-projectile to its less massive skirt portion.
[0049] Alternatively the sub-projectile may be provided with a rearwardly divergent peripheral sealing flange or collar which is deflected outwardly into sealing engagement with the bore upon rearward movement of the sub-projectile. Furthermore the sealing may be affected by inserting the sub-projectiles into a heated barrel that shrinks onto respective sealing portions of the sub-projectiles. The sub-projectile may comprise a relatively hard mandrel portion located by the propellant charge and which cooperates with a deformable annular portion may be moulded about the mandrel to form a unitary sub-projectile which relies on metal flow between the nose of the sub-projectile and its tail for outward expansion about the mandrel portion into sealing engagement with the bore of the barrel.
[0050] The sub-projectile assembly may include a rearwardly expanding anvil surface supporting a sealing collar thereabout and adapted to be radially expanded into sealing engagement with the barrel bore upon forward movement of the sub-projectile through the barrel. In such a configuration it is preferred that the propellant charge have a cylindrical leading portion that abuts the flat end face of the sub-projectile.
[0051] The sub-projectiles may be adapted for seating and/or location within circumferential grooves or by annular ribs in the bore or in rifling grooves in the bore and may include a metal jacket encasing at least the outer end portion of the sub-projectile. The sub-projectile may be provided with contractible peripheral locating rings which extend outwardly into annular grooves in the barrel and which retract into the sub-projectile upon firing to permit its free passage through the barrel.
[0052] The electrical ignition for sequentially igniting the propellant charges of a barrel assembly may preferably include the steps of igniting the leading propellant charge by sending an ignition signal through the stacked sub-projectiles, and causing ignition of the leading propellant charge to arm the next propellant charge for actuation by the next ignition signal. Suitably all propellant charges inwardly from the end of a loaded barrel are disarmed by the insertion of respective insulating fuses disposed between normally closed electrical contacts.
[0053] Ignition of the propellant may be achieved electrically or ignition may utilise conventional firing pin type methods such as by using a centre-fire primer igniting the outermost sub-projectile and controlled consequent ignition causing sequential ignition of the propellant charge of subsequent rounds. Controlled rearward leakage of combustion gases or controlled burning of fuse columns extending through the sub-projectiles may achieve this.
[0054] In other embodiments, the ignition is electronically controlled with respective propellant charges being associated with primers that are triggered by distinctive ignition signals. For example the primers in the stacked propellant charges may be sequenced for increasing pulse width ignition requirements whereby electronic controls may selectively send ignition pulses of increasing pulse widths to ignite the propellant charges sequentially in a selected time order. Preferably however the propellant charges are ignited by a set pulse width signal and burning of the leading propellant charge arms the next propellant charge for actuation by the next emitted pulse.
[0055] Suitably in such embodiments all propellant charges inwardly from the end of a loaded barrel are disarmed by the insertion of respective insulating fuses disposed between insertion of respective insulating fuses disposed between normally closed electrical contacts, the fuses being set to burn to enable the contacts to close upon transmission of a suitable triggering signal and each insulating fuse being open to a respective leading propellant charge for ignition thereby.
[0056] In certain embodiments the barrel assemblies may be of the low-pressure type, which fire grenade-like sub-projectiles although high muzzle pressure barrel assemblies may be used. Respective barrel assemblies may be loaded with different sub-projectiles and the barrel assemblies may have different size bores for accommodating different size sub-projectiles.
[0057] Suitably each sub-projectile includes a trailing collar captively mounted to the sub-projectile body and when stored in the barrel, extends rearwardly to wedge against the nose portion of a trailing sub-projectile body. Suitably a shallow wedge provides the wedging action whereby, in use, the trailing end of the collar is expanded into operative sealing engagement with the barrel.
[0058] The trailing collar may be mounted for limited axial movement relative to the sub-projectile body and the leading end of the collar formed with an annular sealing face engageable with a complementary face formed on the sub-projectile body whereby rearward movement of the sub-projectile body resulting from the reaction of propellant gases thereon forces the its complementary face into sealing engagement with the annular sealing face at the leading end of the collar.
[0059] The complementary face and the annular sealing face may extend substantially radially and be formed with complementary sealing features thereon. However it is preferred that these faces are complementary part-conical sealing faces which wedge into tight sealing engagement with one another. The leading end part may also be expandable into operative sealing engagement with the barrel. Suitably however the wedging between the part-conical faces are relatively steep faces whereby the leading end of the collar is not expanded into operative sealing engagement with the barrel by the wedging action.
[0060] In low pressure applications, preferably each sub-projectile is associated with a high-pressure propellant chamber that exhausts to respective low-pressure propulsion chambers formed between the adjacent sub-projectiles for efficient low muzzle velocity operation. The high-pressure propellant chambers may be formed integrally with the sub-projectile body or the trailing collar or be provided at the exterior of the barrel to communicate therewith through ports provided through the barrel wall.
[0061] Suitably the configuration of the space into which the ignited propellant propagates and the propellant properties are such that only low barrel pressures occur in use, such as in the order of 2,000 psi to 5,000 psi. Typically the collar is such that in its relaxed attitude it does not prevent free movement of the projectile through the barrel either for loading purposes or during firing.
[0062] A pressure pad is mounted on the housing inwardly of the open trailing end. The collar is relocated from the engaged condition upon ignition of the propellant and is retained in a relaxed condition by the pressure pad for passage through the barrel and out the muzzle of the barrel.
[0063] The projectile may be of the conventional type and be conventionally fired or preferably be adapted to be fired from a barrel assembly that includes a plurality of projectiles axially disposed within a barrel wherein each of said projectiles are associated with a discrete propellant charges for propelling said projectiles from the barrel.
[0064] The projectile, in a preferred form, may be generally spherical in shape and have the multiplicity of barrel assemblies radially disposed from the centre of the sphere. The barrel assemblies may be the same or different. For example whilst large diameter barrels may be disposed from the centre of the spherical projectile. Smaller diameter barrels may be positioned between the larger diameter barrels to provide the maximum sub-projectile density in the projectile. It may be desirable to provide the projectile with the maximum barrel packing density and hence firepower. Alternatively it may be desirable to provide the projectile with a variety of barrel bores in order that sub-projectiles of a variety of calibres may be utilised.
[0065] The projectile may be a saboted projectile for advantageous deployment. A spherical projectile may be saboted into a more convenient shape for firing from a conventional deployment system such as in the form of a conventional munition. Alternatively if it is desirable to provide increased muzzle velocity a saboted projectile can accommodate an increased propellant charge without require a prohibitive barrel length.
[0066] Barrel assemblies that are radially disposed from the centre of mass of the projectile allow the projectiles to deploy the sub-projectiles in a regular and readily controlled manner. Barrel assemblies that are radially disposed from the centre of mass of the projectile allow the projectile to maintain its attitude. By deploying sub-projectiles in a manner that results in zero resultant reactive force on the projectile the projectile may be maintained on its desired trajectory
[0067] A number of sub-projectiles can be fired simultaneously, or in quick succession. In such arrangements the electrical signal may be carried externally of the barrel or it may be carried through the superimposed sub-projectiles that may clip on to one another to continue the electrical circuit through the barrel, or abut in electrical contact with one another. The sub-projectiles may carry the control circuit or they may form a circuit with the barrel.
[0068] The projectile of the present invention may deploy the sub-projectiles in a predetermined pattern that may be selected for particular applications. For example, in order to intercept and destroy an incoming missile, it is desirable to deploy the sub-projectiles in a manner that maximises the likelihood of the missile impacting with one or more of the sub-projectiles. Fragmentation systems have been employed to scatter fragments of a projectile in the path of an incoming missile. However, systems such as this that explode the projectile generally produce a band of fragments that disperse and form an expanding spherical shell. The projectiles may deploy the sub-projectiles of the invention in a more homogeneous manner throughout the space occupied by the predetermined pattern. By controlling the timing of the firing of the sub-projectiles it is possible to establish a three dimensional “frag” pattern having a substantially homogeneous distribution of sub-projectiles. Alternatively, the sub-projectiles may be concentrated in areas where the missile is more likely to be intercepted so as to increase the effectiveness of the deployed sub-projectiles.
[0069] The sub-projectile may contain material for forming air-borne images. The image forming material may include, for example, explosive matter, incendiary matter, incandescent or luminous matter or other matter to provide a highly visible temporary image. Alternatively, the image forming matter may include smoke, gas, particles or sheets or strips, such as in the nature of chaff, or other material capable of being dispersed to form, an image. Accordingly, the projectile of the invention may be advantageously employed to launch counter-measures from military aircraft. The image forming matter may also include means for slowing its descent from its dispersed position, such as a parachute and the like.
[0070] The sub-projectiles may be arranged in the barrel assemblies such that once fired and the image forming matter deployed, the desired temporary airborne image is formed. Sub-projectiles containing different image forming matter, either differing in colour or form, may be sequentially loaded into each barrel assembly.
[0071] The image forming matter may be deployed, for example, by explosive means, by stored energy or by separation of separable parts of the sub-projectile to expose the image forming matter or by any other suitable dispersing means.
[0072] The image forming matter may be contained within a housing that may be of any suitable configuration that provides for the containment of the image forming matter and is suitably configured for engagement with the trailing end of the expandable collar of the preceding projectile. Preferably the housing is of the type employed with grenade-like projectiles, having relatively squat shape although projectiles having elongate housings could also be employed.
[0073] The housing may suitably be formed from biodegradable material and/or combustible material. This material may be based on a natural product such as woodchip or a synthetic material, such as a biodegradable polymer.
[0074] Advantageously the projectiles of the present invention may deploy selected sub-projectiles in order to control the course of the projectile. Such deployment may be understood as a divert propulsion system and may be used to affect limited corrections to the position of the projectile for the deployment of the remainder of the sub-projectiles in the desired pattern.
[0075] The projectiles of the present invention may suitably be employed in a defence system of the type described in the present applicant's International Patent Application No. PCT/AU00/01351.
BRIEF DETAILS OF THE DRAWINGS
[0076] In order that this invention may be more readily understood and put into practical effect, reference will now be made to the accompanying drawings which illustrate preferred embodiments of the invention and wherein:
[0077] [0077]FIG. 1 is a cross sectional illustration of a projectile according to a preferred embodiment of the present invention;
[0078] [0078]FIG. 2 is a cross sectional illustration of a saboted projectile for use in a barrel assembly having a plurality of axially disposed saboted projectiles;
[0079] [0079]FIG. 3 is a cross sectional illustration of the firing of saboted projectiles as shown in FIG. 2;
[0080] [0080]FIG. 4 is a side elevational diagram of a defence system according to a further embodiment of the invention; and
[0081] [0081]FIG. 5 is a perspective diagram of the defence system of the further embodiment.
DESCRIPTION OF PREFERRED EMBODIMENTS
[0082] [0082]FIG. 1 shows a projectile 10 having six (6) large bore barrels 12 of a convenient calibre, although only four (4) are shown in this cross sectional representation. The remaining two (2) large bore barrels (extending perpendicularly to the page) are depicted at 11 . The cross sectional representation also shows four (4) medium bore barrels 13 of medium calibre, and forty-eight (48) small bore barrels 14 of relatively small calibre. The large bore 12 , medium bore 13 and small bore 14 barrels each contain a plurality of axially disposed sub-projectiles 16 , as represented on the drawing. The sub-projectiles are associated with propellant charges 17 and ignition means 18 , which ignition means may be sequentially fired under the control of an electronic controller 15 . In some embodiments, the projectile 10 may also contain an explosive charge for terminal detonation.
[0083] The electronic controller 15 , which is disposed in the centre of the projectile 10 behind the barrels 11 , 12 in this embodiment, may include sensors for tracking an incoming missile when in-flight. Alternatively, the electronic controller 15 may receive firing instructions from a remote tracking station via a communications link. The sequenced firing of a number of the sub-projectiles may thus be coordinated to provide an improved likelihood of impacting with the targeted incoming missile or similar threat.
[0084] [0084]FIG. 2 shows a projectile of the type shown in FIG. 1 with a sabot 20 , wherein the sub-projectiles are omitted for reasons of clarity. The projectile 10 is retained in a barrel within the sabot 20 . The sabot includes a forward sabot portion 21 , a rearward sabot portion 22 and an expanding sleeve 23 disposed about a chamfered rear surface 24 of the rearward sabot portion. The detonation and firing of a propellant charge in front of the forward sabot portion 21 forces the rearward sabot portion 22 against the expandable sleeve 23 and causes the expandable sleeve to sealably engage with the bore of a parent barrel.
[0085] [0085]FIG. 3 shows a series of projectiles 10 being fired from a parent barrel assembly 30 , having a plurality of parent barrels 31 , 32 and 33 . Projectile 10 A has been fired from barrel 33 and has discarded its sabot (not shown). Projectile 10 B has been fired from barrel 32 and the sabot 20 is shown in the process of being discarded. The expandable sleeve 23 has detached from the rearward sabot 22 and the rearward sabot 22 has also detached from projectile 10 B. Forward sabot 21 has similarly detached from the projectile 10 B. Projectile 10 C has been more recently fired from barrel 31 and the sabot 20 has commenced detachment from projectile 10 C.
[0086] Referring to FIGS. 4 and 5, it will be seen that a designated area 40 to be defended is monitored by an array of field sensors 41 distributed over the designated area and which may be of any suitable type such as pressure, acoustic or seismic type sensors.
[0087] The illustrated defence system 42 employs a weapon taking the form of a pair of grenade boxes 43 each using the barrel assemblies 30 and coupled to a remote sensing means 44 and to a receiver unit 49 associated with the field sensors 41 . The remote sensing means 44 , which in the embodiment is tower mounted, is adapted to sweep the designated area 40 using electro-optical or microwave techniques to monitor any intrusion into the designated area by a personnel, vehicles or other intruder.
[0088] The receiver unit 49 is adapted to receive signals from the array of field sensors 41 , using a radio frequency (RF) communications link in the embodiment (although a cable link may be employed in the alternative). Upon any sensed intrusion in the area 40 , the zone of the intrusion will be isolated for targeting by projectiles 10 fired from the grenade boxes 43 . Thus the designated area 40 is monitored by either or both of the array of field sensors 41 or by the remote sensing means 44 .
[0089] It is desirable that each grenade box 43 is located in a substantially concealed position, such as a hole in the ground. Once set up, the hole in which the grenade box 43 is placed may be back filled without causing any detrimental effects to the operation of the barrel assemblies 30 therein. In other arrangements, the grenade box 43 may be conveniently concealed in foliage and adjusted by screw jacks 48 associated with a support base 47 for the grenade box.
[0090] A subsidiary control circuit 43 a (see FIG. 5), provided as a plug-in connection to the grenade box 43 , is fitted on-site but not during transport so as to maintain safety of the weapon during transport. Once fitted with the control circuit 43 a , the weapon is armed and ready to fire in accordance with controls provided by the sensor unit 44 and/or the receiver unit 49 . The control circuit is suitably able to communicate with the electronic controller 15 in a respective projectile, as required.
[0091] A central remote sensor 44 in FIG. 2 is linked to multiple grenade boxes 43 via respective control circuits 43 a . In use, if an intrusion into the detected area is detected at a zone, such as any one of the zones indicated as 50 to 59 , the selected grenade box 43 can be activated to fire one or more projectiles 45 into that particular zone. The sub-projectiles may be subsequently fired a respective projectile 45 , either in accordance with a pre-selected sequence or under remote control, to produce a predetermined pattern of deployed sub-projectiles. The pattern of sub-projectiles is desirably chosen in accordance with the nature of the intruder.
[0092] An intruder coming into the designated area 40 may be in any of a number of forms and may include a plurality of intruders. An intruder may be military personnel, in the form of an infantryman or foot soldier. Alternatively, the intruder may be a manned or unmanned vehicle such as an armoured car or tank. The intruder may have sophisticated defence systems that may track the trajectory of an incoming round and calculate the location of the launch apparatus, thereby enabling an attack on the previously hidden launch apparatus. The defence system of the embodiment allows the trajectory of the projectile to be diverted in flight by launching sub-projectiles, thereby enabling an apparent trajectory to be tracked and the true location of the launch apparatus to be masked. If feasible, the apparent trajectory may be selected to draw enemy fire directed at the defence system 42 to other enemy positions.
[0093] Whilst the above defence system is land based, another aspect of the invention concerns projectiles that might be termed water mines. These water mines may be launched from a ship and remain floating in the water and activated for either remote control or autonomous operation using on-board sensor systems, including radar, sonar or infra-red sensors. A line of such mines, incorporating stabilising or anchoring means such as a suspended weight, could be laid to provide a marine defence perimeter capable or being activated or deactivated as required.
[0094] In another mode of deployment, projectiles of the invention may be dropped from an aircraft such as a helicopter. Stabilising or anchoring means, such as spikes, could be provided to fix retain projectiles in one position on the ground. A first layer of sub-projectiles could include sensor systems for launching to detect the presence of enemy troops or vehicles, which could be engaged as required by grenades in subsequent layers in individual barrels of the projectile. Further sensors may be provided in other layers for surveying the result of an engagement.
[0095] A further mode of deployment is to provide a projectile of a size that can be conveniently hand-held and deployed by throwing, similar to a conventional grenade. However, the incorporation of sub-projectiles in barrels in the hand-delivered projectile enables it to be used in a repeating mode using a pre-set time delay or a remote control facility. This may provide certain advantages in engagements that occur in closed spaces, such as in urban warfare or topography including caves. The sub-projectiles may incorporate non-lethal rounds and an audio annunciation system for warning, perhaps in a siege situation, that additional rounds are capable of being fired if the miscreants involved fail to surrender immediately.
[0096] Projectiles of the invention may be carried into space and delivered into orbit around a planet or moon as required, effectively comprising a satellite. Since the barrel assemblies can be radially dispersed within a generally spherical body, they function very effectively to correct the position of the satellite in orbit, protect a zone around a valuable satellite from space junk, meteorites and the like, or to engage an enemy space vehicle or satellite. A change of position can be undertaken much more rapidly in the low gravity environment because of the energy liberated by firing a solid sub-projectile, rather than a burst of gas as in conventional satellites. The satellite projectiles are suitably constructed so as to be consumed by combustion upon re-entry into the atmosphere subsequent to orbital decay.
[0097] In one particular form, the satellite may comprise a super-projectile which in turn may deploy projectiles of the present invention from radially disposed barrel assemblies therein, and those deployed projectiles may themselves be equipped with sub-projectiles, thus providing a two tiered defence system. This two tiered system of course may be employed in other applications of suitable scale.
[0098] It will of course be realised that the above has been given only by way of illustrative example of the invention and that all such modifications and variations thereto as would be apparent to persons skilled in the art are deemed to fall within the broad scope and ambit of the invention as is herein set forth in the following claims.
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A projectile (10) for firing from a barrel, said projectile including a multiplicity of barrel assemblies (12, 13, 14) radially disposed from the centre of mass of the projectile, wherein each of said multiplicity of barrel assemblies includes a plurality of sub-projectiles (16) axially disposed within a barrel; each of said sub-projectiles associated with a discrete propellent charge (17) for propelling a respective sub-projectile from the barrel, wherein said projectile is capable of selectively firing sub-projectiles (16), suitably with the aid of primers (18) each coupled to an electronic controller (15). to provide a predetermined pattern of deployed sub-projectiles. A defence system employing projectiles of the type described is also disclosed, together with a method for disguising the launch location of a projectile utilising divert propulsion.
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FIELD OF THE INVENTION
The invention relates to a high temperature resistant material with variable structural properties and insulative characteristics particularly suitable for use with equipment used in the metal making industry and in foundries.
BACKGROUND OF THE INVENTION
In the past various refractory fiber products have been developed for use in high temperature applications. My U.S. Pat. Nos. 4,396,792 and 4,358,630, the subject matter of which is incorporated herein by reference are examples of the use of refractory fiber as a protective coating and structural member for small molten metal temperature measuring devices. Although these refractory fiber devices have provided good results; their useful life or test repeatability is limited. Also, the cost of refractory fiber is high thus limiting its usefulness for large items.
SUMMARY OF THE INVENTION
The invention provides an insulative refractory fiber composition with a wide range of uses in high temperature applications and temperature measuring devices. When used as a protective coating with molten metal samplers, it greatly enhances the immersion life and reduces the cost and acts as an anti-wetting agent to prevent adhering of molten metal to objects immersed in the bath such as spoon, molten metal sampling devices and bath temperature measuring devices. The composition of the invention is a blend of carbon, a filler, refractory fibers and a curing agent or refractory cement. The composition is molded or cast into the intended article. The source of the carbon can be rice hull ash which also provides an SiO 2 insulative filler. The filler is low cost and light weight. The ash also contains carbon which may be in the form of graphite. The properties of the composition can be varied by changing the aggregate size of the rice hull ash and the proportion of ash in relation to the amount of fiber and the type curing agent and cement. The properties are also controlled by blending powders and aggregates of different particle size. The refractory fiber provides strength to the finished products and abrasion resistance. With large aggregate size the insulative capabilities are increased because of trapped air. Also the large aggregates are less dense, hence increasing the utility of the composition for certain applications requiring large size castings.
The composition can be formed into the desired shape either by casting or vacuum forming with a slurry. The ash provides a source of carbon which when used at high temperatures will form carbon monoxide and or carbon dioxide which will provide an insulating blanket of gas to minimize heat conduction, adhering of molten metal to the structure and enhance the life of the article at high temperatures.
Tests have shown that the composition when used as a protective jacket for devices immersed in molten metal can increase the temperature resistance up to 3200 degrees F. of a particular refractory fiber product whereas without the carbon additive the effective temperature of the refractory fibers will be 2800 degrees F.
Further objects, advantages and features of the invention will be apparent from the disclosure.
DESCRIPTION OF PREFERRED EMBODIMENT
Although the disclosure hereof is detailed and exact to enable those skilled in the art to practice the invention, the physical embodiments herein disclosed merely exemplify the invention. The scope of the invention is defined in the claims appended hereto.
In the following examples, the source of silica and carbon is rice hull ash or expanded rice hull ash which is rice hull ash reburned at a higher temperature and containing from 18% to 2% carbon. A refractory fiber such as Kaowool manufactured by Babcock & Wilcox can be employed. For example, Kaowool 2600 bulk fiber which is 55% alumina and 44.9% silica can be employed in some applications. Curing agents can be anything from Portland Cement, sodium silicate to colloidal silicate or other high temperature Inorganic cements which are readily cured in the air or at elevated temperatures from 100 degrees to 500 degrees F. An example of high temperature cement is Secor high alumina cement with a rating of 3,000 degrees F. and above.
The properties for a particular product or application relating to hardness or brittleness, insulating ability, maximum operating temperatures, breaking and compression strength, resistance to abrasion may be varied by the percentages of the foregoing components. With increases in refractory cement, the resulting product will be harder and more brittle and also at the high end of the density range. Increase in refractory fiber will provide more resistance to breaking and crushing and provide increased abrasion resistance. Increases in the rice hull ash will provide a lighter and cheaper product with high insulating ability. The higher carbon content will provide greater anti-wetting properties with minimum penetration by the molten metal and iron into the product and higher temperature resistance. Higher carbon will result in greater gas evolution at the surface of the product to prevent heat transfer by conduction as well as other insulating properties. The following examples are illustrative of the appropriate product ranges for particular products. In some cases the products are cast and in other cases they are vacuum formed. A curing agent such as sodium silicate can be added later. For instance, in a standard vacuum drawing process, a slurry of the refractory fiber and the SiO 2 and C can be drawn against a screen with the water removed. The article is then immersed in a vessel of sodium silicate and a vacuum is again pulled to coat and penetrate the product with sodium silicate.
In a casting process, all ingredients can be blended and then poured into a mold in the shape of the desired article.
In the examples the mesh sizes of the ash are given where appropriate. Rice hull ash is available at 6-8 mesh with 94%-98% SiO 2 and 6%-2% carbon and at 325 mesh at 86% to 79% SiO 2 and 13% to 20% carbon. In the examples specific percentages were obtained or determined.
The use of powder of 325 mesh in the examples provides increased carbon to enhance the non-wetting characteristics because of the powders increased carbon content. The powder is also a good inexpensive filler which fills the spaces between the aggregates. The large particles of up to 1/8th inch provide the aggregate necessary to enable the cement to bond the particles into an integrated matrix.
The following specific compositions were formed and densities calculated.
Composition No. 1
9 lbs Secor Cement
7 lbs Large Expanded Rice Hulls
4 lbs High carbon fine black rice hulls--Producers
2 lbs 2700 degrees Long Fiber Kaowool
26 lbs Water
Dried 48 hours--after 24 hours heated 12 hours 250 degrees for the 18% further weight loss.
Density 36 lbs per cu ft.
Composition No. 2
15 lbs Large Expanded Rice Hulls
15 lbs Small expanded rice hulls
15 lbs refractory cement
25 lbs Water
Weight loss 32.9% on finished weight, after drying 48 hrs @110 degrees then 250 degrees for 12 hours.
Density 37.95 lbs per cu ft.
Composition No. 3
17 lbs Fine Black Rice Hull Ash
5 lbs refractory cement
Water quantity unknown
Weight loss 43% based on finished weight after 12 hours at 250 degrees.
Composition No. 4
13 lbs Large Rice Hull Ash
5 lbs refractory cement
Water quantity unknown
Weight loss 37% based on finished weight. Density 36.99 lbs per cu ft.
Specific examples for various illustrative products are as follows:
EXAMPLE No. 1
The following composition provided good results for a pouring spoon for taking iron and steel for various tests. Pouring spoons are typically available in sizes which range from 31/2 inches to 10 inches in diameter. Pouring spoons have been used for many years in the industry. This composition is also suitable for use with immersion samplers and bath measuring devices as shown in my U.S. Pat. Nos. 3,805,621; 3,481,201; 3,748,908; 3,859,857; 3,996,803; 4,140,019; 3,905,238, the entire subject matter which is incorporated herein by reference. With the composition set forth herein, pouring spoons have been successfully vacuum formed. Satisfactory results have been provided with a composition comprising 50% 2,700 degrees F. refractory fiber and 50% SiO 2 - C powder. The SiO 2 - C powder is a burned and expanded rice hull ash having a composition 84% SiO 2 , 15% C and 1% miscellaneous elements such as sodium and potassium. These ingredients are mixed in water and vacuum drawn into a screen mold followed by a drawing after immersing in a vessel of sodium silicate solution (Milwaukee solvents silicate 40-42) having a Na 20 to SiO 2 weight ratio of 3/22, 9.1% Na 30%, SiO 2 , a Baume of 30%. The mold then is secured immediately at 110 degrees F. for 24 hours. The resulting product had high temperature resistance at 3,000 degrees F., high crush strength and physical strength, average insulation ability, average density and high abrasion resistance. Also, the non-wetting properties with respect to molten metal were very high because of the high temperature of carbon Shrinkage is not critical.
EXAMPLE No. 2
Ladle or tundish, insulating cover for full or empty units. The foregoing product is made by casting, and comprises 30% Secor high alumina refractory cement, 30% SiO 2 - C powder, 325 mesh, and 40% SiO 2 - C 1/8th inch particle size retained by 1/8th inch mesh screen. The powder has 84% SiO 2 , 15% carbon, 1% other elements. The 1/8th inch size particles comprised 96% SiO 2 and 3% carbon, 1% other elements. The foregoing are mixed with water and cast and cured for 48 hours at 110 degrees F. and then trimmed and formed into the desired shape. The ladle or tundish produced thereby has high insulation characteristics, high temperature capability, low cost, low density, average strength, average abrasion resistance and hardness and average non-wetting capability, also average crush resistance and rates poor in shrinkage, a property not important with this product.
EXAMPLE No. 3
Tundish liner board. This product is made by casting a composition which includes 25% high temperature refractory fiber, 20% Secor high alumina high temperature cement, 35% SiO 2 - C powder, which had a composition of 85% SiO 2 and 15% C and the balance 20% SiO 2 - C 1/8th inch 6-8 mesh with 97% SiO 2 , and 3% C. The resulting product had good temperature resistance, good abrasion resistance, high density and was brittle but hard. It also had average breaking strength.
EXAMPLE No. 4
Ladle to tundish shroud or tundish to mold comprising 40% high temperature long refractory fibers, 50% SiO 2 - C powder, 325 mesh, 85% SiO 2 , 15% C, 10% SiO 2 - C and 6-8 mesh with a silica carbon ratio of 95% SiO 2 and 5% carbon. After the product is formed, sodium silicate cement was applied with the vacuum process recited above regarding Example 1. The resulting product had high resistance to abrasion, good non-wetting characteristics, high strength, hardness, high temperature resistance and crush resistance. The product had low density, insulation value was average, shrinkage was poor.
EXAMPLE No. 5
Ingot stool covers, ingot seals and ingot stool coating formed by-vacuum forming. The composition included 17.5% of high temperature refractory fiber, 40% SiO 2 - C, 85% SiO 2 , 15% C powder, 421/2% SiO 2 - C 6-8 mesh having a composition 98% SiO 2 , 2% carbon. The resulting product was cured with sodium silicate as in Example 1 with a Baume of 30%. The resulting product had good non-wetting properties, good temperature resistance, good breaking strength, average cost, poor crush strength, poor abrasion resistance, poor insulation characteristics, poor shrinkage and hardness.
EXAMPLE No. 6
Insulating block for a wide range of uses including structural uses, the block formed by casting in a mold the following composition: 30% Secor high temperature alumina cement or Portland cement depending on application and if high temperature resistant characteristics are not required, 30% 6-8 mesh SiO 2 - C at a ratio of 95% SiO 2 to 5% carbon, 35% 1/8th inch particle size SiO 2 - C, comprised of 97% SiO 2 , 3% carbon and 5% high temperature refractory fiber mixed with water cast and formed by sawing blocks. The properties are good insulation characteristics, low density and cost, high temperature resistance, average crush resistance, abrasion resistance and hardness, poor braking strength, shrinkage and non-wetting capabilities.
The foregoing examples and tests performed on these products revealed that the anti-wetting capability of graphite together with its formation of CO and/or CO 2 when contacted by molten metal provide the desirable temperature resistance.
The cost savings, temperature resistance and insulation capability as well as the weight and strength characteristics make the foregoing compositions suitable for a wide range of products including those employed in the molten metal and metal smelting business. As indicated, some of these compositions and the ones that use refractory cement are readily cast in a manner similar to concrete. All the products can be worked or machined with woodworking or metal working machinery.
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Disclosed herein is a method and composition of matter for constructing temperature resistant parts for the metal making industry from a mix of refractory fibers and Silca-carbon in the form of burned rice hull ash.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates generally to three-dimensional (3D) computerized tomography (CT) and more specifically, to a method and apparatus for improving the computational efficiency of an exact cone beam reconstruction.
2. Description of the Background Art
Recently a system employing cone beam geometry has been developed for 3D imaging that includes a cone beam x-ray source and a 2D area detector. An object to be imaged is scanned, preferably over a 360° angular range, either by moving the x-ray source in a scanning path about the object or by rotating the object while the source remains stationary. In either case, the area detector is fixed relative to the source, and relative movement between the source and object provides the scanning (irradiation of the object by the cone beam energy). The cone beam approach has the potential to achieve 3D imaging in both medical and industrial applications both rapidly and with improved dose utilization.
The 2D area detector used for 3D imaging generally has detector elements arranged in a 2D array of rows and columns. Available area detectors have generally been of large size and low quality, such as used with x-ray image intensifiers, or of small size and high quality. High cost and other factors have made large area 2D array detectors having high quality and high resolution, generally unavailable. In U.S. Pat. No. 5,390,112 entitled THREE-DIMENSIONAL COMPUTERIZED TOMOGRAPHY SCANNING METHOD AND SYSTEM FOR IMAGING LARGE OBJECTS WITH SMALL AREA DETECTORS issued Feb. 14, 1995, and hereby incorporated by reference, a cone beam CT system is disclosed in which an x-ray source following a spiral scan path is used to image a relatively long object, wherein the x-ray detector is much shorter than the object. The only height requirement for the detector is that it be longer than the distance between adjacent turns in the spiral scan of the x-ray source. As the cone beam source follows the scan path, the detector acquires many sets of cone beam projection data, each set representative of the x-ray attenuation caused by the object at each of the many source/detector positions along the scan path.
The cone beam projection data is then manipulated to reconstruct a 3D image of the object. The manipulation of the cone beam projection data is quite computationally complex and comprises:
1) conversion of the projection data to Radon derivative data. This may be generally be accomplished using the techniques described in U.S. Pat. No. 5,257,183 entitled METHOD AND APPARATUS FOR CONVERTING CONE BEAM X-RAY PROJECTION DATA TO PLANAR INTEGRAL AND RECONSTRUCTING A THREE-DIMENSIONAL COMPUTERIZED TOMOGRAPHY (CT) IMAGE OF AN OBJECT issued Oct. 26, 1993, hereby incorporated by reference,
2) conversion of the Radon derivative data to Radon data at polar grid points using, for example, the technique described in U.S. Pat. No. 5,446,776 entitled TOMOGRAPHY WITH GENERATION OF RADON DATA ON POLAR GRID POINTS issued Aug. 8, 1995, also hereby incorporated by reference, and
3) performing an inverse 3D Radon transformation of the Radon data at the polar grid points using well known techniques, such as those described in detail in the fore-noted U.S. Pat. No. 5,257,183 for reconstructing image data that when fed to a display provides a 3D CT image of the object.
In view of the above computationally complex image data processing, efforts are needed for reducing the complexity.
Prior U.S. Pat. No. 5,333,164 entitled METHOD AND APPARATUS FOR ACQUIRING AND PROCESSING ONLY A NECESSARY VOLUME OF RADON DATA CONSISTENT WITH THE OVERALL SHAPE OF THE OBJECT FOR EFFICIENT THREE DIMENSIONAL IMAGE RECONSTRUCTION, issued Jul. 16, 1994 discloses a technique for reducing the amount of computation needed to make a 3D cone beam CT image by a priori knowledge of the aspect ratio of the object being imaged for reducing the points in Radon space that are sampled. Although this technique reduces computationally complexity, it would be desirable to reduce the required computations at an earlier stage of the reconstruction processing.
Prior U.S. Pat. No. 5,390,226 entitled METHOD AND APPARATUS FOR PRE-PROCESSING CONE BEAM PROJECTION DATA FOR EXACT THREE DIMENSIONAL COMPUTER TOMOGRAPHIC IMAGE RECONSTRUCTION OF A PORTION OF AN OBJECT, issued Feb. 14, 1995 discloses a technique for reducing the amount of computation needed to make a 3D cone beam CT image by attempting to retain for further processing that cone beam attenuation data acquired within a select region on the surface of the detector that provides projection data corresponding to beams actually attenuated by passing through the object. Thus, unnecessary detector data is discarded at the earliest possible opportunity of the image processing. However, the technique of U.S. Pat. No. 5,390,226, as illustrated in FIG. 2 (b) therein, only masks the detector data, i.e, reduces the projection data, by limiting the data used for further processing to that data between upper and lower projections of the object on the detector, i.e., the upper and lower boundaries of the "shadow" of the object. The projection data between the left and right boundaries of the object shadow and the left and right boundaries of the detector are not so limited, and in fact are ignored and assumed to not exist.
Since a practical CT imaging system is designed to image an object having a given maximum width, when the object being imaged is less than the maximum width, when using the technique of U.S. Pat. No. 5,390,226 there will be no useful projection data between the left and right boundaries of the object shadow and the left and right boundaries of the detector. It would be desirable if means were provided to actually determine the width of the object shadow in order to properly reduce the amount of data being processed.
Furthermore, if the actual object being imaged is not symmetric, as is the case, for example, with a medical patient, as the source/detector moves about the scan path, the width of the shadow will vary, resulting in a variable shadow width. The technique of U.S. Pat. No. 5,390,226 assumes a fixed width for the object shadow, requiring that a maximum permissible width be used to prevent the generation of image artifacts.
An object of the present invention is to reduce the computational complexity of 3D cone beam image reconstruction at the earliest possible stage in the reconstruction processing.
It is a further object of the invention to provide such reducing computation in an adaptive manner, thereby maximizing the efficiency of the image reconstruction processing.
SUMMARY OF THE INVENTION
In accordance with the principles of the present invention, for each set of detector data, the right and left boundaries of the object's projection are determined in a pre-processing step. Consequently, later in the reconstruction processing, only those line integrals which contain actual information are carried out, thereby speeding-up the exact cone beam reconstruction algorithm.
More specifically, means are provided for determining the area on the detector which is covered by the width of the object's projection. Based on this knowledge, each integration line is checked to determine if it intersects the projection of the object. If it is determined that the corresponding integral would not contain any relevant information, that line integration is not performed.
Furthermore, the efficiency of the calculation of the line integrals which do contain valid object information is also improved. This is possible by shortening the integration line and integrating the projection data only over the length of the line which lies inside the actual projection of the object on the detector. The narrower the object being imaged, the greater the increase in efficiency for calculating the line integrals.
The present technique is highly efficient and reduces the computations required for objects having a width that is less than the maximum width that can be imaged. Additionally, the present technique is adaptive to the changing shape of the object's projection on the detector, further increasing the computational efficiency. In comparison, the computational cost of the standard implementation is fixed at a relatively high level as determined by the largest possible width of the projection of the object.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a simplified perspective illustration of the imaging of an object using an x-ray source and detector, combined with a simplified block diagram of image reconstruction according to the present invention; and
FIG. 2 illustrates a pixelated detector having object projection data therein, useful for describing the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 illustrates a cone beam 3D CT imaging system useful for carrying out the present invention, which is substantially the same, except as to be specifically described later, as known in the forenoted U.S. Pat. No. 5,390,112. As illustrated, a computer controlled manipulator 6, in response to control signals from an appropriately programmed computer 8, cause a source of cone beam energy 10 and a two-dimensional array detector 12 to cooperate along a defined source scanning trajectory, illustrated as a spiral scan path 14 centered on a predetermined axis 15 of an object 16, allowing detector 12 to acquire complete cone beam projection data for eventual reconstruction of an image of object 16. Computer 6, manipulator 8, source 10 and detector 12 cooperate in a manner generally well understood by those skilled in the art, i.e., such as described in detail in my forenoted U.S. Pat. No. 5,390,112, and therefore further details of their operation is not necessary. Alternatively, and equivalently, object 16 could be rotated to cause scanning by a fixed position source and detector. Furthermore, the scanning can be accomplished in a continuous or stepwise manner, and the spiral path can have equally spaced turns (sometimes referred to as stages), or turns with increasing pitch at the top and bottom edges of a region of interest of the object. Furthermore, although source 10 is shown as an x-ray source, other types of imaging energy might be used, such as neutrons, positrons, etc.
Signals corresponding to the sensed x-ray energy falling on elements within detector 12 are supplied to a data acquisition system (DAS) 17 which, like the previously described portions of FIG. 1, may operate in a fashion well known to those of ordinary skill in this technology for digitizing, pre-processing, and storing of the cone beam projection data.
Cone beam projection data from the DAS 17 is supplied to a processor 18, which may be a computer programmed to perform various data conversions illustrated by the blocks within the processor 18. At block 20 the cone beam data is converted to Radon derivative data. This may be generally be accomplished using the techniques described in the forenoted U.S. Pat. No. 5,257,183. At block 22 the Radon derivative data is converted to Radon data at polar grid points using, for example, the technique described in the forenoted U.S. Pat. No. 5,446,776. The Radon data at the polar grid points is supplied to block 24 which performs an inverse 3D Radon transformation using well known techniques, such as those described in detail in the forenoted U.S. Pat. No. 5,257,183. At block 26 reconstructed image data is developed, and then fed from processor 18 to a display 28, which may operate in known fashion, to provide 3D CT imaging of object 16.
A more detailed description of the blocks of FIG. 1 can be found in the forenoted patents incorporated by reference herein.
As previously forenoted, the exact cone beam reconstruction algorithm as described in U.S. Pat. No. 5,257,183 is based on the calculation of line integrals to determine the Radon transform of the x-rayed object. The line integrals are performed on the projection data provided by the 2-D detector. The size of this detector determines the maximum width of the object.
In a straightforward implementation of the algorithm, one calculates all the line integrals necessary to fill up the Radon support corresponding to this largest possible object. A real object, however, would usually be smaller than the maximal allowable one. Furthermore, when we think of a human patient, the "object" would also exhibit smaller and larger widths for different projections as it is non-cylindrical.
To calculate the full, standard Radon support for such objects is inefficient since one spends time calculating and processing Radon points which contain no information about the image of the object.
In accordance with the principles of the present invention, before calculating the line integral data necessary for developing the Radon derivative data (block 20) for each projection image, the extent of the object projection on the detector, e.g., it's left and right boundaries, are determined. Once determined, only line integrals need to calculated that intersect the actual width of the projection data. Furthermore, one may even speed-up the calculation of the integrals which do contain valid object information. This is possible by shortening the integration line (i.e., adjusting it's start and end points) so as to integrate projection data only over the part of the line which lies inside the object's projection.
FIG. 2 illustrates a pixelated detector having object projection data therein, useful for describing the present invention.
One efficient technique for finding the width of the object's projection is:
1) Check the value of the projection data through one row of pixels (e.g. the top row of the detector), from left to right, until data representative of the object is first encountered (as determined by sensing a value for the projection data that is non-zero). This position is easy to recognize since the contrast between outside and inside of an object (human patient) is strong.
2) From the first encounter, we move back towards the left edge of the detector, now calculating the sum of the projection data over each column of pixels. Assuming the values outside the object are substantially zero, we progress until we encounter the first vertical sum with a value of (about) zero. This corresponds to the left boundary of the projection of the object.
The same procedure, in reverse directions, starting from the right edge of the image, can be used to determine the right boundary of the projected object.
Performing the vertical summation of the projection data is a fast process and could be implemented in hardware. The assumption of values of zero outside the projection is reasonable for practical situations. Due to noise, however, one needs to use a small non-zero threshold when deciding whether a particular column of pixels is completely outside the projected object or not.
The above technique can be simply carried out as a pre-processing step (i.e., before block 20), by DAS 17.
Thus, there has been shown and described a novel method and apparatus for speeding up the reconstruction of an image in a cone beam 3D CT imaging system. Many changes, modifications, variations and other uses and applications of the subject invention will, however, become apparent to those skilled in the art after considering this specification and its accompanying drawings, which disclose preferred embodiments thereof. For example, after finding one of the boundaries of the object's projection, one could continue to sense projection data along the same row until the opposite boundary is found.
Furthermore, although in the illustrated embodiment the left and right boundaries are determined as straight lines, one could examine the object's projection on a row-by-row basis to form contoured left and right boundaries.
Additionally, although in this illustrated embodiment DAS 17 pre-processes the projection data to determine the left and right boundaries, a simple analysis of line integrals that are only vertically oriented on the detector can easily indicate the left and right boundaries, and in fact is equivalent to the forenoted summation of the columns of projection data.
All such changes, modifications, variations and other uses and applications which do not depart from the spirit and scope of the invention are deemed to be covered by this patent, which is limited only by the claims which follow as interpreted in light of the foregoing description.
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A scanning and data acquisition technique for three dimensional (3D) computerized tomographic (CT) imaging of an object, wherein scanning at a plurality of positions along a source scanning trajectory causes an area detector to acquire cone beam projection data corresponding to a shadow of said object at each of scanning positions and Radon derivative data is calculated by processing line integral values from cone beam projection data. In order to improve the calculation efficiency of the Radon derivative calculation, calculation of the Radon derivative data uses a determination of the left and right boundaries of the shadow for each of the scanning positions, and calculates the Radon derivative data only using projection data from within the determined boundaries.
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TECHNICAL FIELD
Embodiments of the invention relate generally to an apparatus and method for direct switching of software threads.
BACKGROUND
A software thread is a stream of instructions that are to be executed by a processor. As known to those skilled in the art, when a software thread is placed in a sleep state, the thread is deactivated by a scheduler and the thread is then re-activated when a given external event occurs such as, for example, the expiration of the sleep time period or when a currently running thread issues a wakeup call to the sleeping thread. Note that in other systems, the “sleep state” is alternatively called a “waiting state” or “suspended state”. In the sleep state, the thread is typically placed in a queue (“sleep queue”) of threads waiting for a lock (i.e., synchronization object). When a thread is placed in the sleep state, the thread does not consume a significant amount of processor time. A lock is associated with a shared resource (e.g., a CPU core) so that other threads will be blocked from accessing the shared resource until a currently running thread has completed its operation in the shared resource and has released the lock.
When a particular thread has to wait for a shared resource because a currently running thread is using that shared resource, the particular thread will go into the sleep state. When the resource becomes available because the currently running thread has released the lock for the resource, the currently running thread will issue a wake-up call to the sleeping thread (i.e., the thread in a sleep state). When the sleeping thread is woken up, the scheduler places the woken-up thread on a run queue. The scheduler can then pick up the woken-up thread in the run queue and execute that thread. However, this woken-up thread is unable to run at least until a currently running thread on the processor is switched out by the scheduler. The wait time for this woken-up thread to run may vary, depending on the run queue load (i.e., the number of threads that are ahead of the woken-up thread in the run queue) and the relative priorities of the threads that are already in the run queue.
One problem that may occur is that a resource may be available (i.e., the resource is in an unlocked-state) for use by threads, but only the woken-up thread is permitted to acquire this available resource. No other thread other than the woken-up thread can acquire this resource. As mentioned above, this woken-up thread may also be waiting in the run queue and waiting its turn to run until other appropriate threads in the queue have run. In this circumstance, it is important that the woken-up thread runs as soon as possible and use the resource that only the woken-up thread can acquire, so that unnecessary contention on that resource by threads and wasted CPU (central processing unit) consumption are reduced. For example, this additional contention is due to the woken-up thread contending with other threads for a global lock before the woken-up thread can obtain a resource-specific lock for that resource. Current approaches do not provide a solution to the above-discussed problem. For example, one possible approach is to increase the priority of the woken-up thread so that the wait time in the run queue of the woken-up thread is reduced. However, this approach is expensive in terms of additional hardware and software overhead, and does not always lead to a significant reduction in the wait time in the run queue of the woken-up thread.
Therefore, the current technology is limited in its capabilities and suffers from at least the above constraints and deficiencies.
BRIEF DESCRIPTION OF THE DRAWINGS
Non-limiting and non-exhaustive embodiments of the present invention are described with reference to the following figures, wherein like reference numerals refer to like parts throughout the various views unless otherwise specified.
FIG. 1 is a block diagram of an apparatus (system) in accordance with an embodiment of the invention.
FIG. 2 is a block diagram illustrating the locality domain bindings of threads that are checked by an embodiment of the invention.
FIG. 3 is a block diagram illustrating the contention of multiple software threads on resources.
FIG. 4 is a flow diagram of a method in accordance with an embodiment of the invention.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
In the description herein, numerous specific details are provided, such as examples of components and/or methods, to provide a thorough understanding of embodiments of the invention. One skilled in the relevant art will recognize, however, that an embodiment of the invention can be practiced without one or more of the specific details, or with other apparatus, systems, methods, components, materials, parts, and/or the like. In other instances, well-known structures, materials, or operations are not shown or described in detail to avoid obscuring aspects of embodiments of the invention.
FIG. 1 is a block diagram of an apparatus (system) 100 in accordance with an embodiment of the invention. The apparatus 100 can be implemented in, for example, a computer system. For purposes of discussing the details of an embodiment of the invention, the software threads T 1 and T 2 are used as examples. The software threads T 1 and T 2 are streams of instructions that are to be executed by a processor 105 for a software 110 . If the processor 105 is a multi-core processor, then a core (e.g., core 105 a or 105 b ) of the processor 105 will execute at least one of the threads T 1 and T 2 . In another example, the thread T 2 may be a thread of a software that is different from the software 110 . The number of threads associated with a software and the number of software in the system 100 may vary.
A scheduler 115 can place any software thread in a sleep state 120 when the scheduler 115 places the thread in the sleep queue 125 . When a thread is sleeping (i.e., is in the sleep state 120 ), the thread is deactivated by the scheduler and the thread is then re-activated when a given external event occurs such as, for example, the expiration of the sleep time period or when a currently running thread issues a wakeup call to the sleeping thread. When a thread is placed in the sleep state 120 , the thread does not consume a significant amount of processor time.
The scheduler 115 can be implemented by, for example, use of known programming languages such as, e.g., C or C++, and can be programmed by use of standard programming techniques.
An embodiment of the invention provides a system (apparatus) 100 to run a woken-up software thread immediately by directly switching to the woken-up thread and the decision to directly switch the woken-up thread is based on a selection criteria 130 , as discussed further below. As a result, this directly switched in thread (e.g., thread T 2 in the example below) is not placed in the run queue 135 . Therefore, the system 100 advantageously reduces the prior latency between the time when a software thread is placed on a run queue 135 (from the sleep queue 125 ) and the time when the software thread will run on a processor 105 (or processor core 105 a or 105 b ). In cases where only the woken-up thread can acquire a particular resource, an embodiment of the invention advantageously reduces the unnecessary contention on that resource by threads and wasted CPU consumption due to the unnecessary contention.
As an example, assume that the threads T 1 and T 2 are to run on the processor 105 . In this example, assume that the threads T 1 and T 2 are to run on the processor core 105 a . If thread T 1 is first running on the core 105 a , then the scheduler 115 will place the thread T 2 in the sleep queue 125 because thread T 2 is waiting for a resource (i.e., core 105 a ) that is currently not available to the thread T 2 .
When the thread T 1 has finished working on a resource and has released a lock (mutex) 141 for the core 105 a , the thread T 1 will issue a standard wakeup call 140 in a conventional manner to the thread T 2 , when thread T 1 releases the lock 141 for the core 105 a . The scheduler 115 detects the wakeup call 140 . In response to the detection of the wakeup call 140 , the scheduler 115 will remove the woken-up thread T 2 from the sleep queue 125 .
As previously discussed above, in prior systems, the thread T 2 is placed in the run queue 135 in a waiting state 145 and will start running on the available resource (e.g., core 105 a ) when the thread T 2 becomes the most eligible thread on the run queue 135 . Therefore, other threads that are ahead of the woken-up thread T 2 in the run queue 135 and higher priority threads in the run queue 135 will run before a scheduler 115 will pick up the thread T 2 to allow the thread T 2 to start running on the core 105 a.
In an embodiment of the system 100 , when the thread T 2 is woken up and removed from the sleep queue 125 , the scheduler 115 applies a set of selection criteria 130 in order to determine if the thread T 2 is eligible for direct switching into the resource that thread T 2 is waiting on, so that the thread T 2 will immediately run on the resource (e.g., core 105 a ).
If the woken-up thread T 2 is eligible for direct switching, the scheduler 115 will directly switch the running thread T 1 with the woken-up thread T 2 . Typically, a context switch module 155 in the scheduler 115 performs a context switch so that the thread T 1 is switched out of the core 105 a and the thread T 2 is directly switched in the core 105 a from the sleep queue 125 . As known to those skilled in the art, a context switch is a computing process of permitting multiple processes or threads to share a single CPU resource. The specific steps that are performed by the context switch module 155 during a context switch are well known to those skilled in the art. In a context switch, the state of a first thread is saved, so that when the scheduler gets back to the execution of the first thread, the scheduler can restore this state and continue normally. The state of the thread includes, for example, all the registers that the thread may be using and any other operating system specific data that are used by the thread.
As a result of this direct switching, the thread T 1 that is issuing the wakeup call 140 is placed by the scheduler 115 on the run queue 135 before switching to the woken-up thread T 2 . The thread T 1 is place on the run queue 135 because this placement is only the next logical transition for T 1 (i.e., T 1 cannot be placed in a sleep queue). When the scheduler 115 directly switches the woken-up thread T 2 , the thread T 2 will then run on the core 105 a . Additionally, when the thread T 2 is switched in, the thread T 2 will then run even if there are other threads (in run queue 135 ) with a higher priority than the priority of thread T 2 .
The thread T 2 , which has been switched in, will typically only be given the remaining timeslice of the switched-out thread T 1 to run on the core 105 a , so that the scheduler 115 can still comply within the POSIX (Portable Operating System Interface) boundaries. As known to those skilled in the art, POSIX is a set of standard operating system interfaces based on the UNIX operating system. Therefore, for a timeslice value 150 that the thread T 1 is permitted to use when running on the core 105 a , the used timeslice 105 a is the actual time that the thread T 1 has already spent running on the core 105 a and the remaining timeslice 105 b is the remaining time in the timeslice value 105 that has not been used by the thread T 1 while running on the core 105 a . The thread T 2 will then run on the core 105 a for the duration of the remaining timeslice 150 b , instead of running for the entire time length of the scheduler timeslice 150 . The used timeslice 105 a and remaining timeslice 105 b are time values that are typically tracked by the scheduler 115 .
In an embodiment, the selection criteria includes a CPU binding or/and locality-domain (LDOM) binding of the thread (generally shown as binding 160 , the amount 165 of time the thread has been sleeping, and/or resources held attributes 180 . The binding 160 contains data structure that indicates the processor or locality domain that a thread is bounded to and will run in. Locality domains are discussed in further details in commonly-assigned U.S. patent application Ser. Nos. 11/104,024 and 11/224,849. U.S. patent application Ser. Nos. 11/104,024 and 11/224,849 are hereby fully incorporated herein by reference.
The resources held attributes 180 tracks the resources that are held by the threads and resources that the threads are trying to obtain. The example in FIG. 3 below discusses how the scheduler 115 uses this attributes 180 to determine if a woken-up thread in the sleep queue 125 should be directly switched into the resource according to the manner discussed above.
Reference is now made to FIGS. 1 and 2 for discussing an example operation of the system 100 . As mentioned above, the scheduler 115 checks the selection criteria 130 to determine if it should switch out thread T 1 and switch in thread T 2 to a resource (e.g., core 105 a ). As an example, assume that a first locality domain LDOM 1 has processors 205 a and 205 b , cache 210 , and memory 215 . Additional details of locality domains are discussed in the above cited commonly-assigned U.S. patent application Ser. Nos. 11/104,024 and 11/224,849. A second locality domain LDOM 2 has processors 220 a and 220 b , cache 225 , and memory 230 . As an example, if thread T 1 is bound to LDOM 1 , then the thread T 1 will populate data into the cache 210 or 215 , where this populated data is needed or used by the running thread T 1 .
As an example, if threads T 1 and T 2 are both bound to the same locality domain LDOM 1 , then the scheduler 115 will directly switch out thread T 1 and switch in thread T 2 to a resource (e.g., core 105 a ) after the scheduler 115 detects the wakeup call 140 ( FIG. 1 ). Therefore, if no other thread can obtain the resource 105 a (other than threads T 1 and T 2 ), then the thread T 2 will be able to immediately use the resource 105 a even if there are other threads in run queue 135 ) where these other threads have a higher priority than the thread T 2 . As a result of thread T 2 being able to obtain the resource 105 a that other threads cannot use, the direct switching of thread T 2 to run on the resource 105 a will reduce the unnecessary contention on that resource 105 a by other threads and wasted CPU consumption due to the unnecessary contention.
As another example, if thread T 1 is bound to LODM 1 and thread T 2 is bound to LDOM 2 , then the scheduler 115 will directly switch out thread T 1 and switch in thread T 2 to a particular resource in LDOM 2 (e.g., processor 220 a or 220 b ) after the scheduler 115 detects the wakeup call 140 ( FIG. 1 ) and if a time amount (e.g., stored in value 165 in FIG. 1 ) that the thread T 2 has been sleeping has exceeded a preset threshold time value 175 ( FIG. 1 ). Therefore, if no other thread can obtain a particular resource in LDOM 2 except thread T 2 , then the thread T 2 will be able to immediately use that LDOM 2 resource if the sleep time of thread T 2 has exceed the threshold time value 175 . If the sleep time of thread T 2 has not exceeded the threshold time value 175 , then the scheduler 115 will not directly switch in the thread T 2 to run on the LDOM 2 resource. If this occurs, the thread T 2 will be placed in the run queue 135 .
One reason to not switch out T 1 and switch in T 2 if they are bound to different locality domains is the associated cost of transferring thread data between the locality domains. However, if the sleep time of a thread has exceeded the threshold time value 175 , then this cost of transferring the thread data between locality domains becomes less significant because other activities in the system 100 may have likely flushed thread data from the locality domains, and as a result, the thread T 2 will have to re-populate the thread data into the cache or memory in LDOM 2 . Therefore, the comparison between the thread sleep time amount 165 and threshold time value 175 permits compliance with processor/LDOM(cell) binding of threads.
The threshold time value 175 can be set to a value of, for example, 2 ticks (cycles), but can be also be adjusted or set to other values. A factor to consider when setting the time value 175 is cache affinity (i.e., the LDOM in which a thread is assigned). For example, if thread T 2 still has some data on processor 205 a in LDOM 1 , there may be some performance degradation (as also noted above) by switching-in thread T 2 to processor 220 a in LDOM 2 .
FIG. 3 is a block diagram illustrating the contention of multiple software threads on resources. In this example, assume that thread T 1 is currently holding the lock A (mutex) and thread T 2 is waiting to obtain the lock A. The scheduler 115 determines this condition by checking the attributes 180 ( FIG. 1 ). When the thread T 1 releases the lock A, the thread T 1 sends the wake-up call 140 to thread T 2 , and the scheduler 115 will directly switch in the thread T 2 from the sleep queue 125 . The woken-up thread T 2 can then run immediately on the resource 305 that is guarded by the lock A. As mentioned above, the woken-up thread T 2 is directly switched in to run on the resource 305 and is not placed in the run queue 135 . Therefore, this direct switching into the resource of the thread T 2 advantageously avoids the run queue overhead of previous systems since the thread T 2 is not subject to the latency of waiting in the run queue, and avoids contention in the kernel by threads on a lock of the run queue 135 . The thread T 2 immediately acquires the resource (e.g., a CPU) which leads to an optimal use of CPU resources. Since the thread T 2 is not placed in a run queue, the system 100 advantageously avoids the starvation of threads that are already sitting in the run queue 135 . As known to those skilled in the art, thread starvation occurs when a thread is unable to obtain a resource that the thread is waiting to obtain.
As another example, assume that thread T 1 is currently holding the lock A and lock B. Lock A and lock B are used to guard the same resource 305 or lock B is used to guard a different resource 310 . Thread T 2 is waiting to obtain the lock A. When the thread T 1 releases the lock A, the thread T 1 sends the wake-up call 140 to thread T 2 . However, thread T 1 has not yet released the lock B which other threads (e.g., thread T 3 ) are waiting to obtain. The scheduler 115 will not directly switch in the thread T 2 from the sleep queue 125 so that the thread T 1 can continue its work on resource 310 and then give up the resource 310 to the other threads (e.g., thread T 3 ) that are waiting to obtain the resource 310 .
As another example with continuing reference to FIG. 3 , assume that thread T 1 is holding lock A and thread T 2 is holding lock B. Thread T 3 is waiting to obtain lock B and thread T 2 is waiting to obtain lock A. When thread T 1 releases lock A, thread T 1 issues the wakeup call 140 to thread T 2 and the scheduler 115 can immediately switch in the thread T 2 to obtain lock A, subject to the selection criteria set 130 that are discussed above. When thread T 2 has given up lock B, thread T 2 issues the wakeup call 320 to the thread T 3 , and the scheduler 115 can immediately switch in the thread T 3 to obtain the lock B, subject to the selection criteria set 130 that are discussed above. Therefore, in a system with multiple threads that are waiting on various resources, the direct switching into resources of the threads reduces the latency and leads to performance improvement. Based on the use of the above selection criteria 130 in the various examples above to determine whether or not to switch in a woken-up thread, there is typically seen, for example, approximately 37% performance improvement in throughput based on a given multithreaded mutex benchmark.
FIG. 4 is a flow diagram of a method 400 in accordance with an embodiment of the invention. In block 405 , the thread t 1 is running on a resource (e.g., a processor core) and thread T 2 is in a sleep state (e.g., thread T 2 is in a sleep queue).
In block 410 , thread T 1 gives up a lock on the resource and issues a wakeup call to the thread T 2 that is waiting for the resource.
In block 415 , the scheduler 115 removes the thread T 2 from the sleep queue.
In block 420 , the scheduler 115 places the thread T 1 on the run queue. Therefore, thread T 1 is switched out from the resource.
In block 425 , the scheduler 115 checks the selection criteria 130 to determine if the thread T 2 will be directly switched into the resource. Therefore, the selection criteria 130 indicate if direct switching of the thread T 2 into the resource is permissible.
In block 430 , the scheduler 115 directly switches in the thread T 2 to the resource, if the selection criteria 130 indicate that direct switching is permitted for the thread T 2 .
In block 435 , the thread T 2 starts running on the resource.
It is also within the scope of the present invention to implement a program or code that can be stored in a machine-readable or computer-readable medium to permit a computer to perform any of the inventive techniques described above, or a program or code that can be stored in an article of manufacture that includes a computer readable medium on which computer-readable instructions for carrying out embodiments of the inventive techniques are stored. Other variations and modifications of the above-described embodiments and methods are possible in light of the teaching discussed herein.
The above description of illustrated embodiments of the invention, including what is described in the Abstract, is not intended to be exhaustive or to limit the invention to the precise forms disclosed. While specific embodiments of, and examples for, the invention are described herein for illustrative purposes, various equivalent modifications are possible within the scope of the invention, as those skilled in the relevant art will recognize.
These modifications can be made to the invention in light of the above detailed description. The terms used in the following claims should not be construed to limit the invention to the specific embodiments disclosed in the specification and the claims. Rather, the scope of the invention is to be determined entirely by the following claims, which are to be construed in accordance with established doctrines of claim interpretation.
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An embodiment of the invention provides an apparatus and a method for direct switching of software threads. The apparatus and method include performing acts including: issuing a wakeup call from a first thread to a second thread in a sleep state; removing the second thread from the sleep state; switching out the first thread from the resource; switching in the second thread to the resource; and running the second thread on the resource.
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BACKGROUND OF THE INVENTION
Field of the Invention
The invention pertains to a system of digital imaging with grey scale setting, especially for the display of blood vessels.
In a digital imaging installation an image, most often an X-ray type of image, comprises points each of which has a digital value assigned to it, representing a radiation intensity. The digital value has a precision which is that of the measuring instruments. This precision is generally such that the said digital value can be represented by a binary number with 10, 11 or 12 bits.
Given that, in daytime (i.e. under the optimum conditions), the human eye is capable of distinguishing only about 1,000 different half-shades between dazzling white and absolute black provided, moreover, that these half-shades are located contiguously, a precision of 0.1% in the luminance is sufficient. But a cathode-ray tube can restore only 100 half-shades. Thus the luminance value assigned to each point during image reproduction is generally a binary number with a maximum of 8 bits (256 values possible) while the measuring instruments allow 10 to 12 bits.
In the reproduction of an image on a television screen, to benefit from all the precision of the digital image, an operation generally known as "window-making" is performed: in this operation, only brightness signal values between a minimum and a maximum are selected, the values between these limits being called a "window". The values of the digital signal which are outside the window correspond, on the one hand, to black (generally for values smaller than the lower limit) and on the other hand, to white (generally for values exceeding the upper limit of the window).
The window can usually be modified at will by the user depending on the object observed and on what he is seeking in this object. For example, to observe a human tissue by digital X-ray photography, one limit of the window corresponds to the highest absorption levels due to the bone while the other limit corresponds to the lowest absorption levels through the ambient air.
A window is defined by two parameters, most usually the width L and the mean level M. The width L of the window is the difference between the two limits while the mean level M is a value between these two limits which gives a value of grey determined on the display screen. The width L influences the contrast while the mean level M represents the luminosity of the image.
Window-arranging can be done by means of a random-access memory, called an equivalence table, receiving at its addressing input a signal representing the digital value of the radiation intensity at a point of the image and the content of the memory box which is at the corresponding address is transmitted to a television screen through a digital-analog converter. To modify the window, there is provision for computing means which modify the content of each box of the equivalence table according to the values of the two parameters which characterize the window. Hence, for each parameter, a setting means, such as a potentiometer, is associated with the computing means.
But the actuating of two commands is a constraint which users often consider to be a handicap.
SUMMARY OF THE INVENTION
The invention remedies this disadvantage.
It makes it possible, under certain conditions, to have only one control element for adjusting the window.
It results from the following observation: digital X-ray machines are most often designed for the observation of images of one and the same nature or one and the same category. For example an X-ray machine used to observe blood vessels (angiography) does not normally have any other use.
According to the invention, the two parameters defining the window are linked by a pre-determined relationship which depends on the nature of the image to be observed. Thus, it is enough to act on only one of the parameters to obtain a satisfactory setting (for the user's viewing) of the window.
BRIEF DESCRIPTION OF THE DRAWINGS
Other characteristics and advantages of the invention will appear from the description of certain of its modes of embodiment, the description being made with reference to the appended drawings wherein:
FIG. 1 is a diagram of a digital imaging installation designed for angiography,
FIG. 2 is a graph explaining the window-making operation and,
FIGS. 3a to 3e are other graphs illustrating the system according to the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
In a digital X-ray installation, the X-ray image is digitalized, i.e. the picture is divided into a certain number of points or zones, and to each of these points is assigned a digital value representing a radiation intensity, this value being most often a binary number with 10 digits. The digitalized picture is stored in an image memory 10 and the various points are read in sequence by a television-type scanning operation, i.e. at the output 11 of this memory 10, the digital values at each point appear one after the other. These values are transmitted to the addressing input 12 of a random-access memory through an interface circuit 14.
The random-access memory 13 constitutes an equivalence table which performs the window-making operation, the signals which appear at the output 15 of this memory 13, or table of equivalence of greys, being applied to a television screen 16 through an analog-digital converter 17.
The content of the memory 13 can be modified by computing means 18 with two inputs 18 1 , 18 2 for setting the parameters of the window, these computing means being connected, through an interface circuit 19, to the data inputs 20 of the memory 13 to change the content of each box of this memory. In other words, the digital value of each box of the memory 13 depends on the setting of two elements, such as potentiometers 21 1 21 2 giving signals at the outputs, 18 1 and 18 2 respectively, of the computer These signals represent the two parameters defining the grey window as shall be seen below with respect to FIG. 2.
The x-axis of the graph of FIG. 2 gives the digitalized values N in the memory 10. In the example, these values range between 0 and 1024. The y-axis gives the values G appearing at the output 15 of the memory, or table, 13. These so-called grey values are binary numbers ranging between G 0 =0 and G max =255.
The window-making done by means of the memory 13 consists in making the signal G at the output 15 follows the law of variations depicted by the straight line segments 22, 23 and 24.
The segment 22 is on the x-axis between the values 0 and N min . The segment 24 is on a straight line parallel to the x-axis of the ordinate G max between the value n max (greater than N min ) and the maximum value of N, i.e. 1024. The segment 23 links the end of the abscissa N min of the segment 22 to the end of the abscissa N max of the segment 24.
It can be seen that window-making thus consists in considering luminance levels with values below N min as black and luminances with values above N max as white. Thus only one "window" of digital luminance values is chosen in the image which is in the memory 10, and this amplifies this window on the screen of the monitor 16. A window-making operation of this type can be used, especially if the window is adjustable, to observe details which, in practice, it would not be possible to observe if the entire scale of the values of the image digitalized were to be reproduced on the screen.
It will be easily understood that a window can be defined by two parameters, for example, N min and N max , or again the width L=N max -N min and the value M of the number N which gives a mean grey level, that is (G max -G 0 )/2, i.e. G max /2 in the example. In the following part of the description, for both parameters, reference will be made only to the width L and the mean level M.
We shall now describe the invention in the context of subtractive, digital angiograhy.
Subtractive imaging consists in first making an initial image of the area of the patient to be observed (in this case, blood vessels) before injecting a contrast product, and then in making the same image after injecting the contrast product into the blood of the patient and finally, in subtracting, at each point, the digital value obtained with the contrast product from the digital value obtained without this product. It is also possible to establish the ratio between these two values.
At each point of the image, the digital value depends on the thickness crossed by the X-rays. More precisely, the attenuation increases with the length that is passed through. In the example, the number N represents this attenuation, more precisely the logarithm -- V ij of the ratio between the radiation intensity at each point of the image obtained with the contrast product and the intensity of the background (without contrast product).
A blood vessel may be likened to a cylinder. The X-rays cross this blood vessel perpendicular to the axis of the cylinder. The rays which are at a tangent to the cylinder provide no attenuation; for these rays, it is therefore possible to choose the value N=0. However, the rays which pass through the axis of the cylinder travel over a very great length and are the most attenuated; For these points, the binary number of the digitalized image is N max .
The above considerations result in the fact that the width L of the window to be used is all the greater as the blood vessel has a big diameter. Furthermore, this window has a fixed point, for example the origin on the x-axis N.
Thus, when blood vessels of various diameters (or cross-sections) are observed, it is enough to modify the width L of the window according to the diameter. In other words, a single parameter suffices to characterize the window.
FIG. 3a, which is a graph similar to that of FIG. 2, shows the segments 25 and 26 representing the window-making operation for a vessel with a relatively small diameter, while the segments 25 1 with broken lines and 25 2 with both types of lines correspond to the window-making operation for the observation of blood vessels with bigger cross-sections, the window corresponding to the segment 25 2 pertaining to vessels with bigger cross-sections than those observed by means of the window depicted by the segment 25 1 . It is seen in this FIG. 3a that, to characterize the segment 25 (or 25 1 , 25 2 ) only one parameter is enough, the width L or the value N max or again the slope of the segment 25. The mean level M is directly linked to this parameter. It suffices to act on only one of the adjusting means, for example that bearing the reference 21 1 , to modify the window.
FIG. 3a corresonds to light-coloured vessels on a black background. But it is generally preferred to obtain a complementary image, namely dark vessels on a light background. In the case of FIG. 3b, the background is white. This FIG. 3b depicts, as in FIG. 3a, segments 25', 25' 1 and 25' 2 corresponding to three windows of different widths.
If we use the method just described in relation with FIG. 3b, the background is saturated, and this might be disagreeable to the user. Furthermore, the resolution of the eye is in these conditions (saturated background) relatively poor for the observation of the blood vessels. This is why it is preferable for the background to be light grey and not white. The transformation of N into G, shown in FIG. 3c, might be adopted, i.e. the segments 27, 27 1 , 27 2 representing the window would all pass through a determined point 28 of the y-axis, the ordinate of this point 28 being lower than G max .
The studies conducted by the inventor have shown that it is possible to further improve the method of FIG. 3c, i.e. that it is possible to vary the window differently to the way shown in FIG. 3c to obtain a satisfactory visual relationship between the vessels and the light grey background. A "satisfactory visual relationship" here means sufficient contrast between the vessels and the background without loss of information by truncation, i.e. so that the small-diameter vessels remain visible.
The best result obtained by experiment is a transformation of the type shown in FIG. 3d where the segments 30, 30 1 , 30 2 etc. representing windows do not all pass through a single point as is the case with FIG. 3c. However, as was already mentioned above, the window is always defined by a single parameter, i.e. there is always a pre-determined relationship between the mean level M and the width L of the window. This pre-determined relationship, which is empirically established, is represented by the curve 31 in FIG. 3e where the width L has been shown along the x-axis and the mean level M along the y-axis. This curve 31 has a part 32 which is substantially rectilinear and a part 33, towards the greater values of L, with an upward curving shape.
The curve 31, is for example, stored in the computer 18 during the construction of the device.
With a device of this type, it is possible to provide for only one setting element 21 1 . However, the element 21 2 can be preserved to provide for a modification of the mean level M with a view to other applications.
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Digital imaging system wherein a digital value is assigned to each point or zone of the image, and this value is transformed in such a way that only a range or window of values representing luminances for a display device is selected. Control means are provided to modify the two parameters which characterize the window in the transforming device.
Since the system is designed to form images of one and the same category, for example X-rays of blood vessels, a pre-determined relationship is established between the two characteristic parameters of the window so that this window can be modified by actuating a single setting element.
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BACKGROUND OF THE INVENTION
This invention relates to a vehicle transmission control system, in particular a microprocessor-based electronic control system for a powershift transmission having solenoid valve operated transmission control elements, such as brakes and clutches, and more particularly to a calibrating method which is a method of determining key parameters relating to the operation and control of the brake or clutch elements.
Some manufacturers have used versions of electrohydraulic transmission controls with some success. Some such control systems have utilized proportionally controlled valves, but most such systems have used mostly simple on-off valves, with just one or two transmission control clutches controlled by proportional valves. For example, a powershift transmission sold by Ford New Holland, Ltd. has two modulating valves which control three different transmission control clutches. These valves are in turn controlled by an electronic controller. Such a proportional control allows a clutch element to be modulated during engagement and release of that element, and the controller provides the ability to vary the modulation for a particular element for each unique shift. Another system which includes on-off valves and at least one proportional control valve is described in U.S. Pat. No. 4,855,913, issued Aug. 8, 1989 to Brekkestran et al.
In such systems with proportional control valves it is possible and desirable to accurately control the torque capacities of the clutches during engagement. While the electrical command supplied to the control valve may be very precise, manufacturing tolerances in the valves and transmission cause large variations on an actual vehicle. If it is known what electrical command corresponds to the initial clutch engagement pressure which causes a clutch to just begin carrying torque, then this command could be used to modify the shift command for that clutch during shifting to provide optimized control.
It is also useful to determine the clutch fill time, which corresponds to volume of oil required to fill and engage a transmission control clutch. This is because manufacturing tolerances may cause variations from one transmission to the next. Also, the clutch fill time will change as a result of normal component wear as the transmission ages. If this variation can be measured, then the shift commands can be modified to compensate for such variations.
For example, the Brekkestran reference discloses that the key parameters in the control system include the initial clutch engagement pressure (represented by DC-MAX) and the fast-fill clutch delay (represented by T1). The Brekkestran reference further states that DC-MAX and T1 must be determined by laboratory or field tests. However, the Brekkestran reference does not disclose any method for determining these values.
A calibrating method or a method of determining the pressure necessary to achieve clutch engagement in a microprocessor-based transmission control system is described in U.S. Pat. No. 4,989,471, issued on Feb. 5, 1991 to Bulgrien. The Bulgrien method includes braking the transmission output shaft, then gradually increasing the clutch pressure and saving a value corresponding to the clutch pressure at which the engine speed begins to decrease. However, this method requires use of the vehicle brakes to prevent rotation of the transmission output shaft. Such a procedure could be dangerous if the vehicle brakes are not applied or if the brakes fail, because then undesired vehicle motion could result during calibration. The Bulgrien patent also illustrates an alternate method of calibrating a clutch by sensing when the clutch transmits sufficient torque to move the vehicle. This alternate method requires that the vehicle be placed in a position where vehicle motion is not a safety concern, and the results of such a method will vary depending upon the terrain on which the vehicle is placed. The Bulgrien reference does not disclose any method for determining a clutch fill time value.
U.S. Pat. No. 5,082,097, issued on Jan. 21, 1992 to Goeckner et al. relates to a transmission controller for a transmission which includes a solenoid valve operated clutch and a solenoid valve for operating the clutch. The Goeckner et al. system also discloses a calibrating system or a system for determining a current signal corresponding to the point at which the clutch begins to transmit torque. This system includes a vehicle monitor for producing a threshold signal when the clutch begins to carry a predetermined amount of torque and a memory for storing a calibration value corresponding to the value of the current at which the clutch carries the predetermined amount of torque. However, this system requires a controller which generates a controlled current signal and a current monitoring circuit which generates a signal which corresponds to the current flow to the solenoid valve. Furthermore, the threshold signal in this system is either vehicle movement or engine droop, and the calibration procedure does not appear to involve disconnecting an output shaft of the transmission from a vehicle drive shaft. As a result, the calibration procedure described in Goeckner et al. would appear to be similar to the methods described in the Bulgrien patent, and would appear to have to involve allowing vehicle movement during calibration, or applying the vehicle brakes during calibration.
SUMMARY OF THE INVENTION
An object of the present invention is to provide a method of determining key parameters for the control of proportional control valves for a powershift transmission.
Another object of the invention is to provide a such method which can be used at the time the powershift transmission is first built or installed in the vehicle and which can be used as the powershift transmission ages or is repaired.
Another object of the invention is to provide such a method which can be used without application of the vehicle brakes and without requiring that the vehicle move during operation of the method.
These and other objects are achieved by the present invention wherein a control system for a vehicle powershift transmission is calibrated. First, the transmission output shaft is disconnected from the drive wheels and the engine is run at a predetermined speed. Depending upon which transmission control element is to be calibrated, certain ones of the plurality of the control clutches, other than the control clutch being calibrated, are engaged in order to prevent rotation of a part of the control clutch being calibrated. Then the duty cycle of a pulse-width-modulated voltage signal applied to the proportional control valve is gradually modified to increase the pressure applied to the control clutch being calibrated while the engine speed is monitored. When the monitored engine speed droops by a predetermined amount, a value corresponding to the pressure applied to the proportional control valve is stored as the clutch calibration pressure value. In order to determine the fill volume of an element, the element is fully pressurized while the engine speed is monitored. The time required for this pressurization to cause a decrease in engine speed will represent the volume of fluid required to fill the element so that it begins to carry torque.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic block diagram of a microprocessor-based transmission control system to which the present invention is applicable.
FIG. 2a is a schematic representation or a transmission to which the present invention is applicable.
FIG. 2b illustrates in greater detail a portion of the transmission of FIG. 2a.
FIG. 3 is a simplified logic flow diagram of a motion detection interrupt algorithm which is performed by the method of the present invention.
FIGS. 4a and 4b are simplified logic flow diagrams of a main loop algorithm which is performed by the method of the present invention.
FIG. 4c is simplified logic flow diagram of a clutch engagement checking algorithm which is performed by the method of the present invention.
FIG. 5 is a simplified logic flow diagram of a stabilization algorithm which is performed by the main loop algorithm of the present invention.
FIGS. 6a and 6b form a simplified logic flow diagram of a pressure calibration algorithm which is performed by the main loop algorithm of the present invention
FIGS. 7a and 7b form a simplified logic flow diagram of a volume calibration algorithm which is performed by the main loop algorithm of the present invention.
DETAILED DESCRIPTION
As shown in FIG. 1, a vehicle power train includes an engine 10 which drives a power shift transmission 12, which has an output shaft 13, which, via a conventional tow disconnect mechanism 14, drives an output drive shaft 16 which is connected to drive wheels (not shown). The power shift transmission 12 includes a transmission 18 which is operated by a set of pressure operated control elements or clutches 20 which are controlled by a corresponding set of solenoid operated proportional control valves 22. The transmission 18 may be a transmission such as described in U.S. Pat. No. 5,011,465, issued Apr. 30 1991 to Jeffries et al , and assigned to the assignee of this application. The valves 22 may be two-stage electrohydraulic valves as described in U.S. Pat. No. 4,741,364, issued May 3, 1988 to Stoss et al. and assigned to applicant's assignee.
The power shift transmission control system includes a transmission control unit 30, a chassis computer 32 and a dash display 34. The transmission control unit 30 and the chassis computer 32 are preferably microprocessor-based electronic control units Manual control is achieved via a gearshift lever 36. A gearshift switches and encoder unit 38 provides signals representing the position of the lever 36 to the transmission control unit 30. A clutch engagement switch 40 and a clutch disengagement switch 42 provide signals representing the position of a clutch pedal 44. The transmission control unit 30 also receives signals from a ground speed sensor 48. The chassis computer 32 also receives signals from an engine speed sensor 46 and a transmission oil temperature sensor 50. The chassis computer sends information from these sensors to the transmission control unit 30.
The transmission control unit 30 includes a commercially available microprocessor (not shown) which, in response to an operator generated signal, executes a computer program which implements operation of the calibration methods described hereinafter. The transmission control unit 30 also includes valve drivers (not shown) which provide variable duty cycle pulse-width-modulated voltage control signals to the valves 22. The transmission control unit 30 and the valve drivers (not shown) will generate such control signals as a function of various sensed and operator determined inputs in order to achieve a desired pressure in the clutches and to thereby control the shifting of the transmission 12 in a desired manner. However, the present invention is not concerned with the control of the shifting of the transmission 12, the transmission 12 itself, or the valves 22, since the present invention is concerned only with the calibration of certain parameters. The method of the present invention is implemented by the control unit 30 which executes the computer program which is listed in the microfiche appendix. The computer program listing is in (Motorola 68HC11) assembly language.
Referring to FIG. 2a and 2b, the control elements of transmission 12 include a set of brake elements B1, B2, B3, B4 and B5, and a set of clutch elements C1, C2, C3, and CLO. The input shaft 52 is connected by splines 54 to the clutch drum 56 of clutch C1 and of clutch C2 (not shown in FIG. 2b). The drum 56 in turn is splined to the clutch separators 58 of clutch C1. The clutch disks 60 of clutch C1 are splined to the clutch hub 62 of clutch Cl. The clutch hub 62 is splined to a first intermediate shaft 64. The first clutch C1 is provided with a piston 66 for activating the clutch C1 by compressing the clutch separators and disks 58, 60. A spring 68 is provided to bias clutch C1 out of engagement. For further information regarding the details of such a transmission reference is made to U.S. Pat. No. 5,011,465, which is incorporated by reference herein.
The clutch piston 66, as well as the pressure operated elements of the other clutches and brakes, are each provided with hydraulic fluid from a pump (not shown) under the control of a corresponding one of the valves 22, in the usual fashion which is well-known to one of ordinary skill in the art, and therefore will not be described further herein.
Calibration Method
The following calibration method will determine the valve pressure command signal Pfill(el) required to just engage each clutch or brake element, and it will determine the fill volume times twake(el) required to nearly fill the corresponding clutch and brake elements
Before the automatic calibration procedure of the control unit 30 is enabled, the operator should disengage the tow disconnect device 14 so that the transmission output shaft 13 is free to rotate, the shift lever 36 must be in neutral, the oil temperature must be above a threshold, and the engine speed must be set to a certain level (within a range).
Referring to FIG. 3, the control unit 30 continuously performs a motion detection interrupt algorithm 300 which is in the background while other functions are being performed. This algorithm 300 monitors the signal from speed sensor 48 to detect motion of the vehicle. If vehicle motion is detected, any other functions are interrupted and the transmission 18 is automatically shifted to neutral to prevent further vehicle motion.
Main Calibration Loop
In the main calibration loop 400 (FIGS. 4a and 4b) the control unit 30 performs the following calibration procedure. First, step 401 checks to make sure the shift lever 36 is in neutral before starting the calibration procedure. If the shift lever 36 is not in neutral, step 403 displays a message or symbol on the display 34 until the shift lever 36 is in neutral. If the shift lever 36 is in neutral, the calibration procedure continues to step 402. This is important because it prevents unexpected motion if the operator if the calibration procedure is activated by mistake with the shift lever in gear. Without this step, if the oil is warm and the lever 36 is in Forward and the engine speed is 2100 rpm, first gear will be engaged every time calibration procedure is selected.
Step 402 monitors the oil temperature signal from sensor 50 and, if the oil temperature is less than Tcal, step 405 displays a message or symbol on the display 34 until the oil temperature is greater than or equal to Tcal. If the oil temperature is greater than or equal to a threshold temperature "TcalOil", the calibration procedure continues to step 404.
Step 404 checks if the shift lever 36 is placed in a forward gear position by monitoring the condition of "Forward" and "Not Neutral" lever position switches (not shown), and if not, then step 407 a message or symbol on the display 34 to prompt the operator to place the shift lever 36 in a forward position until lever 36 is placed in a forward position.
Next, step 406 monitors the engine speed signal from sensor 46 and, if the engine speed is outside of the desired range, step 408 displays a message or symbol on the display 34 until the engine speed is within the desired range. If the engine speed is within the desired range, the calibration procedure continues to step 410.
For each element to be calibrated, step 410 applies full pressure to a certain set of the clutch and/or brake elements in order to create an internal fight between the different parts of the element to be calibrated when that element is pressurized, in other words, to cause relative rotation between the different parts of the element to be calibrated. For example, with respect to clutch C1 and referring to FIG. 2b, the clutch drum 56 will be rotating with the input shaft 52. When brakes B1 and B2 are pressurized, this prevents rotation of hub 62 so that there is relative rotation between parts 56 and 62 of clutch C1.
The following table sets forth one possible order in which the elements are to be calibrated, and for each element being calibrated, the set of the other elements which are fully pressurized to create the appropriate internal fight, it being understood that other orders are possible and that other combinations of elements can be pressurized to create the desired internal fight. This table applies to the particular transmission described in U.S. Pat. No. 5,011,465. However, one skilled in the art would be able to determine similar combinations of elements for other powershift transmissions.
______________________________________Calibration TableElement to be Elements to beCalibrated Fully Pressurized______________________________________Tow Test C1, B1 and C3C2 B1, B2B2 C1, C2, CLO, B5C3 C2, B2, B3B3 C1, C2, CLO, B5C1 B1, B2B1 C1, C2, CLO, B5B5 C2, B2, B3B4 C2, B2, B3______________________________________
Next, step 500 calls a "Stabiliz" subprocedure shown in FIG. 5. This subprocedure (steps 504-520) pauses for a length of time sufficient for the hydraulic system and the engine to stabilize before proceeding. A check is made (step 508) to determine that the lever 36 remains in the forward position. If not, an error message is displayed (step 506) until the lever 36 is placed in a forward position.
After the prescribed time has elapsed, the engine speed is checked (step 512) to make sure it is within tolerance for the procedure. If not, a message is displayed (step 514) to indicate that the calibration method is waiting for the system to stabilize. If the engine speed becomes correct (step 516), control returns to the beginning of this "Stabiliz" subprocedure (step 504). When step 512 determines that the engine speed is within the proper speed range then step 518 checks to see if the clutch pedal is engaged. If not, a message is displayed by step 520, the algorithm returns to the main loop 400 and the calibration procedure is aborted without executing the Calibrate subprocedure 600. If the clutch pedal is engaged, then step 518 causes a return to step 600 of the main loop 400. It should be noted that if the clutch is not engaged when tested in step 518, the algorithm not only returns to the main loop 400, but the algorithm also does not execute step 600 (or 700) before aborting.
Fill Pressure Calibration
The "Press. Cal" subprocedure 600 for fill pressure calibration is performed to determine the calibration pressure "Pfill(el)" value for each transmission control element. If an element cannot be calibrated for any reason, the previously stored Pfill(el) for that element shall not be altered. Also, if Pfill(el) is determined for an element during the calibration and then the calibration procedure crashes later for some other element, the elements which were calibrated correctly shall retain their correct values for Pfill(el).
Referring now to FIGS. 6a-6b, step 602 of this subprocedure displays a message or symbol to indicate which element is being calibrated. As shown in the preceding table, at the beginning of the automatic calibration procedure elements C1, B1 and C3 are automatically fully pressurized (engaging gear 1F). If the tow disconnect device 14 is engaged this will cause the motion detect algorithm 300 to detect vehicle motion, whereupon the calibration method is interrupted and the transmission 12 is automatically shifted to neutral. This operates as a check on whether or not the tow disconnect device 14 is disengaged.
If the tow disconnect device 14 is disengaged, no motion will be detected whereupon the system exits procedure 600, returns to the main calibration loop at step 410 and automatically determines the pressure command required to just engage each clutch or brake by continued execution of the main calibration loop. In step 604 the engine speed from sensor 46 is read and stored. Next, for the element being calibrated, a low starting pressure Pstrt(el) which corresponds to that element is commanded by step 606. If the element is C1 or C2, this Pstrt(el) is modified or reduced by an amount which depends upon the engine speed in order to compensate for centrifugal head which is the pressure created by the spinning of the element itself (compensating for pressure generated centrifugally in a rotating hydraulic cylinder is known from U.S. Pat. No. 4,718,306, issued Jan. 12, 1988 to Shigematsu et al.). These adjustment pressures are illustrated in the following table and are stored in a "lookup" table in the memory of the control unit 30. Table locations are in increments of 128 revolutions per minute beginning with the first table location. For engine speeds above 2176 revolutions per minute, the controller shall use 0 kPa as the compensation value.
______________________________________Centrifugal Head Compensation TableEngine Speed Compensation Value(r/min) (kPa)______________________________________ 640 133 768 127 896 1201024 1131152 1071280 1001408 931536 801664 671792 601920 472048 332176 13______________________________________
This starting pressure is held while steps 608 and 610 operate to compare the droop to a threshold value NeFull for a time 532. If the engine droop speed (or engine speed reduction) does not exceed the threshold NeFull, then control passes to the step 612. If the droop does exceed the threshold, then steps 624-632 operate to display a certain character and turn off or depressurize all elements. Step 628 prevents further operation until switch 40 is toggled (off then on). Then, once switch 40 has detected that the clutch pedal 44 is depressed and released, step 630 causes the controller to leave the current element without storing a Pfill(el) value and to set up for calibrating the next element.
Next, in step 612 the pressure command applied to the element being calibrated is increased by an increment "Pinc". If in step 614 the new pressure command is greater than Plimit(el) for the corresponding element, then in steps 634-640 a certain character is displayed (step 634) and all elements are turned off (step 635). Step 636 prevents further operation until Clutch Engaged switch 40 is toggled, then step 638 causes the controller to leave the current element without storing a fill pressure and set up to calibrate the next element. If in step 614 the new pressure does not exceed Plimit(el), then control proceeds to step 616.
Then, in step 616 the engine droop is again calculated and compared to the threshold NeFull and the increased pressure command is held for time t33 by step 618.
If the droop is greater than or equal to NeFull, then the element is considered to be "full" and the currently commanded pressure (minus any centrifugal head compensation pressure, if applicable) is the fill pressure Pfill(el). This Pfill(el) value is stored in step 642 and the drivers for all elements are turned off by step 644. Then step 646 delays for a period of time, step 648 sets up for the next element and step 650 causes a return to the main loop.
If in step 616 the droop is less than NeFull, then control is returned to step 612 and the algorithm continues in this manner until the droop has reached threshold NeFull in step 616 or until the pressure command has exceeded a predetermined limit for that element (Plimit(el)) in step 614, whereupon control is returned to step 412 of the main loop.
Returning now to FIGS. 4a and 4b, step 412 returns the algorithm to s 402 if either of the stabilization or the calibration procedures is aborted because the lever 36 was in neutral or because the clutch pedal 44 was depressed. Steps 410, 500 600 and 412 are repeated until step 414 determines that the last element has been calibrated, whereupon the algorithm proceeds to step 416 which prepares for start of fill volume calibration, then to step 418 which applies partial pressure to the element set for the element to be calibrated. Then the Stabiliz subroutine 500 is executed and then a fill volume calibration procedure 700 is performed. Step 424 returns the algorithm to step 416 if the calibration procedure is aborted, otherwise the algorithm proceeds to step 426. Steps 418, 500, 700 and 424 are repeated until step 426 determines that the last element has been calibrated, whereupon the algorithm is exited.
The values determined by this calibration procedure are also preferably adjusted to compensate for variations in oil temperature, battery voltage, etc.
With this system and method, all transmission brake and/or clutch elements may be calibrated in turn without any further input from the operator. This virtually eliminates any chance of operator induced error (such as not calibrating one or more elements) in the procedure.
Because the tow disconnect device 14 is disengaged and internal fights between transmission elements are used to determine when engagement occurs, the output shaft 13 is not restrained from rotation and no vehicle motion can occur. Therefore, with this calibration method it is not necessary to rely on the vehicle brakes to prevent dangerous vehicle movement. As an additional safety feature, this calibration routine also continually checks for vehicle motion (by monitoring the output of ground speed sensor 48), and stops the process and places the transmission 18 in neutral (all valves 22 off) if motion is sensed. In particular, a forward gear of the transmission is engaged during the initial stages of the calibration method so that if the tow disconnect device 14 is not disengaged, the vehicle will move only a very short distance before the transmission 18 is automatically shifted to neutral.
It should be noted that, during steps 600 and 700, the controller continually monitors the clutch pedal 44 to make sure it remains fully engaged during calibration. If during calibration the clutch pedal 44 is not engaged", the controller exits the routine and aborts the calibration procedure as shown in steps 412 and 424.
It should be noted that in subprocedure 600, this clutch pedal check is active until execution reaches step 624 or 634. After that, the clutch pedal is required for acknowledging the fault so that operation can continue to the next element to be calibrated. In subprocedure 700, the clutch pedal 44 is similarly checked until step 718 or 732, and may even be checked until step 752. In other words, the check is required during the actual calibration of the element. This checking procedure is illustrated by the flow chart of FIG. 4c.
Fill Volume Calibration
The "Vol. Cal." subprocedure 700 for fill volume calibration is performed to determine the fill volume calibration value for each transmission control element. The fill volume calibration method is similar to the fill pressure calibration method. Each element will be calibrated individually, and preferably in the same order as in the fill pressure calibration method. As before, the tow disconnect device 14 must be disengaged to prevent unexpected motion, and any vehicle movement during the calibration cycle will cause the transmission 18 to be automatically placed in neutral. This calibration cycle is automatically entered upon completion of the fill pressure calibration procedure. Again, the cycle proceeds without the need for any operator input.
Each individual element is fill volume calibrated by engaging the same combination of elements for the element being calibrated as used in fill pressure calibration method. However, all of these elements will only be partially pressurized.
Referring now to FIGS. 7a-7b, step 702 of this subprocedure displays a message or symbol to indicate which element is being calibrated. The procedure begins with element C2 of the Calibration Table. Then, the system proceeds to step 704 where the engine speed from sensor 46 is read and stored. Next, in step 706, for the element being calibrated, a "wakeup" pulse is applied to the element being calibrated. This means that the element will be commanded to full system pressure for an initial time period. This time period is variable, depending upon which element is being calibrated. Steps 708-710 operate to calculate the engine speed droop and compare the droop to a threshold value Ne2Ful during the time the wakeup pulse is applied.
If the wakeup pulse terminates and the droop has not exceeded the threshold NeFull, then control passes to the step 712. If the droop does exceed the threshold, then steps 718-726 operate to display a certain character and turn off or depressurize all elements. Step 722 prevents further operation until switch 40 is toggled (off then on). Then, once switch 40 has detected that the clutch pedal 44 has been depressed and is now released, step 724 causes the controller to leave the current element without storing a volume calibration value twake(el) and to set up for calibrating the next element.
In step 712 the wakeup pulse is terminated and steps 714-716 operate to calculate the engine speed droop and compare the droop to a threshold value Ne2Ful during a time t35 after the start of the wakeup pulse is applied. If the droop does exceed the threshold, then step 714 directs control to previously described steps 71814 726. If the droop does not exceed the threshold, then at the end of time t35 step 716 directs control to step 728.
Step 728 increases the duration of the wakeup pulse by one time interval. If in step 730 the new duration is greater than tlimit(el) for the corresponding element, then in steps 732 -733 a message is added to the display in the right-most display digit and all elements are turned off. Step 734 prevents further operation until Clutch Engaged switch 40 is toggled, then step 736 causes the controller to leave the current element without storing a fill volume value and set up to calibrate the next element. If in step 730 the new duration does not exceed tlimit(el), then control proceeds to step 740.
Steps 742-744 operate to calculate the engine speed droop and compare the droop to the threshold value Ne2Ful during the new duration of the wakeup pulse. If the droop does exceed the threshold, then the element is considered to be "full" and step 742 directs control to step 752-760. Step 752 stores the last wakeup pulse time twake(el) as the volume calibration value and all drivers are turned off by step 754. Step 756 delays for a time period, step 758 sets up for the next element and step 760 causes a return to the main loop. If the droop does not exceed the threshold, then at the end of the new duration of the wakeup pulse step 744 directs control to step 746 which turns off the wakeup pulse at the end of the new duration.
Then steps 748-750 operate to calculate the engine speed droop and compare the droop to a threshold value Ne2Ful during a time t35 after the start of the new wakeup pulse. If the droop does exceed the threshold, then step 748 directs control to previously described steps 752-760. If the droop does not exceed the threshold, then at the end of time t35 step 750 directs control to back to step 728.
A portion of the disclosure of this patent document contains material which is subject to a claim of copyright protection. The copyright owner has no objection to the facsimile reproduction by anyone of the patent document or the patent disclosure, as it appears in the Patent and Trademark Office patent file or records, but otherwise reserves all other rights whatsoever.
While the invention has been described in conjunction with a specific embodiment, it is to be understood that many alternatives, modifications and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, this invention is intended to embrace all such alternatives, modifications and variations which fall within the spirit and scope of the appended claims.
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The hydraulically operated brake and clutch elements (controlled by proportional control valves) of a vehicle powershift transmission have fill pressures which are calibrated by a method wherein the output shaft of the transmission is disconnected from the vehicle drive shaft so that the transmission output shaft is free to rotate and certain ones of the plurality of the control elements other than the control element being calibrated are fully pressurized in order to prevent rotation of a part of the control element being calibrated. The engine is run at a predetermined speed and the pressure applied to the control element being calibrated is gradually increased while engine speed is monitored. When the monitored engine speed changes by predetermined amount, a value is saved corresponding to the calibration pressure. The transmission is automatically shifted to neutral if vehicle motion is sensed. The volume of hydraulic fluid required to initially engage the control element may be calibrated in a similar manner.
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INCORPORATION BY REFERENCE
Applicants incorporate by reference the teaching and technology as disclosed in pending application Ser. No. 11/702,381, filed Feb. 6, 2007
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to Liquified Petroleum Gas (LPG) fueled internal combustion engine powered arrangements and, more particularly, to such arrangements in which the internal combustion engine is powered by the gas phase of the LPG at all times and may be as utilized in lawnmowers, weed whackers, leaf blowers, string trimmers and the like
2. Description of the Prior Art
Utilization of LPG as a fuel for internal combustion engines has been heretofore been known for use in large internal combustion engine powered arrangements such as forklifts, trucks, buses and other such arrangements and devices. As such, the tank capacity of the LPG is quite large: on the order of 5 gallons or larger and in which the LPG is withdrawn from the LPG tank in liquid phase form and this requires that the LPG tanks be mounted in a particular orientation so that only liquid phase LPG is withdrawn therefrom during operation of the internal combustion engine 12 . Further, the LPG tank is, generally, mounted in regions remote from the engine or any normally occurring heat source during operation and/or storage of the device.
During operation of such devices, the liquid phase LPG travels through transfer lines to either a vaporizer or a vaporizer/regulator structure. The vaporizer or vaporizer/regulator causes the liquid phase LPG to be converted to the gas phase LPG. The latent heat of vaporization of the liquid phase LPG as it is converted to the gas phase LPG would cause the vaporizer or vaporizer/regulator to get extremely cold and in many applications would freeze the liquid phase LPG to a solid phase and thus stop the flow of LPG to the engine unless means are provided to heat the vaporizer or vaporizer/regulator. Various structural arrangements have heretofore been utilized to supply heat to the vaporizer or vaporizer/regulator. In liquid cooled internal combustion engines the hot engine coolant was often routed to pas through or adjacent to the vaporizer or vaporizer/regulator in order to transfer heat thereto. In air cooled internal combustion engines some or all of the hot exhaust products may be forced over the vaporizer or vaporizer/regulator by the engine cooling fan. In other prior art applications, the LPG transfer lines may be placed in close proximity to the exhaust manifold or the vaporizer or vaporizer/regulator may be close coupled to the exhaust manifold for receiving heat therefrom.
In yet other prior art devices, an electrically powered heater was provided at the vaporizer or vaporizer/regulator.
Thus, such prior art applications and devices utilizing the large tanks of LPG often required many complex structural arrangements and components in order to insure that the liquid phase LPG was converted to the gas phase LPG.
In many other applications, the use of a large, e.g., 5 gallon LPG tank and its attendant complexity is not needed or desired. For example, in many smaller internal combustion engine powered devices, it is often desired to utilize a small LPG tank such as one containing one or two pounds of LPG. Such devices include, but are not limited to lawnmowers, leaf blowers, string trimmers, or the like. The one or two pond LPG tanks are readily available as such LPG tanks are widely utilized in the camping industry to provide LPG for portable for stoves, lamps and the like. However, in such applications, the LPG tank is oriented to provide that only the gas phase LPG exits the LPG tank and, therefore, the freezing of the LPG would occur in the LPG tank rather than external the LPG tank. Depending on the rate of flow of the gas phase LPG from the LPG tank, the freezing of the LPG occurs in the LPG tank.
However, in many applications it is desired that the mounting of the LPG tank be such that no specific orientation of the LPG tank is required for the internal combustion engine to operate on the gas phase of the LPG.
Accordingly, there has long been a need in an It is another object of the present invention provide an LPG fueled internal combustion engine apparatus utilizing propane as the LPG from a conventional one to two pound LPG propane tank for the supply of the LPG and which does not require a particular orientation of the LPG tank with respect to gravity for satisfactory operation.
Additionally, many of the prior art LPG fueled internal combustion engine powered devices have utilized butane as the LPG. Such devices are common in many foreign countries such as Japan and Korea. In the United States and in Europe, on the other hand, propane LPG tanks are quite readily available. The physical properties of propane as compared to butane makes the propane LPG tanks more attractive as a fuel for the small internal combustion engine applications. For example, for an equivalent amount of LPG, a butane fueled device would run for about one half hour while for a propane fueled device would run for about three to four hours. Also, the butane LPG tanks that are readily available in Japan and Korea provide for only gas phase butane to be withdrawn from the bottle and are provided with an internal tube to insure that only gas is withdraw and thus require a preferred orientation with respect to gravity. Since liquid phase butane becomes a gas phase butane at about 31 degrees F. which is only about 39 degrees F. different from the conventionally stated standard operating temperature of a nominal 70 degrees F., there is little cooling effect due to the evaporation and freezing in the LPG tank or in the system is not likely by utilization in a small internal combustion engine. Liquid phase propane, on the other hand, becomes gas phase propane at about minus 44 degrees F. which is about 114 degrees F. different from the conventionally stated standard operating temperature of a nominal 70 degrees F. Therefore, the propane would freeze to the solid phase in the LPG tank or elsewhere in the delivery system long before the LPG tank is empty depending on the consumption rate and the temperature. As contrasted to butane, the propane requires structure to prevent freezing to the solid phase.
Therefore, it is an object of the present invention to provide an LPG fueled internal combustion engine apparatus utilizing propane as the LPG.
It is another object of the present invention to utilize a conventional one to two pound LPG propane tank for the supply of the LPG.
It is another object of the present invention provide an LPG fueled internal combustion engine apparatus utilizing propane as the LPG and in which the propane is provided from a conventional one to two pound LPG propane tank for the supply of the LPG.
It is another object of the present invention provide an LPG fueled internal combustion engine apparatus utilizing propane as the LPG from a conventional one to two pound LPG propane tank for the supply of the LPG and which does not require a particular orientation of the LPG tank with respect to gravity for satisfactory operation.
It is another object of the present invention provide an LPG fueled internal combustion engine apparatus utilizing propane as the LPG from a conventional one to two pound LPG propane tank for the supply of the LPG which does not require a particular orientation of the LPG tank with respect to gravity for satisfactory operation and in which the possibility of freezing of the liquid phase LPG to the solid phase LPG is substantially prevented in both the LPG tank and in the gas phase supply system to the internal combustion engine.
It is yet another object of the present invention to provide an LPG fueled internal combustion engine apparatus utilizing propane as the LPG from a conventional one to two pound LPG propane tank for the supply of the LPG which does not require a particular orientation of the LPG tank with respect to gravity for satisfactory operation and which insures that only gas phase LPG propane is withdrawn from the LPG tank regardless of the orientation thereof during operation.
SUMMARY OF THE INVENTION
The above and other objects of the present invention are achieved, in a preferred embodiment thereof as utilized in a LPG gas phase fueled internal combustion engine lawnmower. This embodiment has an LPG tank containing propane which has both a liquid phase LPG and a gas phase LPG therein mounted in a vertical orientation with respect to gravity so that liquid phase LPG is at the discharge valve of the LPG tank for the conventional operation of the lawnmower on a relatively flat surface though operation will also satisfactorily occur for any other orientation of the lawnmower such as, for example, on a sloping surface of lawn even though the gas phase LPG may be at the discharge valve.
The LPG tank is mounted by a mounting bracket on the internal combustion engine so as to be in both heat transfer relationship to a portion of the internal combustion engine from which the mounting bracket receives heat as well as in vibration receiving relationship to the internal combustion engine. The heat and vibration from the mounting bracket is transferred to the LPG tank and thus into the LPG in the LPG tank. The mounting bracket is also coupled to the discharge valve of the LPG tank so as to provide heating to the discharge valve.
The discharge valve of the LPG tanks utilized in the present invention has a spring biased poppet that is moved from a spring biased closed position to an open position when coupled to a standard mounting plug. The standard mounting plug has a probe that unseats the poppet when the mounting plug is attached to the discharge valve. As liquid phase propane starts to flow from the LPG tank under the force produced by the gas pressure in the LPG tank, the small size of the orifice at the poppet causes the liquid phase to vaporize into the gas phase. Since, depending on the flow rate of the liquid phase LPG through the poppet orifice, the latent heat of vaporization might cause the discharge vale to become so cold as to freeze the liquid phase LPG into the solid phase LPG, heat is supplied to the mounting plug at the discharge valve so as to heat the discharge valve and thus prevent freezing of the LPG. Such heating of the discharge valve may be provided by coupling a portion of the mounting bracket to the mounting plug.
The supply of gas phase LPG is passed from the mounting plug through a shutoff valve, through a pressure regulator and into the carburetor of the internal combustion engine. The carburetor is preferably a chokeless carburetor of conventional design and may, if desired, be incorporated as a single unit with the pressure regulator. The vacuum generated in the carburetor by the operation of the internal combustion engine draws the gas phase LPG into the carburetor. At substantially zero vacuum, no liquid phase LPG is drawn into the carburetor. Gas phase LPG is drawn into the carburetor commensurate only with the vacuum thereby providing that the gas phase LPG flow rate is at the rate demanded by the internal combustion engine.
Thus, according to the principles of the present invention regardless of whether the liquid phase of the LPG or the gas phase of the LPG is at the discharge port, satisfactory operation of the apparatus is insured.
In another embodiment of the present invention achieving the objects as stated above, the LPG tank may be mounted on an LPG fueled internal combustion engine driven leaf blower or a string trimmer. As such, in operation the leaf blower or string trimmer and, consequently, the LPG tank, may be in any orientation with respect to gravity. For the technological advances as described above, satisfactory operation is achieved by having only gas phase propane LPG flow from the LPG tank into fuel supply system to the internal combustion engine.
BRIEF DESCRIPTION OF THE DRAWING
The above and other embodiments of the present invention my be more fully understood from the following detailed description taken together with the accompanying drawing wherein similar reference characters refer to similar elements throughout and in which:
FIG. 1 is an exploded view of a preferred embodiment of the present invention as utilized in an LPG fueled internal combustion engine powered lawn mower;
FIG. 2 is a sectional view showing the attachment of the LPG tank to the internal combustion engine in the embodiment illustrated in FIG. 1 ;
FIG. 2A is a block diagram illustrating the flow path of the fuel supply system of the present invention;
FIG. 3 illustrates another embodiment of the present invention as utilized in a string trimmer, leaf blower or the like; and
FIG. 4 is an exploded view of the attachment of the LPG tank to the embodiment illustrated in FIG. 3 .
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawing, there is shown on FIGS. 1 and 2 an embodiment, generally designated 10 , of an LPG fueled internal combustion engine apparatus utilizing the gas phase of propane as the LPG from a conventional one to two pound LPG propane tank for the supply of the gas phase LPG and which does not require a particular orientation of the LPG tank with respect to gravity for satisfactory operation. In embodiment 10 , an internal combustion engine 12 is incorporated on a powered lawnmower 14 . An LPG tank 16 is provided in a vertical orientation mounting position with respect to both gravity as indicted by the arrow 11 and the lawnmower 14 in the most common orientation of the lawnmower 14 during use which is generally horizontal. The LPG tank 16 contains a liquified petroleum gas 18 such as, preferably, propane, though the LPG propane may include a mixture of propane with small amounts of additives such as butane, propylene or other desired additives The LPG 18 in the tank 16 does not fill the tank completely so that there is both a liquid phase 20 and gas phase 22 of the LPG 18 in the tank 16 . According to the principles of the present invention, the LPG utilized to fuel the internal combustion engine 12 is provided from the liquid phase 20 of the LPG which is vaporized to the gas phase at the discharge of the LPG tank and thus prior to introduction to the internal combustion engine 12 .
A tank support bracket 24 is utilized for supporting the LPG tank 16 on the internal combustion engine 12 . In the embodiment 10 , the bracket 24 is mounted on the cylinder head 26 by head bolts 28 . The tank support bracket 24 preferably incorporates a quick release, such as an over center clamp for coupling the LPG tank 16 to the tank support bracket 24 , though other types of coupling arrangements such as an elastic band, a snap on latch, or even a hook and loop band or the like may be utilized as desired for particular applications. The tank support bracket 24 is fixed to the cylinder head 26 of the internal combustion engine 12 by, for example, cylinder head bolts 30 .
The tank support bracket 24 is, in preferred embodiments of the present invention, closely coupled to a part of the internal combustion engine 12 so that it receives both vibration and heat from the internal combustion engine 12 during operation of the internal combustion engine 12 . The vibration transferred from the internal combustion engine 12 to the tank support bracket 24 and thus to the LPG tank 16 and the LPG 18 provides agitation to the LPG 18 so as to aid in keeping the LPG 18 from freezing as the temperature thereof drops during the withdrawal of the LPG 18 therefrom, as described below in greater detail. Further, such agitation of the LPG 18 increases the surface area 34 of the LPG 18 in the tank 16 thereby causing an increase in the gas phase 22 of the LPG in the tank 16 .
As shown more clearly in FIG. 2 , in the conventional one to two pound propane LPG tanks utilized in the present invention is provided with a discharge valve 32 . The discharge valve 32 has a spring biased poppet 34 normally biased into the closed position by spring 36 . The discharge valve 32 is threaded into a mounting plug 38 having a probe 40 that unseats the poppet 34 against the bias of the spring 36 to allow the start of the flow of liquid phase LPG therethrough. However, the flow orifice 42 around the poppet is so small that the liquid phase propane 20 is vaporized into the gas phase propane 22 a at the discharge valve 32 as it flows through the mounting plug 38 . The probe 40 of the mounting plug 38 has walls defining a gas flow passage 40 ′ therethrough.
A clamping nut 44 having walls 46 defining a gas storage volume 48 therein is provided and the gas volume 48 is in gas flow communication with the gas flow passage 40 ′ and contains the gas phase propane 22 a until gas phase propane is required by the internal combustion engine 12 . The clamping nut 44 threadingly engages the mounting plug 38 at 44 a and clamps a heating portion 24 a of the mounting bracket 24 between the clamping nut 44 and the mounting plug 38 . The heating portion 24 a of the mounting bracket 24 heats the mounting plug 38 , the discharge valve 32 and the clamping nut 44 to prevent any freezing of the gas phase propane flowing through the orifice 42 of the discharge valve. An “O” ring 50 may be provided between the clamping nut 44 and the mounting plug 38 .
The gas phase propane 22 a flows through a connector assembly 52 as indicated by the arrow 54 .
A tank heating portion 24 b of the mounting bracket 24 is in heat and vibration transfer relationship to the LPG tank 16 to heat and agitate the liquid phase LPG therein.
FIG. 2A illustrates a block diagram the flow path of the fuel system according to the principles of the present invention. As shown on FIG. 2A , the gas phase propane 22 a flows from the storage volume 48 into a gas phase transmitting tube 61 , through a shutoff valve 60 and for the shutoff valve in the open position thereof, into a gas phase transmitting tube 61 , through a pressure regulator 62 and into a chokeless carburetor 64 for transmission to the internal combustion engine 12 as indicated by the arrows 54 a , 54 b , and 54 c . The shutoff valve 60 , pressure regulator 62 and chokeless carburetor 64 may be of any desired commercially available gas phase design suitable for the purpose. When the shutoff valve 60 is opened, gas phase propane 22 a from the storage volume 48 of the clamping nut 44 is allowed to flow to the internal combustion engine 12 in the amount as demanded by the vacuum created by the internal combustion engine 12 .
Referring now to FIGS. 3 and 4 there is illustrated another preferred embodiment generally designated 100 of an LPG fueled internal combustion engine apparatus utilizing gas phase propane as the LPG from a conventional one to two pound LPG propane tank for the supply of the gas phase LPG and which does not require a particular orientation of the LPG tank with respect to gravity for satisfactory operation. The embodiment 100 is shown as incorporated in a weed whacker, string trimmer, leaf blower or the like. The power units of such devices are often strapped onto the back of the user and in use the user may bend to various degrees so that the orientation of the LPG tank may vary during operation with respect to the direction of gravity.
As shown on FIGS. 3 and 4 , many of the components described above in connection with embodiment 10 may be utilized in embodiment 100 . the LPG tank 16 is connected to the internal combustion engine 12 by the mounting bracket 24 ′ which is generally similar to the mounting bracket 24 of embodiment 10 described above. the mounting bracket 24 ′ is provided with a retaining strap 28 for securing the LPG tank 16 to the mounting bracket 24 ′. In embodiment 100 the mounting bracket 24 ′ is coupled to the crankcase 70 of the internal combustion engine 12 . The crankcase 70 is another portion of the internal combustion engine 12 which is heated during operation and thus heat and vibration are transferred from the crankcase 70 to the mounting bracket 24 ′ and thus to the LPG tank 16 by the portion 24 b ′ and to the discharge valve 32 by the portion 24 a ′ to prevent conversion of the gas phase of the LPG flowing through the discharge valve 32 to the solid phase.
The mounting bracket 24 ′ is retained against or in close proximity to the crankcase 70 to provide the heat transfer and vibration transfer thereto by bolts 72 and 74 . The gas phase propane from the LPG tank 16 through the shutoff valve 60 to the pressure regulator 62 as indicated by arrow 54 a , from the pressure regulator 62 to the carburetor 64 as indicated by the arrow 54 b . The gas phase propane is mixed with air flowing into the air filter 78 and to the cylinder of the internal combustion engine 12 .
In FIGS. 3 and 4 , the cylinder 26 ′ of the internal combustion engine 12 may be aligned vertically with respect to the direction of gravity 11 and the LPG tank mounted horizontally or at right angles to the cylinder 26 ′. This relationship between the cylinder 26 ′ and the LPG tank 16 is maintained regardless of the orientation of the embodiment 100 with respect to the direction of gravity 11 as the user (not shown) may bend or twist during use. Thus, it is possible for either liquid or gas phase propane to be at the discharge valve 32 . However, in accordance with the principles of the present invention, it makes no difference since there is heat transfer and vibration transfer to the contents of the LPG tank 16 as well as to the discharge valve 32 . Therefore, regardless of whether the liquid phase LPG tends to freeze in the tank 16 or at the discharge valve 32 the heat and vibration transferred is sufficient to provide that there is gas phase propane flowing into the shutoff valve 60 .
If the liquid level of the liquid propane in the LPG tank 16 is below the discharge valve 32 gas phase propane will flow therefrom to the shutoff valve 60 . If the liquid level of the liquid phase propane in the LPG tank 16 is above the discharge valve 32 , it is converted to the gas phase propane as described above. No matter where the freezing of the propane to the solid phase might occur, the heat transfer and vibration transfer prevents such freezing regardless of the flow rate of the propane.
A recoil starter of conventional design as indicated at 80 may be incorporated on the internal combustion engine 12 in the embodiment 100 and, if desired a similar recoil starter may be incorporated in the embodiment 10 .
From the above it can be seen that there has been provided an improved gas phase fueled internal combustion engine adapted to power various types of devices. and in which only gas phase LPG flows from the LPG tank regardless of the orientation of the LPG tank with respect to gravity and regardless of whether liquid phase propane or gas phase propane is present at the discharge of the LPG tank. Such arrangements eliminate the need for costly and complex heating devices downstream from the LPG tank to convert the liquid phase propane to the gas phase propane before introduction thereof into the carburetor of the internal combustion engine.
Although specific embodiments of the present invention have been described above with reference to the various Figures of the drawing, it should be understood that such embodiments are by way of example only and merely illustrative of but a small number of the many possible specific embodiments which can represent applications of the principles of the present invention. Various changes and modifications obvious to one skilled in the art to which the present invention pertains are deemed to be within the spirit, scope and contemplation of the present invention as further defined in the appended claims.
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A gas phase of LPG such as propane is used to power a small internal combustion engine driving or powering a preselected device such as a powered lawnmower, weed whacker, string trimmer, leaf blower or the like and the fuel system is provided with heating arrangements that insure the gas phase of the LPG is discharged from the LPG tank for all operating conditions of the device.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to the lining of pipelines or passageways.
2. Description of the Prior Art
This invention relates to the lining of pipelines or passageways, using materials which are now referred to as "cured in place" materials. Specifically, "cured in place" materials comprise flexible lining tubes including absorbent materials such as fibrous felts, e.g. polyester felts which are impregnated with curable synthetic resin such as polyester or epoxy. Whilst the lining tube is still flexible and is so impregnated, it is held by fluid (liquid and/or gas) pressure against the surface of the pipeline or passageway to be lined, so that it conforms to the surface shape of the pipeline or passageway, and whilst so held it is caused to become hard or rigid by curing of the said synthetic resin. The method of curing may be any of a number of methods including curing by heat, curing by radiation such as ultra violet radiation, or curing by ultrasonics. When heat is used the inflating medium may be heated whilst in the case of light cure and ultrasonic cure resins, an appropriate light or ultrasonic source As pulled through the applied lining tube. Some resins such as epoxy resins cure naturally, and are referred to as ambient curing resins, and these may be used if required.
Various methods as disclosed An U.S. Pat. Nos. 4,064,211 and 4,009,063 have been proposed for curing "cured in place" systems, including that the lining tube, having been pre-impregnated, may be everted into the pipeline or passageway, or alternatively may be pulled into the pipeline or passageway and then inflated, for example by means of an everting membrane. Arrangements have been suggested for effecting the impregnation of the lining tube whilst it is in or whilst it is moving into the pipeline or passageway to be cured as disclosed in U.S. Pat. No. 4,602,974.
Generally speaking, the known methods comprise inserting the lining tube into the pipeline or passageway so as to cover the surface of the pipeline or passageway between respective access points of the pipeline or passageway, such access points comprising for example access manholes, but frequently complete lining of the pipeline or passageway between man-holes is not necessary, as for example it may be the case that only a section of a pipeline or passageway has a defect or is in a poor state of repair such as to require relining by a "cured in place" method. The present invention is devoted to the provision of a system and method for the lining of a section of a pipeline or passageway.
There have been proposals for repairing sections of underground pipelines or passageways using "cured in place" lining tubes, and one such proposal is disclosed in U.S. Pat. No. 5,044,405 wherein a length of the impregnated lining tube is carried inside a flexible carrier tube. The carrier tube is in turn located inside an outer tubular casing, and the entire assembly is located in position inside the pipeline or passageway having the section to be lined. The interior of the casing is pressurized in order to evert the carrier tube and with it the lining tube out of the end of the casing and into fluid pressure contact on the section of pipeline or passageway to be lined. The pressure is maintained whilst the resin is caused to cure by any suitable method, and then the carrier tube and and casing are detached from the lining tube leaving the cured lining tube in position lining the appropriate section of the pipeline or passageway. The use of the carrier tube and casing make the method somewhat complicated as many steps are to be carried out An order to create the assembly which is inserted in the pipeline or passageway.
The present invention provides a simpler method of installation by arranging that an inflatable bladder as the lining tube applied to the outside thereof, and in this connection is might be mentioned that the lining tube may be a continuous tube when view in cross sectional elevation, or it may be a tube formed by a flat web wrapped round the bladder with the meeting edges overlapped. In some cases it is advantageous to overlap the lining tube in this way because then the lining tube need not be critically matched to the pipeline or passageway inner diameter as it will take up the correct diametrical dimension as the bladder is inflated and the degree of overlap of the edges of the lining tube will vary.
Patent specification WO 90/12243 does disclose that it is known to provide a core member around which is an inflatable bladder, and the lining tube is applied over the bladder so as to be inflated by the bladder into contact with the pipeline or passageway surface, but the core member in connection with that proposal is made up of a number of rigid sleeves which are tensioned together by means of steel cables which pass through apertures in the sleeves. The sleeve ends are configured so as to be complimentary and to interfit whereby the length of the core member can be varied as required.
A disadvantage of that arrangement is that the core member by its construction inhibits the feeding of the assembly the pipeline or passageway, because pipelines or passageways often have bends and curves and the lining and bladder are relatively delicate items which if dragged against for example the surface of an underground pipeline or passageway which is in the form of a sever, could well tear and fracture these components,
SUMMARY OF THE INVENTION
The present invention is concerned with providing an arrangement wherein an assembly including a core member and inflatable bladder with a "cured in place" lining tube thereon can be effectively positioned in an underground pipeline or passageway.
In accordance with the present invention, in a first aspect, a method of lining a section of a pipeline or passageway by a "cured in place" system comprises providing a length of lining tube which is impregnated with a curable synthetic resin and carrying that lining tube on an assembly including an annular inflatable bladder to the inside of which is provided a core tube, transporting the assembly to the section of pipeline or passageway to be lined, inflating the annular inflatable member to press the length of lining tube to said section of the pipeline or passageway and effecting the cure of same, the said core tube being a flexible unitary continuous hollow tube of sufficient rigidity to support the air pressure and of sufficient bendability to enable it to bend round curves and corners around which the assembly must pass in travelling along the pipeline or passageway to said section.
In this connection, the core or central tube, although having rigidity, in fact is of a semi-rigid construction such that it can bend slightly so as to follow the curvature of the pipeline or passageway, and also is of sufficient hoop stress to withstand an internal vacuum, because in a preferred arrangement the tube serves as a means for applying a vacuum to the assembly in order to hold the length of lining tube and the annular inflation member in collapsed condition whilst the assembly is introduced into the pipeline or passageway. Typically the rigid tube maybe a rigid rubber like material of sufficient thickness to meet the characteristics indicated above.
By virtue of providing the assembly with the central rigid tube, arrangements can be made such that several assemblies can be provided on the tube and can be applied to different sections of the pipeline or passageway simultaneously, and if the pipeline or passageway has normally accommodates liquid flowing medium, the medium can continue to flow through the tube whilst the assembly is being inserted and curing is taking place.
The present invention also provides an assembly for introduction into a pipeline or passageway, said assembly comprising a core tube surrounded by an annular inflatable bladder, said core tube being of sufficient rigidity to support the bladder when inflated without collapse of the core tube and also being of sufficient bendability to enable it to bend around curves in the pipeline or passageway into which it is inserted.
The core tube may be connected by one of its ends only to the bladder which may also be tubular formed with an inner side and an outer side but which sides are integrally connected at one end of the bladder. This construction provides that the core tube may be moved into and out of the bladder which action causes the bladder to evert and invert in the nature of a rolling pig which means that the inner side and outer side change positions when the assembly is fed into the pipeline or passageway the core tube is inside the bladder and for the purposes of clarity of explanation the terms "inner side" and "outer side" as applied to the bladder mean the inner side and outer side in relation to the core tube when the core tube is inside the bladder.
To construct the unit comprising the assembly and lining tube to be inserted in the pipeline or passageway, a length of the lining tube duly impregnated may have the bladder introduced thereinto by rolling the bladder inside out upon itself, and at the same time introducing the core tube into the central region of the pig. In this connection the bladder may communicate with a pressure hose contained inside the core tube whereby air for inflating the bladder may be provided.
The unit is constructed above ground, and then is introduced into the pipeline or passageway for subsequent inflation, the unit having the bendability of the core enabling it to be fed down manholes and along the pipeline or passageway.
To the outside of the length of lining tube there may be provided a film encasing the lining tube, and which also serves as a means enabling the creation of a vacuum inside the film thereby to collapse the assembly onto the core tube, and there may be an aperture in the central core tube enabling the vacuum to be created inside the external film.
BRIEF DESCRIPTION OF THE DRAWINGS
Embodiments of the present invention will now be described, by way of example, with reference to the accompanying diagramatic drawings, wherein;
FIG. 1 is a sectional side view inside a sewer pipe having a section to be lined and shows a lining tube and assembly in accordance with an embodiment of the invention;
FIG. 2 is a view similar to FIG. 1, but showing the assembly bladder in inflated condition;
FIG. 3 is a view similar to view 1, but showing the lining tube after the resin thereof has been cured.
FIG. 4-7 show the method of assembling the arrangement of FIG. 1;
FIG. 8 is a diagram showing the introduction of the assembly of FIG. 1 into the pipe and also showing how the centre portion of the assembly is extracted upon completion of the curing;
FIG. 9 shows an arrangement similar to FIG. 7 when in the FIG. 7 condition;
FIG. 10 shows the arrangement of FIG. 9 when the bladder is collapsed;
FIG. 11 shows a transporter for the arrangement of FIG. 10 to enable it to be transported into the sewer;
FIG. 12 shows the arrangement of FIG. 10 when carried by the transporter of FIG. 11 and having transporting lines connected thereto; and
FIG. 13 is a sectional elevation of the arrangement of FIG. 12 taken on the line A--A of FIG. 12
DETAILED DESCRIPTION
Referring to the drawings, and firstly to FIG. 1, a length of sewer pipe (10) to be lined with a length of cured in place lining tube is shown as having imperfections (12) giving rise to the reason for the lining operation. It is assumed that the remainder of the pipe Is otherwise sound, and complete relining of the pipe is therefore inappropriate.
In register with the section (10) to be lined is shown a unit (14) which comprises a tubular construction having a central core tube or pipe (16) of hard rubber to the like of sufficient rigidity to withstand an inflation pressure and internal vacuum which as will be explained is applied thereto, but is bendable so as to be capable of following any bends or curves in the pipe (10) as the unit (14) is fed thereinto, as will be explained. The pipe (16) may be of corrugated construction and have internal reinforcing and circumferentially extending metal wires in the corrugations so that it can function as described above.
Surrounding the pipe (16) Is an annular inflation bladder (18) Of flexible plastics material, and formed in an endless arrangement in that tubular bladder (18) is defined by a length of tubular flexible and inflatable material turned inside upon itself, so that its ends as indicated by (20) and (22) are sealingly anchored to the tube (16) at one end only so as to form an annular pocket which can be inflated by means of an air pressure hose (24) and in particular an outlet (26) thereof which opens into the chamber created by the inflation member between the said ends (20) and (22).
The tube (18) may for example be of a silicone material so that it can be removed from the assembly after the inflation operation as will be described.
Surrounding the annular tubular bladder (18) is the length of lining tube (28) which comprises suitably a tube or overlay of felt material which is impregnated thoroughly with a curable synthetic resin. The felt may typically be of polyester fibres, and a polyester resin may be used for the impregnation. Other felts and mixtures and other resins can be used.
Surrounding the felt layer (28) is a shrouding tubular film (30) to complete the unit.
In the condition of FIG. 1, the assembly is in flexible but collapsed condition, to enable it to be fed into the pipe (10) so that there is in fact as shown a substantial clearance between the shroud (30) and the surface of the pipe (10). This arrangement is achieved in that a vacuum is drawn through an aperture (32) in the pipe (16) which leads to the inside of the shroud (30), but to the outside of the inflation bladder (18) thereby by drawing the assembly tightly onto the pipe (16). To this end sealing tapes may be applied to the ends of the shroud (32) to prevent vacuum leaks.
When the unit is in position, as shown in FIG. 2 the vacuum inside the pipe (16) is removed, and the interior of the inflation bladder (18) is pressurised so as to blow up the lining tube length (28), to cause it to be forced to the surface of a pipe (10), as shown clearly in FIG. 2. Whilst in this condition the resin is allowed to cure or is caused to cure by some initiation means such as heat, light, ultrasonics or the like, and after curing takes place, the pipes (16) and the inflation bladder (18) are withdrawn leaving the cured resin lining (28) in place as shown in FIG. 3. FIG. 4-7 illustrate how the assembly (14) is put together, and it will be seen than initially from FIG. 4 the lining tube length (28) with its shroud (30) is arranged end to end with the inflation bladder (18), from which has been pulled core pipe (16) so that it is arranged end to end with the pipe (16). The right hand end of the inflation tube (18) is introduced into the interior of the lining tube length (28), and the right hand end of the pipe (16) is inside the left hand end of the inflation tube (18).
It is now simply a matter of inflating the inflation tube (18) for example to a low pressure in the order of 5 p.s.i. as shown in FIG. 5 and then the inflated member (18) is evened into the lining tube (28), by progressively pushing the pipe (16) into the interior of the inflation tube (18) as shown in FIG. 6, (the lining tube being held by hand pressure if necessary) until the arrangement indicated in FIG. 7 is reached. The pressure is removed from the inflation tube (18), and then vacuum is applied through the port (32), to cause the assembly to collapse to the FIG. 1 condition.
FIG. 8 shows that the assembly (14) can be introduced by means of a traction apparatus (36) with a vacuum coupling (38) from a ground level trailer (40), there being appropriate air hoses (42) connected through the central pipe (16) of the assembly to enable the inflation and deflation of the assembly inflation bladder (18) as described above for the completion of the insertion.
FIG. 8 shows that the unit marked `U` can be fed down a manhole `M` and fed into the pipe.(10) bending as it turns from the manhole `M` into the pipe (10), without collapse of the core tube (16), which is an important aspect of the present invention. This bendability of the unit `U` is also important when the unit lies to transverse underground pipes which curve as it is important not to have heavy frictional forces on the unit `U` as it is travelling along the pipe (10).
An effective means is therefore provided for positioning and applying a length of lining tube of a "cured in place" type to a specified section of a pipeline. The positioning of the assembly (14) may take place by any conventional means such as by the use of a television camera, or by arranging for some pre-determined datum to be established and in relation to which the assembly (14) is positioned, but such positioning method is not part of the present invention.
Referring now to FIGS. 9-13, which show an alternative embodiment of the invention, the assembly shown is constructed and operates in the same principle as already described in relation to the previous embodiment, but includes a number of modifications which also can be included in the embodiment of FIGS. 1-8. The unit shown in FIGS. 9-13 is put in place in the manner already described in relation to the previous figures.
Referring to these drawings, in FIG. 9, the unit shown is in the position corresponding to the position shown in FIG. 7 for the previously described unit, and similar reference numerals are used in relation to the equivalent parts already described in relation to the previous figures. Thus, the lining tube is indicated by reference 28, and it is shown as being supported on the inflated bladder (18) which in turn receives centrally thereof the core pipe (16). The core pipe (16) has enlarged ends (16A) which may be formed by shaping the pipe ends or by adding thereto enlargement rings or the like. These ends (16A) stabilize the pipe inside the inflated bladder (18), and if such enlargement (16A) are not provided, there can be a tendancy for the core pipe (16) to be held by the bladder in a slightly unstable manner such that the merest force might cause the pipe (16) to be ejected from the bladder as the bladder rolls upon itself. The enlarged ends inhibit this difficulty.
In collapsing the bladder (18) from the FIG. 9 position the FIG. 10 position, any suitable arrangement may be adopted such as by simply exhausting the air inside the bladder or by positively withdrawing it through suitable means. For example the air may be withdrawn through pipe (24) which also serves as the air pressure pipe.
When the bladder is collapsed, the bladder and the lining (28) are then folded around the core pipe (16) as shown in FIG. 10, and the meeting edges of the lining tube (28) are temporarily held by means of adhesive tapes (30) applied across the meeting edges as shown. The assembly in the condition shown in FIG. 10 is inserted into the pipeline or passageway by being carried on a transporter (32) which resembles a hammock and is made of a sheet of flexible material such as a reinforced plastic sheet. The ends of the hammock transporter (32) are connected to pull ropes (34) and (36) by which the assembly can be inserted in the pipeline or passageway.
FIG. 12 shows that the hammock transporter (32) after it receives the unit of FIG. 10 is wrapped around the sides of the unit and further temporary adhesive holding patches (38) are applied across the transporter edges and the adjacent bladder and lining tube as shown in FIG. 12.
FIG. 12 also shows the air line (24), and at the other end of the assembly the guide ring (40) Which passes through an aperture (42) in the end (16A) of core pipe (16) so that an extension of rope (34) in the form of a slip rope (42) can pass therethrough as shown.
FIG. 13 shows the arrangement of FIG. 12 in sectional elevation.
The assembly of FIG. 12 is pulled into the underground pipeline or passageway in the direction of arrow (44) by pulling on ropes (34) and (42), the rope (36) serving as a hold back means in order to control the in feed of the assembly into the pipeline or passageway. Positioning of the assembly of FIG. 12 inside the pipeline or passageway is again by any suitable means such as a television camera, and the entire assembly shown in FIG. 12 as the bendability hereinbefore referred to enabling smooth positioning of the assembly with minimal damage due to friction on the components of the assembly as it travels around curved sections of the pipeline or passageway. In this connection, the slip rope (42) serves to prevent the assembly of FIG. 10 from slipping relative to the hammock transporter (32) should the unit rub against the pipeline or passageway walls in its travel to its final position.
When the unit is in its final position, rope (34) is pulled whilst air line (24) is held, so that the transporter (32) separates from the assembly of FIG. 10, such assembly remaining in the correct position. During this separation, the slip rope (42) is allowed to slip through ring (40) and it will also be separated from the assembly. Hold back rope (36) travels with the transporter (32), and therefore is removed from the pipeline or passageway leaving the assembly in the correct position. It is to be mentioned that during this separation operation, the adhesive patches (38) yield due to the separating forces.
It is now simply a matter of inflating the bladder (18) to break the holding effect of the tapes (30) and to allow the assembly to inflate to the condition shown in FIG. 9 and also as shown in FIG. 2 cured by the lining tube is applied against the surface to be aligned and the procedure is similar to that already described in relation to the previous figures.
The core pipe (16) and the bladder (18) are removed by pulling on the air line (24) to pull out the core pipe and to invert the bladder (18) and to peel it away from the cured lining tube leaving the condition as shown in FIG. 3.
By the provision of the central rigid pipe (16), simultaneous inflation of a number of assemblies inside the pipeline may be effected.
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An assembly which can be inserted into a pipeline or passageway on which a curable resin impregnated flexible lining is placed about an inflatable bladder is provided. The bladder is mounted to one end of a core pipe and folded over on itself. Medium flowing in the pipeliner passageway can pass through the core pipe during a lining operation. The core pipe is of sufficiently rigid nature to withstand inflation pressure to move the lining tube into the pipeliner passageway surface by inflation of the bladder, but yet is sufficiently flexible and bendable so as to bend enabling it follow curbs and falls in the pipeliner passageway into which it is inserted. Temporary holding means restrain the liner during insertion.
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BACKGROUND OF THE INVENTION
This invention relates to a quilting machine with relatively moving cloth holder carriage and sewing head in mutually orthogonal directions.
Currently available, commercially, are various quilting machine types which are employed for quilt working mattresses, bedspreads, comforters, and the like articles. One type, such as disclosed in U.K. Pat. No. 1,207,451, comprises a first carriage, on which a cloth to be quilted is held, arranged to run linearly on a second carriage. The latter carriage runs, also linearly, on an orthogonal plane to that of the first carriage.
Both carriages are driven to move under a stationary sewing head along a path determined by a template or other costraint.
Another type of a quilting machine, such as disclosed in French Pat. No. 1,550,051, operates in precisely the opposite way, i.e. with the sewing head moving along orthogonal axes over a stationary carriage holding a cloth to be quilted.
A further quilting machine type comprises one or more sewing heads which are driven back-and-forth relatively to a cloth which is being fed continuously lengthwise thereunder.
The first two of the types mentioned above can provide elaborate sewing. However, the carriage drive poses, on account of the inertia masses involved, somewhat narrow limits on operation, and the unavoidable shaking encountered adversely affects the quilting operation accuracy.
The quilting machine of the third type, alternatively, finds application for just repeatitive quilting of an inferior class.
SUMMARY OF THE INVENTION
It is a primary object of this invention to provide a quilting machine which can obviate such prior shortcomings, in particular by significantly attenuating the vibratory effects on the cloth holder carriage, so as to afford high quality sewing in a shorter time.
A further object of this invention is to provide a quilting machine which is highly flexible in operation, in connection with its ability to perform elaborate seam lines.
These objects are achieved by a quilting machine which is characterized in that it comprises a cloth holder carriage whereon a cloth to be quilted is stretched on a horizontal plane and which is movable along a rectilinear path, above said cloth there being arranged at least one sewing head guided in an orthogonal direction to the carriage travel direction, and a means being provided for driving said carriage and sewing head along respective runways to cause the seam line to follow a preset pattern.
BRIEF DESCRIPTION OF THE DRAWINGS
Further features of the invention will be more readily understood from the detailed description which discloses an embodiment thereof, as illustrated by way of example in the accompanying drawings, where:
FIG. 1 is a front elevation view of a twin sewing head sewing machine according to the invention;
FIG. 2 is a view taken on the plane II--II of FIG. 1;
FIG. 3 is a view taken on the plane III--III of FIG. 1;
FIG. 4 is a view taken on the plane IV--IV of FIG. 2 and to an enlarged scale; and
FIG. 5 is a view, also to an enlarged scale, of the carriage as shown in FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
With reference to the drawing views, generally indicated at 1 is an overhead frame comprising an upper horizontal beam 2 and lower horizontal beam 3 which are supported at the opposed ends thereof by two floor-standing pillars 4,5. The lower beam 3 is supported by a third pillar 6 located intermediately between the pillars 4,5 but shifted toward the latter. The beams 2,3 have, when viewed in cross-section, the shape of two U's opening toward each other.
Between the beams 2,3 and pillars 4,5 there are defined two openings 7,8 of equal length the lower whereof is split in two by the intermediate pillar 6 to define an additional opening 9.
Attached to the inward faces of the pillars 4,6 are two brackets 10,11 which protrude from said pillars in horizontal alignment and to which two respective horizontal longitudinal stringers 12,13 are attached which extend parallel to each other and perpendicularly to the frame 1.
The longitudinal stringers 12,13 extend through the opening 8 to overhang on opposed sides of the frame 1. The ends of the longitudinal stringers 12,13 stand on the floor through substantially vertical adjustable height feet, 14 thereby enabling said longitudinal stringers to be supported on a truly horizontal plane. The longitudinal stringers have spacers 15 attached thereto to which are in turn attached two cylindrical bars 16,17 which serve as runways for a carriage 18 whereon a cloth to be quilted is to be stretched.
The carriage 18 comprises a rectangular frame formed by lengthwise 19 and crosswise 20 sectional members, having at its corners four idle wheels 21 which are grooved circumferentially and enable the carriage 18 to travel along the bars 16,17.
The crossmembers 20 have the horizontal portions of two pairs of right-angled elements 22,23 attached thereto.
Rigidly connected to the vertical portions of said two pairs of right-angled elements 22,23 are two pairs of plates 24 and 25 which support two parallel shafts 26,27 through bearings.
The shaft 26 is driven rotatively via a center reduction gear 28 which receives its motion from a motor 29 through a drive belt 30 and respective pulleys 28a,29a keyed on the output shafts of the reduction gear and motor. The motor 29 and reduction gear 28 are mounted on a box-like bracket 31 attached to the crossmember 20.
Keyed on the shafts 26,27, at the opposed ends thereof, are respective pairs of output 32 and input 33 sprocket wheels which are in mesh engagement with two chains 34,35 trained therearound in closed loop configuration and being deflected by deflector wheels 36,37 to present two proximate, horizontal runs. Such horizontal runs are enclosed by shrouds 38,39 the end portions whereof are bent arcuately upwards above the sprocket wheels 32.
The links of the chains 34,35 comprise juxtaposed arms 40,41 (see FIG. 5) which project in opposed directions and carry blocks 42,43 bristling with outwardly facing needles 44,45. Keyed on the shaft 26, adjacently to, and rotating concurrently with the blocks 42,43, are disks 46,47 the outer diameter whereof is larger than that defined by the ends of the needles.
The needles have the purpose of holding the cloth to be quilted along two longitudinal edges. Penetration of the needles into the cloth is achieved by means of a pair of circular brushes 48 carried rotatably in arms 49 articulated to the ends of extensions 50 of the pair of right-angled elements 23.
The brushes 48 are coplanar with the needles 44, 45 and held against the latter by pneumatic jacks 51 interposed between the tops of said pair of right-angled elements 23 and oscillating arms 49. The cloth which should be stretched between the needles 44,45 is picked up by a roll 52 supported on a frame 53 which is attached to the carriage 18 through a hinge 54. The frame 53 has two feet 55 comprising rotatable wheels 56 which run on a pair of rails 57 secured on the surface and parallel with the rails 16,17.
The motion of the carriage 18 is derived from a gear motor 58 suspended, through brackets 59, from the lower beam 3 of the frame 1. The gear motor 58 drives a shaft 60 which is supported, at its opposed ends, on shoulders 61,62 projecting downwards from the beam 3.
Keyed to the ends of the shaft 60 projecting beyond the shoulders 61,62 are pinion gears 63,64. On each shoulder 61,62 are cantilevered a pair of idle gear wheels 65,66 lying on the same plane as the pinions 63,64 but on opposite sides with respect to the latter.
The pairs of gear wheels 65,66 keep trained at a certain angle around the pinion gears 63,64 two chains 67 stretched between the front and rear crossmembers 20 of the carriage 18 to form two racks which are in mesh engagement with said pinion gears 63,64.
As illustrated in FIG. 3, the chains 34,35 are passed through the opening 7 as the carriage frame moves through the opening 8, thereby the beam 3 is located under the chains 34,35 and over the longitudinal stringers 19.
Inside the beams 2,3, and extending over the full length of the latter, are two pairs of guide bars 68, 69 supporting the sewing head carriage 70.
The bars 68,69 have a square cross-section and are positioned edgewise on the sidewalls of the beams 2,3 by means of diagonal elements 71,72 whereto they are attached.
The carriage 70 comprises two plane parallel plates 73,74 identical to each other and shaped like a "C" with two horizontal portions 75,76 which extend into the beams 2,3 and are connected through vertical portions 77 (see FIG. 4).
The plates 73,74 are interconnected by partitions interposed between the horizontal upper portions 75 and partitions 79 interposed between the horizontal lower portions 76. Attached to the outer faces of the plates 73,74 are pairs of small blocks 81,82,83 and 84, of which the first pair are rigid with the upper portions 75 and the second pair with the lower portions 76. Cantilevered from each block 81-84 are a pair of small rollers 85 having their rotation axes arranged at 90° to each other and in tangential rolling engagement with the juxtaposed faces of the bars 68,69. Mounted between the vertical portions 77 of the carriage 70 is a bracket 86 which projects from the vertical portions 77 in the opposite direction to the horizontal portions 76.
On the bracket 86, which is strengthened by underlying ribs 87, there is mounted an electric motor 88 with a shaft whereto the drive pulley 89 is keyed. Trained around the pulley 89 is a belt 90, which is also trained around the driven pulley 91.
The pulley 91 is keyed to a shaft 93 which is journaled within, and carried rotatably in between two partitions 78 and extending on the centerplane of the carriage between the upper portions 75 over nearly the full length of the latter. Keyed to the shaft 92, beside the pulley 91, is a positive drive sprocket wheel 93 which, through a toothed belt 94, transmits the motion to a second sprocket wheel 95 rotatively keyed to a shaft 96 journalled at the partitions 79. The shaft 96 is parallel to the upper shaft 92 and extends between the horizontal lower portions 76, of the carriage 70.
Fastened between the upper portions 75 is a plate 97 having slots 98 extending parallel to the shaft 92.
Suspended from the plate 97, by means of brackets 99,100 is a sewing head 101 of conventional design, which receives its motion from the shaft 92 through a drive including two sprocket wheels 102,103 and a corresponding toothed belt 104. The pulley 102 is rotatively rigid with a splined portion 105 of the shaft 92 and has a circumferentially grooved side bushing 106, with which engages a yoke 107 presented at the top of the bracket 100. Thus, on loosening the fastening bolts of the brackets 99,100 from the plate 97 it becomes possible to shift the sewing head along the plate itself and the pulley 102 along the splined portion 105. Likewise, between the ends of the upper portions 75, there are arranged two plates 108 from which a second sewing head 111 is suspended through brackets 109,110, stationary relatively to the carriage 70. This sewing head also receives its motion from the shaft 92 through a drive including two sprocket wheels 112,113 and a corresponding toothed belt 114.
Cooperating with each of the sewing heads 101,111 are respective "hook" devices 115,116 mounted on respective plates 117,118 interposed between the carriage lower portions 76.
The hook device 115 can be shifted across the plate 117 to proceed the displacement of the sewing head, whereas the device 116 is stationary. The device 115 receives its motion from the shaft 96 via a belt drive 119 which is trained around a pulley 120 keyed to the shaft 96 and a pulley 121 keyed to a shaft suitably journaled within the hook device 115. The device 116 is juxtaposed to the device 115, in order to extend the lateral bounds of the sewing machine working range and improve access to the cops thereby facilitating their replacement. To obtain the same direction of rotation for the hook, however, a reversing gear is provided which comprises two gear wheels 122,123 accommodated in the device and meshing together, of which the wheel 122 drives the hook and the other wheel 123 is secured on the axle carrying the pulley 124 which receives its motion from the shaft 96 through the belt 125 and pulley 126. It should be noted that the shaft 96 is divided into two sections which may be coupled together by means of an axially sliding splined bushing 127. The bushing 127 is in constant rotary engagement with the end of one section and can overlap the end of the adjacent section to rotatively engage the latter on operation of a yoke lever 128 journalled between the portions 76. Thus, it becomes possible to isolate the end section 129 of the shaft 96 from the drive means 88-95 when the second sewing head 111 is not to be operated (see FIG. 4).
The movement of the carriage 70 along the guides 68, 69 is generated by a gear motor 130 having a sprocket wheel 131 around which a chain 132 is trained. The lower run of the chain 132 extends below the beam 3 through openings in the pillars 4 and 6 and is passed around a sprocket wheel 133 journalled axially in a support 134 attached to the outside of the pillar 4. The upper run of the chain 132 extends into the beam 3 and is deflected away from the axis of said sprocket wheel 131 by an idle roller 135, thereby defining a horizontal trajectory, parallel to said lower run. One point on the chain upper run is secured to the carriage 70 by means of a small plate 136 (FIG. 2).
The quilting machine described hereinabove operates as follows. First, the cloth is positioned on the carriage 18. To accomplish this, the cloth is unwound from the roll 52 and deflected horizontally by a roller 137 on the frame 53 (FIG. 3) under the brushes 48 which drive its edges onto the needles 44, 45. The driving of the chains 34,35 generated by means of the motor 29 causes the desired length of cloth to be fed a corresponding distance under the sewing heads and over the respective hook devices.
Then, the sewing step begins with the actuation of the motor 88 which powers the sewing heads 101,111 and hook devices 115,116.
Simultaneously the motors 58 and 130 are operated to move the cloth holding carriage 18 along the rails 16,17, and respectively, the carriage 70 along the bars 68,69. The orthogonal reciprocating movements of the carriages 18 and 70 enable the formation of any seam lines and, hence, of an indefinite range of patterns.
The carriage drive motors are suitably controlled by an electronic processor. It is possible, however, to perform the quilting operations by controlling the carriages through a tracer point arranged to follow a template.
On completion of the quilting operations, a fresh cloth section paid out from the roll 52 can be stretched between the chains 34,35, while the completed quilted cloth section is simultaneously ejectd from the carriage 18. Disengagement of the needles 44,45 is accomplished by the disks 46,47 which, having a larger diameter, than that defined by the ends of said needles, will raise the cloth edges off the needles as the cloth is on the point of leaving the carriage. The machine may be equipped with a cutter device to sever the completed quilted cloth section from the remaining cloth.
It may be appreciated that the invention fully achieves its objects. In particular, it is to be noted that the cloth to be quilted is only allowed to move in one direction, thus greatly reducing the margin for errors due to the carriage being stopped and restarted.
An additional advantage is that the moving masses are reduced to permit higher speed operation.
Particularly advantageous has proved to be the use of several sewing heads placed at adjustable mutual spacings to optimize performance and, simultaneously achieve highly versatile operation features regarding cloth size and effectuation of complex pattern seam lines.
The invention as disclosed is susceptible to many modifications and changes. One of these envisages, for instance, that a frame be used instead of the chains 34,35 whereon the cloth would be stretched and held down by suitable clamps. Another modification provides for the roll of cloth to be either supported directly on the carriage or held stationary on the floor. The quantity of rolls may vary according to the number of layers composed within the manufactured article.
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A quilting machine for quilting mattress, bedspreads, comforters, and the like comprises a carriage on which an article to be quilted is held stretched. The carriage is guided by horizontal rails along which it is moved back-and-forth by a drive unit. Said carriage is overlaid by another carriage which is guided in an orthogonal direction to that of said first-mentioned carriage and carries one or more sewing heads. The latter carriage is driven by a unit which determines, in cooperation with the drive unit of said first-mentioned carriage, the relative movement of the sewing heads and cloth in accordance with a preset pattern for the seam line.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application Ser. No. 61/530,688, filed Sep. 2, 2011, titled “Premium Seat Offering Extra Wide Bed,” the entire contents of which are hereby incorporated by reference.
FIELD OF THE INVENTION
[0002] Embodiments of the present invention relate generally to premium seats for aircraft and other passenger transport vehicles that provide extra seat room. Certain embodiments are also designed to allow easier access to the seat.
BACKGROUND
[0003] Premium seats for civil aircraft have various seat positions, from the most upright to a full flat or lie flat bed position, especially for long or overseas flights. It is desirable to provide premium seats that allow such flexibility in seat movement, but that also provide as much space as possible for the passenger in each desired position.
[0004] Additionally, passenger vehicle seats need to be designed in order to provide easy access to passengers, particularly disabled passengers. For that reason, aisle side armrest are usually either removable, droppable, or rotatable in order to allow a passenger to be translated laterally from a wheel chair to the seat (or to otherwise provide increased access to the seats).
BRIEF SUMMARY
[0005] Embodiments of the invention described herein thus provide premium seats for aircraft and other passenger transport vehicles that offer extra seat room by providing a new tray table configuration, which also enhances privacy for each passenger. Certain embodiments also provide an improved outer armrest configuration.
BRIEF DESCRIPTION OF THE DRAWINGS
[0006] FIG. 1 shows a front perspective view of a seating system according to one embodiment of the invention, with one of the tray tables in a deployed position and both of the seats in the upright position.
[0007] FIG. 2 shows a front plan view of the seating system of FIG. 1 .
[0008] FIG. 3 shows a side perspective view of the seating system of FIG. 1 , with one of the tray tables in a deployed position and one of the seats in the bed position.
[0009] FIG. 4 shows a front plan view of the seating system configuration of FIG. 3 .
[0010] FIG. 5 shows a side perspective view of a first tray table embodiment having a hinge and a slide.
[0011] FIG. 6 shows a side perspective view of FIG. 5 with the tray table moving to its stowed position.
[0012] FIG. 7 shows a side perspective view of a second tray table embodiment, which rotates up and down.
[0013] FIG. 8 shows a side perspective of a retractable and sliding outer armrest according to one embodiment of the invention.
DETAILED DESCRIPTION
[0014] Embodiments of the present invention provide improved passenger seating systems for passenger transport vehicles. Although they are particularly useful in connection with commercial aircraft and/or private aircraft, they may also be installed on buses, trains, RVs, or any other vehicle where passengers may desire larger seating spaces for longer travel times. As shown in FIG. 1 , the seating system 10 generally includes at least two seats 12 , 14 separated by a center console 16 . Although a seating system with two seats is shown, it should be understood that the concepts described herein are equally applicable to seating systems having more than two seats, such as three, four, or more seats in an aisle. There will be provided a single center console for a two-seat unit, and two center consoles provided for a three-seat unit, and so forth, with one center console between adjacent seats. Center console 16 is shown having two trays 18 , 20 associated therewith (although it should be understood that a center console for an odd-number of seats in a system may only need to have one tray associated therewith.)
[0015] In the embodiment shown in FIGS. 5-6 , the trays 18 , 20 are positioned on a slide 22 . In one embodiment, the center console 16 may be provided with a track 24 along its underneath surface 26 or alongside the console edge that allows the slide 22 to move forward and backward to effect movement of the trays 18 , 20 . When the passenger wishes to store the tray table, he rotates it upward along a hinge 23 and then slides it backward along slide 22 . These figures also show a compartment 50 positioned between the headrests that may be used to provide a cleaner looking storage location for the tray tables, as well provides as an improved privacy feature between passengers.
[0016] FIG. 7 shows an alternate embodiment, with the tray table moveable on a slide, but having a pivot feature 52 configured to allow the food tray to be moved from its stored position to its fully deployed position. The table is allow to pivot around an oblique axis 54 in use.
[0017] In prior seat systems, a center console generally has in its lower portion, below the level of the armrest, a compartment designed to store the tray tables. When they are not in use, the passengers simply open a cover lid on the console and store the tray into the space provided therein. Such a compartment will have a minimum width which limits the space available for the passenger in bed position. The center console 16 of the present invention is designed to offer a maximum space to the passenger in bed position, minimizing the thickness of its mid portion 32 , which acts only as a structural barrier between passengers. In other words, the mid portion 32 is not wide enough or thick enough to serve as a food tray stowage compartment, which allows the seating system to provide more leg room and space to the passenger, whether they are seated or in the lying down position.
[0018] The tray tables 18 , 20 have been designed to be stored in a vertically upright position between head rest portions 36 of adjacent seats 12 , 14 , and above the armrest level. This provides a stowage location for the trays, but it also provides an additional privacy screen between passengers.
[0019] A further feature of the seating system 10 is a retractable outer armrest 38 . The present invention provides an outer armrest with a design that allows the armrest 38 to slide back into an opening 42 in the privacy shell 40 . In addition to increasing the ease of entry into the seat and to comply with regulations regarding accessibility for disabled passengers, this feature also increases the available width when the seat is in the bed position. When the armrest 38 is deployed, it affords a privacy enclosure to the passenger. The inner area provided by the curved shape provides a few extra centimeters or inches of valuable passenger space.
[0020] In a particular embodiment, the armrest 38 has a C-shaped cross section, provided by an outer panel 44 with an inwardly curved upper portion 46 , as shown in FIG. 5 . A lower portion of the seat shell may have a track 48 along which the armrest is configured to slide. The rear portion privacy shell is then provided with an opening 42 that can receive most (if not all) of the armrest 38 when it is in a retracted position.
[0021] Changes and modifications, additions and deletions may be made to the structures and methods recited above and shown in the drawings without departing from the scope or spirit of the invention and the following claims.
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Embodiments of the invention provide premium seats for aircraft and other passenger transport vehicles that provide extra seat room by providing an improved tray table configuration, which also enhances privacy for each passenger. Certain embodiments also provide an improved outer armrest configuration.
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TRADEMARKS
[0001] IBM® is a registered trademark of International Business Machines Corporation, Armonk, N.Y., U.S.A. Other names used herein may be registered trademarks, trademarks or product names of International Business Machines Corporation or other companies.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] This invention relates to a method for using a diagnostic software tool that allows a software developer to track the number of times each memory block is enlarged, and highlights the most frequently enlarged memory blocks, and in particular, to identifying to the software developer areas in code where coding reliability and or efficiency improvements can be made to reduce the processing time utilized for memory reallocations.
[0004] 2. Description of Background
[0005] Application developers sometimes attempt to conserve virtual memory by allocating memory blocks that may or may not be too small for their intended purposes. In general, memory blocks may be repetitively enlarged in small increments via reallocation, whenever the need arises. The resulting application programs may also reallocate memory blocks frequently. Processing time is consumed each time memory is allocated, reallocated, and or moved. As memory manipulations occur excessively, the performance of the software and as such the system in general can be degraded.
[0006] The performance impact of repeating reallocations can depend on the state of the underlying heap. If the heap manager needs to move a memory block to a new virtual address range to accommodate the block's enlargement, then the act of copying the block's contents, from a central processing unit (CPU) processor time and performance perspective, can be costly. If the heap manager needs to commit additional virtual memory to provide space for a moved block, the performance costs can increase further. In addition, the empty space that remains after a block has been moved may not be filled until another block of the original size or a smaller size is allocated. Because of these factors, reallocation can cause intrablock waste, heap fragmentation, and reduced performance.
SUMMARY OF THE INVENTION
[0007] The shortcomings of the prior art are overcome and additional advantages are provided through the provision of a method of determining code efficiency by monitoring memory reallocation, the method comprising tracking a plurality of memory blocks allocated and or deallocated; incrementing a reallocation count associated with a specific one of the plurality of memory blocks when a memory reallocation occurs; incrementing a move count associated with a specific one of the plurality of memory blocks when a memory move occurs; and displaying, when a heap snapshot and end-of-run occurs, an object reference graph view highlighting the plurality of memory blocks with the highest reallocation count, and highest move count.
[0008] System and computer program products corresponding to the above-summarized methods are also described and claimed herein.
[0009] Additional features and advantages are realized through the techniques of the present invention. Other embodiments and aspects of the invention are described in detail herein and are considered a part of the claimed invention. For a better understanding of the invention with advantages and features, refer to the description and to the drawings.
TECHNICAL EFFECTS
[0010] As a result of the summarized invention, technically we have achieved a solution, which is a method of determining code efficiency by monitoring memory reallocation within a software application that is analyzed at runtime.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] The subject matter, which is regarded as the invention, is particularly pointed out and distinctly claimed in the claims at the conclusion of the specification. The foregoing and other objects, features, and advantages of the invention are apparent from the following detailed description taken in conjunction with the accompanying drawings in which:
[0012] FIG. 1 illustrates one example of a diagnostic routine for determining code efficiency by monitoring heap memory activity; and
[0013] FIG. 2 illustrates one example of a diagnostic routine for displaying the profiling results of heap memory activity.
[0014] The detailed description explains the preferred embodiments of the invention, together with advantages and features, by way of example with reference to the drawings.
DETAILED DESCRIPTION OF THE INVENTION
[0015] Turning now to the drawings in greater detail, it will be seen that in FIG. 1 there is illustrated one example of a diagnostic routine for determining code efficiency by monitoring memory reallocation.
[0016] A general-purpose profiling tool, when applied to a software application under test, may indicate overall time spent in methods, or intrablock waste within heap memory blocks, or fragmentation of heap regions. However, no such diagnostic tool can signal the combined set of problems caused by recurring memory block enlargement. An application that frequently reallocates memory may suffer from heap fragmentation and performance degradation, depending on its runtime conditions, input data, and other factors. Even when such an application seems to perform well and shows encouraging profiling results in a test setting, it may perform poorly when it is deployed.
[0017] In an exemplary embodiment of the present invention, a diagnostic routine is used to determine and display the most frequently enlarged memory blocks. In this regard, the routine tracks the number of times each memory block is enlarged, and then highlights the most frequently enlarged block(s) on the object reference graph. As such, a software engineer and or a programmer can utilize the results of the diagnostic routine to identify and make changes to the code of the software application under test, in an effort to minimize the amount of processing time consumed and or number of occurrences encountered by memory manipulations, thus improving reliability, efficiency, and performance of the software application under test.
[0018] Referring to FIG. 1 there is illustrated one example of a diagnostic routine for determining code efficiency by monitoring heap memory activity. In an exemplary embodiment, the routine intercepts malloc( ), realloc( ) and other heap memory allocation and deallocation application programming interface (API) functions. The routine tracks each heap memory block that is allocated, when a block is reallocated a reallocation counter is incremented for that block, and if a block is moved to make room for enlargement, a move counter is incremented for that block. The method begins with the program running in block 1002 .
[0019] In block 1002 heap memory is allocated, deallocated, and or reallocated by the application under test. Processing then moves to decision block 1004 .
[0020] In decision block 1004 a determination is made as to whether or not a memory allocation or deallocation occurred. If the resultant is in the affirmative that a memory allocation and or deallocation occurred then processing moves to block 1006 . If the resultant is in the negative that a memory allocation or deallocation did not occur then processing moves to decision block 1008 .
[0021] In block 1006 each allocated heap memory block is tracked. Processing then moves to decision block 1008 .
[0022] In decision block 1008 a determination is made as to whether or not a memory reallocation occurred. If the resultant is in the affirmative that a memory reallocation occurred then processing moves to block 1010 . If the resultant is in the negative that a memory reallocation did not occur then processing moves to decision block 1012 .
[0023] At block 1010 a reallocation counter for that block is incremented. Processing then moves to decision block 1012 .
[0024] In decision block 1012 a determination is made as to whether or not memory has been moved. If the resultant is in the affirmative that memory has been moved then processing moves to block 1014 . If the resultant is in the negative that memory has not been moved then the program continues to run and the routine is exited.
[0025] In block 1014 a move counter for that block is incremented and the program continues to run after the routine is exited.
[0026] Referring to FIG. 2 there is illustrated a diagnostic routine for displaying the profiling results of heap memory activity. In an exemplary embodiment when a heap snapshot occurs, or at the end-of-run, an object reference graph view highlighting the block(s) with the highest reallocation count and or move count is displayed. The method begins with the program running in block 2002 .
[0027] In block 2002 a snapshot or end-of-run condition is detected. Processing then moves to block 2004 .
[0028] In block 2004 processing takes steps to block all other application threads. Processing then moves to decision block 2006 .
[0029] In decision block 2006 a determination is made as to whether or not the threads have been blocked. If the resultant is in the affirmative that is the threads have been blocked then processing moves to block 2008 . If the resultant is in the negative that is the threads have not been blocked then processing returns to block 2004 .
[0030] In block 2008 an object reference graph view highlighting the block(s) with the highest reallocation count or move count is displayed. Such display can be in accordance with any user preference settings. Processing then moves to block 2010 .
[0031] In block 2010 the other application threads previously blocked are unblocked. The program continues to run or exits after the routine is exited.
[0032] In an exemplary embodiment, because some developers will want to understand the performance characteristics of their reallocation scenarios in a test setting, this method could be implemented as part of a general-purpose performance profiling tool such as IBM RATIONAL QUANTIFY, a member of the IBM PURIFY PLUS product family. QUANTIFY provides a call graph that shows the amount of time spent in each method of a profiled application. A “Highlight:” pull down menu in QUANTIFY allows users to select subsets of the call graph that are expensive in various ways. If QUANTIFY is modified to do PURIFY-style memory tracking, then a QUANTIFY call graph could be informed by this reallocation-tracking method of the present invention. The method(s) responsible for repetitive reallocations could be highlighted. A QUANTIFY user could then select the highlighted method(s) to show the amount of time spent performing those reallocations.
[0033] Furthermore, like “classic” PURIFY, QUANTIFY also does not currently provide an object reference graph. Both PURIFY-style memory tracking and PURIFY for Java's object reference graph would be needed in QUANTIFY, in order to show both block reallocation counts and the method performance data outlined in the previous paragraph, all in one tool.
[0034] In another exemplary embodiment, in integrating this method into QUANTIFY one might want to associate tracked memory blocks with the methods shown in QUANTIFY's call graph. The simplest way to make this association might be to track each block's “allocation location”, as PURIFY does today, and to search the call graph for the node that corresponds to the most frequently enlarged block(s). An internal set of links between each call graph node and a list of associated tracked memory blocks might prove to be highly reliable but would also require more memory overhead for QUANTIFY.
[0035] The capabilities of the present invention can be implemented in software, firmware, hardware or some combination thereof.
[0036] As one example, one or more aspects of the present invention can be included in an article of manufacture (e.g., one or more computer program products) having, for instance, computer usable media. The media has embodied therein, for instance, computer readable program code means for providing and facilitating the capabilities of the present invention. The article of manufacture can be included as a part of a computer system or sold separately.
[0037] Additionally, at least one program storage device readable by a machine, tangibly embodying at least one program of instructions executable by the machine to perform the capabilities of the present invention can be provided.
[0038] The flow diagrams depicted herein are just examples. There may be many variations to these diagrams or the steps (or operations) described therein without departing from the spirit of the invention. For instance, the steps may be performed in a differing order, or steps may be added, deleted or modified. All of these variations are considered a part of the claimed invention.
[0039] While the preferred embodiment to the invention has been described, it will be understood that those skilled in the art, both now and in the future, may make various improvements and enhancements which fall within the scope of the claims which follow. These claims should be construed to maintain the proper protection for the invention first described.
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A method for use of a diagnostic software tool that can allow software developers to track the number of times each memory block is enlarged, and highlight the most frequently enlarged memory blocks. In this regard, in better understanding the performance characteristics of memory reallocation a developer can use this method to identify and implement better coding techniques to improve code efficiency and reduce the processing time utilized for memory reallocations. In addition, graphs can be generated to indicate the time/CPU utilization dedicated to the memory reallocation process.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention concerns an alloplastic material for producing an artificial soft tissue component and/or for reinforcing a natural soft tissue component, for example a ligament, a tendon or a supporting tissue of a human or animal body.
The alloplastic material may be used in medicine and surgery, and be implanted into a human or animal body. In the following the term `body` will frequently be used to mean `human or animal body`. Similarly, the term `bundles` referring to components of the alloplastic material, will frequently be used to mean `one or more bundles`. The invention equally concerns a method for producing the alloplastic material of the invention.
2. The State of the Art
Artificial ligaments and tendons made of bundles interwoven or plaited, and consisting of plastic fibers or of carbon fibers coated with a substance absorbable inside the body are known in the art. The plastic fibers used for the purpose have been of thicknesses between 20 and 30 micrometers, whereas the carbon fibers used have been from 7 to 8 micrometers thick. Attention is called in this connection to the article titled "Implantatmaterialien fur den alloplatischen Bandersatz" by L. Claes, C. Burri and R. Neugebauer, which appeared in the 5th Series of Lectures of the Work Committee for Implants (5.Vortragsreihe des Arbeitskreises Implantate) dated Nov. 13, 1984, page 193 of the Deutscher Verband fur die Materialprufung e.v. Fibers made of plastic materials are subject, however, to strong aging effects within the body, probably caused, at least in part, by their absorbing water from body fluids. As time goes on, the plastic fibers may undergo the phenomenon known as creep, involving a slow change in length, a reduction in strength or mechanical resistance, and brittleness. The mechanical properties of carbon fibers used at present predominantly for implants are strongly non-isotropic, due to the graphitic structure of carbon. Bending loads or stresses with small radii of curvature, or even relatively slight shearing stresses, may cause fibers to fracture. This is confirmed by the cited publication of Claes et al. Furthermore, carbon fibers have only low ductility and tend to crumble, particularly if their coats have been dissolved after a longer stay inside the body.
SUMMARY OF THE INVENTION
It should therefore be apparent, that the art is still in need of an alloplastic material for producing an artificial soft tissue component and/or for reinforcing a natural soft tissue component, as well as of a method for producing the alloplastic material, which are not associated with the aforementioned drawbacks and limitations of the state-of-the-art proposals.
It is therefore a primary object of the invention, to provide a novel alloplastic material for making an artificial soft tissue component and/or for reinforcing a natural soft tissue component, for example a ligament, a tendon or a supporting tissue of a human or animal body, as well as a method for producing the alloplastic material, which is not associated with the drawbacks and limitations of the prior art as heretofore discussed and which effectively and reliably fulfills an existing need in the art.
Another and more specific object of the invention is to provide a novel alloplastic material which is to avoid the disadvantages of known materials and which, in particular, is capable of resisting bending stresses resulting from bending to small radii of curvature as well as relatively large shear stresses, and which is able to preserve its mechanical strength and flexibility even if it remains in a human or animal body for a relatively long duration.
The foregoing and other objects are attained in accordance with some aspects of the invention by providing an alloplastic material which comprises fibers of a thickness less than 20 micrometers containing a metallic material.
Further objects of the invention are attained by providing a method for producing an alloplastic material comprising steps in which a number of wires corresponding to the number of wires to be formed are embedded into a matrix consisting of a metallic material different from the metallic material of the fiber, the wires together with the matrix are made longer and thinner by deformation and subsequently the matrix is dissolved by means of an acid to yield a bundle of fibers.
A few advantages of the invention will be described in the following.
The alloplastic material may comprise one or more bundles or, by preference, two or more bundles of fibers. One such bundle may contain a number of fibers within the range of 200 to 1000, or even up to 3000.
The fibers belonging to one bundle should be preferably held together loosely, in the relaxed state of the alloplastic material not yet implanted into the body, to generally have clearance spaces between adjacent fibers. The term `generally` is meant to imply, that fibers, at least at longitudinal sections, having sums amounting to a substantial part, such as more than 60%, and preferably 80% of the entire fiber length, are separated from the nearest neighbouring fiber by a clearance space. However, at some places, for example at places at which the bundles are bent to small radii of curvature, as at the longitudinal edges of a plaited ribbon, the fibers may touch each other in pairs or groups. As an alternative, the fibers of a bundle may run parallel to the longitudinal axis of the bundle or be wound around this axis. In the latter case, the pitch of the fibers in the bundle may be equal to from 5 to 10 times, or more, the diameter of the bundle.
In preferred embodiments of the alloplastic material, the fibers have a plane zigzag- and/or wave-shape, and/or a 3-dimensional helix-shape. If a single fiber bundle is involved, this bundle may be zigzag-, wave-,or helix-shaped. If, as is generally the case, two or more fiber bundles are provided, for example from 8 to 20, then the bundles may be mutually connected, in a loose manner, by plaiting, knitting, weaving or twisting. As an alternative, several types of connections may be combined with each other. These methods of connection may lend the bundles their zigzag-, wave-, or helix-shapes, while mutually supporting each other along their entire length, in regular intervals or without interruptions. Instead, two or more bundles may run zigzag-, wave-, or helix-shaped adjacent to each other, along parallel axes, and be fastened at their ends to common fastening members, but for the rest unconnected.
The alloplastic material may have an elongated shape, a shape suited for making an artificial tendon or an artificial ligament. If it possesses a defined longitudinal direction, then the alloplastic material may have to advantage the central axis of the zigzag- or wave-line, or the helix formed by respective bundles to run parallel to the defined longitudinal direction. In this way, at least the bundle sections forming, in regards to length the largest part of each fiber bundle, will form an angle with this longitudinal direction. It is of course possible, to produce areal fiber formations, that do not necessarily have a defined longitudinal direction, but rather a contour of polygonal or roundly shape, suited for making pieces of a supportive tissue, such as the diaphragm, or pieces of a membrane, or pieces of an inner or of an outer skin or membrane.
The fibers or, if they are provided with a non-metallic case, their cores, comprise a metallic material with at least one metal, and, in a preferred embodiment, may consist of an alloy, which, in addition to titanium as base metal, also contains one or more of the metels niobium, tantalum, zironium, chromium, molybdenum, iron and aluminum. The percentage by weight of titanium in the alloy should be the largest, and generally have a value of 50% or more. Furthermore, not considering any impurities that might be present, the fibers should preferably not contain any other metals than titanium and the alloy components mentioned before.
Titanium is reactive toward oxygen. Thus, if a fiber consisting of a titanium alloy is placed into an oxidizing environment containing free or bound oxygen, where it subjected to the action of oxygen from the air or from the inside of a human or animal body, such as oxygen present in electrolytic body fluids, then a compact film-like metal oxide layer, specifically TiO 2 , if the fiber contains titanium, will be generated on the outside surface of the fiber. An oxide layer of this kind provides good protection against corrosion to the metal underneath. The protection of the oxide layer is effective against chemical influences too, which may come from the fluids and other natural substances of a body and act upon an alloplastic material implanted into such a body. Investigations carried out on titanium parts implanted into the body have shown, that the oxidation reaction is very slow and proceeds even in a layer close to the metallic surface at a rate of oxidation of about 2×10 -5 micrometers/day only. Thus, based upon the aforementioned rate of oxidation, the degradation require a least 50,000 days i.e. at least 137 years to accomplish the removal of 1 μm. The actual time required for the oxidation is, however, substantially longer, because the surface layer of oxide protects the metal underneath against corrosive effects, and specifically against oxidation too, and thus slows down the progress of the oxidation. Therefore, with a typical diameter of the fibers of 10 to 15 μm the degradation by oxidation will have practically no effect. A similar situation exists in regards to the possible alloy components niobium, tantalum, chromium and aluminum, which are similarly reactive with respect to oxygen. Iron, also a possible alloy component, is corrosion-resistant, at least as a component of titanium-based alloy. Moreover, titanium and the aforementioned alloy metals show no toxic effects when implanted into the body. Thus, titanium and the titanium-based alloys are biologically inert and not toxic, and correspondingly produce no tissue reactions. Moreover, the surface metal oxide layer is effective to electrically insulate the metal below against the bodily tissue.
Titanium and the named titanium alloys also have good mechanical strength and a comparatively low modulus of elasticity. This latter property is of particular advantage, because it keeps stresses resulting from bending loads low. Titanium belongs to the metals of the alpha-type. Titanium alloys have various phase structures, depending on their compositions, and correspondingly belong to the alpha-type, the alpha-beta-type, or the beta-type. The TiNbTaAl-alloy containing 3% by weight niobium, 1% by weight tantalum, 6% by weight aluminum and the rest titanium, belongs for example to the alpha-type. Other alloys of the alpha-beta-type include for example the TiAlFe-alloy containing 5% by weight aluminum, 2.5% by weight iron and the rest titanium, and the TiNbAl-alloy containing 7% by weight niobium, 6% by weight aluminum and the rest titanium. Alloys of the beta-type are the TiNb-alloy containing 40% by weight niobium and the rest titanium, and the TiMoZrAl-alloy containing 15% by weight molybdenum, 5% by weight zirconium, 3% by weight aluminum and the rest titanium. The modulus of elasticity typically lies at 100 to 120 GPa for titanium, the alloys of the alpha-type and of the alpha-beta-type, and at about 65 to 110 GPa for the alloys of the beta-type, the exact values being dependent upon the heat treatment applied. The alloys of the beta-type have a cubic structure and as a feature shared to some extent by the alloys of the alpha-beta-type they display larger plastic deformability than titanium and than the alloys of the alpha-type having hexagonal structure. In consequence, the alloys of the alpha-beta-type and, above all those of the beta-type display more advantages than the materials of the alpha-type. Moreover, the mechanical strength of the alloys of the beta-type may be increased by heat treatment such as annealing, in particular solution annealing, and/or aging.
Subsequent to having been made, the metallic fibers display a relatively rough surface. This rough surface structure makes a good adherence of the bodily tissue possible, which tissue grows interpenetratingly into the alloplastic material implanted into the body. The interpenetrating growth of the connecting tissue may be improved, however, by the additional measures of enclosing the metallic formation and/or the bundles consisting of this formation and/or the formation consisting of the totality of several bundles, into an organic substance that may be absorbed inside the body, specifically, by the body fluids. Organic substances suited for this purpose, and which may be absorbed by the body within a few days are collagen, polyglactin, polylactate and gelatin.
The fibers should not be stressed beyond the elastic limit even if an alloplastic material containing the fibers runs over a sharp edge inside the body, or is strongly bent for other reasons. It was found that this condition can be fulfilled, by keeping the value of the so-called critical radius of curvature r c at less than 1 mm, and by preference at less than or approximately at 0.5 mm. In this context, the term critical radius of curvature r c is meant to refer to the smallest radius of curvature, to which the fibers may be bent, without any fracture occurring. If the fibers are circular in cross-section and are of diameter d, and if the fiber material has a modulus of elasticity E and a maximum allowable tension stress σ z , it can be shown, that the critical radius of curvature may be expressed by the formula: ##EQU1## For cold-formed titanium, for example, the allowable tension stress has a value σ z =0.9 GPa and the modulus of elasticity a value of E=105 GPa. For a cold-formed TiNb-alloy containing the percentages by weight specified before, the corresponding values are σ z =0.88 GPa and E=69 GPa. If a critical radius of curvature of 0.5 mm is assumed, there results for titanium a fiber diameter of about 9 micrometers and for the named TiNb-alloy a fiber diameter of about 13 micrometers. If the maximum allowable tension stress is replaced in formula (1) by the lower allowable fatigue stress corresponding to repeated application of bending loads, then the corresponding fiber diameters must be further reduced by about 40%.
If the fibers are circular in cross-section, their thickness, i.e. their diameter, should be in the range of at least 5 and less than 20 micrometers. If the fibers are coated with an organic substance, the specified fiber thickness is meant to refer to the thickness in the uncoated state, i.e. the thickness of the metallic cores of the fibers. Rather than having the preferred circular cross-section, the fibers may have, as an alternative, a different, roundly cross-sectional shape, that deviates more or less from the circular cross-section. In such a case, the fiber thickness is meant to refer to the maximum cross-sectional dimension of the uncoated fiber.
If the alloplastic material is implanted into the body, then the loose structure of the material will enable the body fluids to penetrate between the fibers and to make natural body tissue interpenetratingly grow between the fibers. If the fibers consist of titanium or of a titanium-containing alloy, then TiO 2 will be generated on the outer surfaces of the fibers, as described before. Hydroxide ions, radicals with a hydroxyl-group and radicals with an amino-group can readily deposit on these outer surfaces. Titanium and its named alloys therefore display bioactive behaviour. This is intended to mean, that after the alloplastic material has been implanted into the body, the titanium and its alloys will enable and encourage an intimate bond between the fibers and the natural, soft tissue and perhaps the solid bone substance. There will result, so to speak, a composite material consisting of alloplastic material and of natural tissue, the latter assuming the function of a matrix. If, in spite of the good pliability of the fibers, one individual fiber of the alloplastic material should break, then the natural soft tissue that fixedly adheres to the respective fiber will be able, by itself, to transmit the force onto the neighbouring fibers and, evidently, to bridge over the place of fracture. The force of adhesion by which the natural body tissue fixedly adheres to the outer surface of the fibers, is equal to the product of the outer surface of the fiber times the adhesive stress σ h . By defining the critical shearing and tear-out length L as a specific length of a section of a fiber, at which the adhesive force is equal to the fracture stress of the fiber, said length L may be expressed as ##EQU2## Experimental tests referring to the adhesion of bones to rough titanium surfaces, yielded adhesive stresses of 3 MPa. Assuming that the adhesive stress for soft tissues has about the same value, there results for titanium fibers of a diameter of 13 micrometers, a critical tear-out length of about 1 mm, or slightly less. If, as mentioned before, the fiber diameter d has a value less than 20 micrometers and, for example, between 5 and 15 micrometers, it is possible to obtain, on the one hand, a sufficiently small critical radius of curvature, and on the other hand, a tear-out length L clearly larger than the distance between adjacent fibers in a bundle of fibers loosely held together. This last feature contributes, should a fracture of an individual fiber take place, to a good transmission of force from the fractured fiber onto the adjacent fibers.
If natural, human or animal tissues, such as ligaments, fasciae, and tendons are stretched to the point of fracture and the applied tension force is plotted as a curve, then the slope of the curve will increase at the beginning and remain constant thereafter, until the curve flattens out and subsequent to reaching the ultimate tension stress, i.e. the maximum tension force before fracture, it will slightly fall off. On the other hand, if an individual metallic fiber is stretched, the corresponding curve will rise linearly from the beginning, until the region of plastic deformation is reached and the slope of the curve will slightly decrease, but will remain positive until fracture occurs. Irrespective of these different forms of the curve, the mechanical strength and elongation properties of the metallic fibers strongly differ, quantitatively too, from the corresponding properties of natural tissues. Whereas the modulus of elasticity of natural tissues, tendons and ligaments, lies in the range of 0.5 to 1.8 GPa in the linear portion of the curve, the modulus of elasticity of the fibers of titanium has a value of 105 GPa, as already mentioned, and it lies between 65 and 120 GPa for the titanium alloys of the mentioned types. The maximum allowable tension stress has a value between 60 and 110 MPa for the named natural tissues, a value of 800 MPa for pure titanium, and a value between 800 and 1400 MPa for titanium alloys. Significant is, however, that natural, soft tissues of the mentioned kind may be typically stretched in the elastic region of deformation about 10%, and about 15% to fracture, whereas metallic fibers can only be stretched about 1% in the elastic region of deformation.
However, the fibers may be loosely interconnected in the way mentioned before and arranged to follow a zigzag-, wave-, and/or helix-shaped course. In the case of an alloplastic material comprising for example a defined longitudinal direction and serving for example for making a tendon or the like, the fibers may run at least generally obliquely to this longitudinal direction, and thus to the direction along which the alloplastic material is meant to transmit a tension force while in use. In the case of an areal alloplastic material destined to be made into a diaphragm, the fibers thereof may be arranged to run, at least in certain places, obliquely to the direction along which a tension force is to be transmitted while the alloplastic material is in use. The individual fibers will then be able to move relative to each other, during the deformation of the alloplastic material, to a limited degree. The alloplastic material will thus obtain a certain elasticity of form. This elasticity of form will be considerably increased after the alloplastic material has been inserted into the body, due to the fact that natural soft tissue, such as connecting tissue, will interpenetrate the clearance spaces between the fibers. By suitable design, one may achieve to have the alloplastic material, starting out from its relaxed state while changing the course of the fibers, stretched at least after it has been interpenetrated by natural tissue at least in one direction, by 5% or more, or even by 10 to 20%, without causing the fibers to undergo any plastic deformation worth mentioning, and evidently without any fiber fracture.
If the alloplastic material implanted into the body has been grown into or interpenetrated by natural tissue, there will form a composite material, the forces exerted onto this material being taken up in part by the metallic fibers, and in part by the natural tissue. In this case, the effective modulus of elasticity, at least in the initial phase of a stretching process, will be equal to the weighted average between the modulus of elasticity of the alloplatic material and the modulus of elasticity of the natural tissue, the weighting factors used for computing this weighted average being proportional to the share of the sum of the fiber cross-sectional areas and the share of the sum of the soft tissue cross-sectional areas in the total cross-sectional area of the composite material. Moreover, the loose structure of the alloplastic material makes it possible, to have the tension forces acting upon it be distributed relatively uniformly over many fibers. It is only when the form-elastic elongation of the composite material has been exhausted that the fibers themselves will begin to stretch to any extent worth mentioning, whereby then the modulus of elasticity will become larger. Thus, even though the metallic fibers and the natural tissue strongly differ from each other in regards to mechanical strength and deformation properties, it is nevertheless possible to use metallic fibers for making an alloplastic material, which, as a whole, particularly after it has been grown into or interpenetrated by natural, soft tissue, will yield a qualitatively similar relationship between tension stress and elongation, as the corresponding relationship of the originally provided natural tissue.
When making a strap- or hose-shaped plait, the plaiting angle, i.e. the angle between a fiber bundle and the longitudinal direction of the plait may, if a form-elastic extensibility of at least 10% is to be realized, have a value between 30° and 60° or, for example, between 40° and 50°, depending upon the density and the degree of space filling of the plait. If the alloplastic material comprises one single fiber bundle running zigzag- or wave-shaped within a plane, or several fiber bundles having such shape and running, at least to some extent, freely next to each other, and if a form-elastic extensibility of 5% to 10% or more is desired, then the ratio between the wave length and the wave height may have a value of about 4, or less. If one or each fiber bundle is by itself helix-shaped, then the ratio between pitch and diameter of the helix for achieving extensibility of 5 to 10% or more, may be for example of the order of magnitude of 6 or less.
It is possible, by mathematical analysis, to estimate the manner in which, in a composite material which consists of metallic fibres and of natural tissue that fills in the clearance spaces between the metallic fibers, the forces become distributed over the fibers and the natural tissue, as well as the kinds of forces that the fibers and the tissue are able to take up before fracture. These analyses show, that the natural tissue, if its share in the total volume of the composite material reaches a value between 90 and 99%, will take up at least the same share of the total force as will the fibers, and can take up at least a similar maximum force before fracture, as the fibers. This means that, for example, after implanting an alloplastic material to serve as an artificial ligament, so much material may interpenetratingly grow into the implanted ligament, that a new ligament consisting of natural tissue will arise, within which the alloplastic material will merely serve as guide frame for the interpenetrating tissue.
The total cross-sectional area of a fiber bundle and the ratio V between the sum of the cross-sectional areas of the fibers belonging to the same bundle and the total cross-sectional area of the bundle, may vary along the bundle. If, for fulfilling its intended role, an elongated, alloplastic material comprising one or several fiber bundles, is fastened at its ends onto parts of the body, then the fibers at these ends will evidently be additionally pressed together at the fastening places. Furthermore, the fibers may also become pulled together, if the alloplastic material, while used as artificial ligament or tendon is subjected to tension stress. If, subsequent to being implanted into the body, the alloplastic material is interpenetratingly grown into by natural tissue, the material may become deformed by this growing-in tissue, causing its total cross-sectional area to increase, for example. Even though the distances between adjacent fibers after the implantation will not be the same as those before implantation, the ratio between the total volume of the fibers and the total volume of the grown-in tissue, resulting after the natural tissue has grown into place, will still be largely influenced by the distances between fibers in the relaxed unstressed alloplastic material before implantation. In order to enable the alloplastic material to be sufficiently interpenetrated and grown into by natural tissue, it is likely to be of advantage to have the ratio V for the material, in relaxed state and before implantation, be not more than 0.5, by preference not more than 0.2 and for example not more than 0.1 or 0.01. These limit values should preferably be valid for the average value of the ratio V also, the term average value being meant to refer to the value of the ratio V averaged over the entire length of the fiber bundle of the relaxed and unfastened alloplastic material.
Metallic fibers having diameters less than 20 micrometers cannot be produced by methods used for manufacturing individual wires. Such fibers may, however, be produced in bundles, by inserting comparatively thick wires of preferably circular cross-section, in a number corresponding to the desired number of fibers in a bundle, and consisting of the same material as the material of the fibers to be made, into bores of a block consisting of a different metallic material than the fibers. The material of the block effective to function as a matrix, is to preferably be softer than the material of the fibers and to have a similar ductility in regards to elongation-deformations, as the material of the fibers. The matrix may consist for example of copper or of a copper-nickel alloy. The composite blank consisting of the matrix and the wires imbedded thereinto, may be stretched and reduced in diameter, in steps, by hot and/or cold deformation processes, such as pressing and/or rolling and/or drawing, to make the thickness of the wires decrease to the desired thickness of the fibers. At least the terminal part, or terminal phase, of the deformation process shall consist by preference of a cold forming process. The deformation may be carried out by hot-pressing and subsequent cold-drawing. In a deformation process of this kind effecting a reduction in the cross-section as well as a lengthening of the rough blank and of the wires, the volume of the blank and of the individual wires remains preserved. A similar method of deformation is known to be used in the manufacture of superconductors, in which fibers of a titanium-niobium-alloy are imbedded into a copper matrix. Whereas in the completed superconductors the matrix remains preserved as a component, when manufacturing fibers for an alloplastic material the matrix is dissolved after deformation, by means of an acid, such as nitric acid, not reacting with the fiber material.
As already explained, each fiber bundle of the completed alloplastic material should preferably be formed to follow a zigzag-, wave-, and/or helix-shaped course, while several bundles may be united to yield a plaited, knit or woven formation and/or a hose and/or a rope or a yarn. Such a shape of the fiber bundles may be implemented by means of a form-giving process, in which the fibers are subjected essentially to bending only and are not made any thinner or longer, or at least not significantly so, in contrast to the deformation they previously underwent, while they were being produced of wires. During this form-giving process, which takes place without any substantial reduction in cross-sectional area or elongation of the fibers, the fiber bundles may be twisted and/or, depending on the desire type of alloplastic material to be produced, formed as individual bundles zigzag-, wave-, or helix-shaped, and/or connected with other fiber bundles, in advance of dissolving the matrix, together with the same, or after matrix dissolution. If the twisting and/or plaiting and/or other formgiving of the fiber bundle is carried out before the dissolution of the matrix, then the rigid connection between the fibers and the matrix will guarantee that the fibers will be bent in the same way the matrix that surrounds them is bent, without breaking. The ductility and/or mechanical strength of the fibers may be additionally influenced in desired manner by heat treatment, such as annealing, for example soft annealing or solution annealing, and/or by aging. This heat treatment may be carried out after the fibers have been manufactured in a volume preserving and elongating reduction in cross-section, specifically before and/or concurrently with and/or subsequent to the dissolution of the matrix, as well as before and/or concurrently with and/or subsequent to the form-giving of fibers carried out, in the described manner, without any substantial elongation and reduction in cross-section. If the fibers consist for example of a titanium alloy of the beta-type, and particularly if, in addition, in the course of a multi-stepped deformation process serving for the manufacture of fibers by elongation and reduction in cross-section, a cold forming process is applied, at least in the terminal phase, then the strength of the fibers may be additionally increased by heat treatment, such as by solution annealing and/or aging. Furthermore, the fibers may be coated by means of one of the named organic substances. This coating-step may be carried out either subsequent to producing a fiber bundle, or only after the bundle has been formed to zigzag-, wave-, or helix-shape, and/or connected with other fiber bundles, but evidently after the matrix has been dissolved.
BRIEF DESCRIPTION OF THE DRAWINGS
The subject matter of the invention shall now be explained by making reference to embodiments shown in the drawing. There show:
FIG. 1 a plan view of an alloplastic material plaited into a plane strap,
FIG. 2 a schematic cross-section through part of a bundle of fibers drawn to a larger scale,
FIG. 3 a schematic end view of a hose-shaped alloplastic material,
FIG. 4 a schematic view of an alloplastic material comprising a helix-shaped bundle of fibers, and
FIG. 5 a schematic view of an alloplastic material comprising a zigzag- or wave-shaped bundle of fibers.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The alloplastic material 1 shown in FIG. 1 consists of an areal, single-layer strap and comprises a number of loosely interconnected mutually plaited bundles 3. Each bundle runs zigzag- or wave-shaped within a plane, the bundles being mutually connected at regular intervals over their entire length by the plaited formation. Each bundle 3 consists of fibers 5 loosely held together. In FIG. 1, the fibers 5 are shown only in two of the bundles, also the number of fibers is in reality substantially larger than shown in the drawing. Each fiber comprises at least one metallic material, namely titanium or a titanium-based alloy.
The bundles 3 form a plaiting angle θ of 45° with the longitudinal direction of the strap, and have a substantially circular cross-section of a diameter D. The fibers 5 are of circular cross-section of diameter d, as shown in FIG. 2. The fibers 5 of a bundle 3 are loosely twisted together, so that, in general, clearance spaces exist between adjacent fibers. However, the fibers may come in contact with each other in pairs or in groups in certain places, for example in places in which the bundles 3 are greatly curved, such as at the longitudinal edges of the strap. The fibers 5 are thus given the possibility to move relative to each other, generally transversely with respect to the longitudinal direction of the fibers and bundles, at least in the relaxed, unstressed state of the strap. Since the bundles 3 follow a bent or curved path, the loose structure of the fiber formation enables longitudinal sections of the fibers 5 to also move, within certain limits, relative to each other, in longitudinal direction of the fibers.
The distances between fibers nearest to each other may vary from place to place and from fiber to fiber. To be able to explain a few variables and notations it will now be assumed, that the distance between fibers nearest to each other has the value a for all fibers, this value to be interpreted, to advantage, as a mean value averaged in a suitable manner. The distance a must evidently be larger than the diameter d of the fibers. While drawing the FIG. 2 it was assumed that the fibers 5 are distributed, in a cross-section running transversely to the respective bundle 3, in a two-dimensional, regular, hexagonal lattice, and are located in the corners and the centers of continuously interconnected hexagons of uniform sizes. The average distance denoted by a, of the fibers nearest to each other is thus equal to the length of the side of a hexagon. If the assumption is made, that the fibers define a hexagonal lattice as illustrated in FIG. 2, and the ratio V is to have the value V hex , where `hex` stands for hexagon, then
V=V.sub.hex =0.906 d.sup.2 /a.sup.2 (3)
The fibers could also define, in places, a two-dimensional square lattice, i.e. they could be located within a cross-section lying transversely to the direction of the bundles, in the corners of continuously interconnected squares of uniform sizes. In this case, the ratio V would have the value V sq , where `sq` stands for square, and
V=V.sub.sq =0.785 d.sup.2 /a.sup.2 (4)
Thus if, for example, the diameter d and the ratio V are preselected, then the approximate value of the average distance a may be calculated or at least estimated using the formulas (3) and (4). In the case of FIG. 2, the ratio V has a value of about 0.1, and d/a correspondingly a value of about 0.3.
The alloplastic material 1 may be made by first producing bundles of fibers in accordance with the method described in the introduction, by subsequently twisting the bundles around, i.e. winding them around the longitudinal axis of the bundle, and by mutually plaiting the desired number of bundles. Instead, it is possible to twist the previously stretched composite wires containing a matrix consisting for example of copper, in addition to the fibers, and to mutually plait them, and to dissolve the matrix by means of an acid after the plaiting has been accomplished. Furthermore, the fiber bundles may be coated before or after being plaited and subsequent to dissolving the matrix, with an organic substance that may be absorbed later inside the body. This substance will then enclose the individual fibers, with the exception of those fiber sections that may be in direct contact with each other, there being no clearance spaces therebetween. As an alternative, the twisting or winding of the fibers of a bundle could be dispensed with, and instead the fibers of a bundle could run more or less parallel to the longitudinal axis of the bundle. Subsequent to plaiting the bundles, the fibers of the bundle will be held together by the plaited formation. If the fibers are made of a titanium alloy of the beta-type, their mechanical strength properties may be additionally improved by solution annealing and/or by aging, either before or after the fiber bundles have been plaited.
In order to make an artificial ligament or an artificial tendon, the strap-shaped alloplastic material 1 may be fastened with its ends on bones, when inserted into the body. To this effect, holes may be drilled into the bones and the fiber formation clamped fast on pins inserted into the holes, the pins too consisting of bone material. The natural, rigid bone material may then, in analogy to the soft tissue, grow to a certain extent onto the metallic fibers.
Tests were carried out producing rough blanks comprising 1800 wires made of a TiNb-alloy of the beta-type and containing 40% by weight niobium and the rest titanium, the wires being imbedded into a matrix of copper. The rough blanks were converted by hot-pressing and cold-drawing, into composite wires having diameters of 0.8 mm, and lengths between 10 and 15 m, these lengths being subsequently cut to the desired lengths. The fibers remaining after the copper matrix has been dissolved, had diameters between 12 and 13 micrometers. The fibers present in a bundle thus had a total cross-sectional area of about 0.22 mm 2 . The tensile strength of the bundles were between 150 and 200 N per bundle. An alloplastic material was constructed by plaiting 18 bundles together to form a strap having a tensile strength of about 3 kN. This is significantly higher than the tearing stress of a natural knee-ligament.
In analogous manner were constructed fiber bundles of an alloy of the beta-type containing 15% by weight molybdenum, 5% by weight zirconium, 3% by weight aluminum and the rest titanium. This alloy is similar to the TiNb-alloy in showing good deformability without any disturbing stiffening effects. The fiber bundles were subjected, before dissolving the matrix, to a heat treatment at about 500° C. Tearing tests yielded ultimate stress values as high as 1.4 GPa.
If an alloplastic material to serve as artificial ligament or as artificial tendon is implanted into the body, there will form, after a certain amount of time, a matrix of natural soft tissue interpenetrating the fibers 5, enclosing the same and adhering to them. This soft tissue will be equally stretched when the fiber formation 1 is stretched, while the forces will become distributed onto the fiber formation 1 and the natural soft tissue. When the length of an individual piece of fiber on which natural soft tissue has adhered is at least equal to the critical tear-out length L defined in the introduction, then the shearing force required for shearing the natural soft tissue off the fibers, is larger than the fracture stress of the fiber when subjected to tension. According to formula (2), the critical tear-out length of fibers made of the named titanium-niobium-alloy and having diameters between 12 and 13 micrometers lies between 0.6 and 1 mm. This is, compared to the length of common ligaments and tendons, too short, so that the natural soft tissue, as soon as it has grown into a short part of the alloplastic material, will be able to compensate for unequal stresses in the fibers and, if a fracture occurs in one fiber, it will be able to transfer the force transmitted by the respective fiber, onto the neighbouring fibers. If the ratio V, i.e. the share of the total cross-sectional area of the fibers 5 of a bundle 3 in the total cross-sectional area of the bundle grown into by natural tissue, has a value of 0.1 for example, so that a ratio approximately corresponding to the ratio shown in FIG. 2 will result between the distances a of adjacent fibers and the diameters d, and the distances a will be on the average about 0.04 mm, then, on the one side, the distances a will still be substantially smaller than the critical tear-out length L, thus making possible a good transmission of force, and, on the other side, the volume of the additionally grown natural tissue will be large enough, to enable this tissue to fulfill the full function, so to speak, of a ligament or a tendon.
The embodiment of the alloplastic material 11 illustrated in FIG. 3 comprises a number of fiber bundles 3, the individual bundles being mutually plaited to form a hose. The plait is preferably constructed to have all of the bundles 3 form helices running around the longitudinal axis of the hose with identical pitch, one half of the bundles being arranged to run like a right-handed screw-thread and the other half like a left-handed screw-thread.
The alloplastic material 21 shown in FIG. 4 also comprises at least one helix-shaped bundle 3 of, for example, slightly twisted fibers. However, in this case the bundle 3 is not plaited with any other bundle, but may be connected at its ends with other bundles, by means of fastening members not shown in the drawing, and is thus left free over the largest part of its length. The pitch S is larger than the average diameter D w of the helix and, for example, has a value of approximately 6 D w or less.
The alloplastic material 31 shown in FIG. 5 comprises a fiber bundle 3 that runs zigzag-, and/or wave-shaped within a plane. The wave-length L w is larger than the wave height H of the bundle, as measured between center axes of the bundle, and has a value of approximately 4H or less. If several bundles are provided, these should be connected, at the utmost, at their ends, by way of common fastening members.
The helix- or wave-shaped bundle according to the FIGS. 4 or 5, respectively, may be manufactured by subjecting a bundle of wires of titanium or a titanium alloy imbedded into a matrix, to deformation, in the manner described in the introduction, until the wires acquire the desired diameters. The composite wire resulting in this way may then be formed into a helix-shape or a wave-shape, as the case may be. The matrix may then be dissolved by means of an acid.
While there are shown and described present preferred embodiments of the invention, it is to be distinctly understood that the invention is not limited thereto but may be otherwise variously embodied and practiced within the scope of the appended claims.
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The alloplastic material comprises bundles of metallic fibers loosely held together. The fibers preferably consist of a titanium-based alloy containing at least one of the metals niobium, tantalum, zirconium, chromium, molybdenum and aluminum, and may be provided with a coat of an organic substance selected to be absorbed inside a human or animal body. On the outer surfaces of the fibers consisting of the named alloy there may arise layers of oxides effective to protect the metal beneath against chemical influences taking place in the body. Moreover, the metals present in the fibers in the form of alloy components are not toxic and enable a good bond with natural tissue to take place. Without the optional coat, the fiber thickness has a value of less than 20 micrometers and preferably 15 micrometers or less. Thus, subjecting the fibers to bending, as takes place with alloplastic material inside the body, will not cause any fatigue fractures.
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CROSS-REFERENCE TO RELATED APPLICATIONS
Not applicable.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not applicable.
BRIEF SUMMARY OF THE INVENTION
When displayed, greeting cards are typically organized on a display fixture that has multiple rows or levels upon which to sit the cards. Each row may have a front piece that holds in the card, yet is transparent or short enough to still view at least a portion of the greeting card. Because display fixtures are manufactured to have a specified amount of rows or levels at a specified depth, in order to adjust the specifications of a display fixture, other pieces must be used, for example, attaching a separate divider to the display fixture to add another level or tier between a set row of the display fixture. By providing another row using a dividing piece, another set of greeting cards may be displayed between cards already displayed on adjacent rows of the original display fixture, thereby increasing the density of the overall display. However, when an extra row is not desired, the dividing piece must be removed from the display fixture and stored elsewhere. This presents problems with storage and may result in a loss of the divider.
In one embodiment of the present invention, a card assembly apparatus for displaying multiple rows of greeting cards is provided. The apparatus comprises, in part, a display section with a back piece, one or more rows, and one or more front pieces, where a greeting card is placed on a row and portions thereof can be viewed through and/or above the front piece. The apparatus further comprises a collapsible row having a front divider and bottom divider attached at a joint. The joint permits movement of the collapsible row between a use or display position and a storage or non-use position. In the display position, the front divider is pulled out away from the display fixture, such that the bottom divider is perpendicular to the back piece. This allows for a greeting card to be supported for display on the bottom divider. In the storage or non-use position, the joint allows the front divider to be pushed against the back piece, such that the bottom divider is setting against the back piece. The apparatus also includes a divider clip that hooks on the front piece of the display section to separate cards and assist with maintaining the collapsible row in the display position.
In yet another embodiment, a collapsible row for use with a display section for displaying greeting cards is provided. The collapsible row comprises, in part, a front divider, a bottom divider, and a joint connecting the front and bottom dividers. The joint allows the collapsible row to be moved between a display position, where the front divider is pulled out away from a display section such that the bottom divider is perpendicular to the back of the display fixture to allow for a greeting card to be displayed on the bottom divider, and in a non-use position, where the front divider can be pushed against the back of the display section such that the bottom divider is setting against the display section.
In still another embodiment, a divider or support clip for separating greeting cards within a row of a display fixture and supporting a collapsible row is provided, in accordance with an embodiment of the present invention. The divider clip includes, in part, a clipping mechanism to attach the divider clip to the display fixture and an adjustable portion capable of adjusting itself to support a collapsible row used in the display fixture.
BRIEF DESCRIPTION OF THE DRAWINGS
The features of the invention noted above are explained in more detail with reference to the embodiments illustrated in the attached drawing figures, in which like reference numerals denote like elements, in which FIGS. 1-7C illustrate several possible embodiments of the present invention, and in which:
FIG. 1 is a front perspective view of an exemplary card display fixture with a plurality of divider pieces, in accordance with an embodiment of the present invention;
FIG. 2 is a cross-sectional side elevation view of the card display fixture with a plurality of divider pieces of FIG. 1 taken along the line 2 - 2 ;
FIGS. 3A and 3B are enlarged, fragmentary views taken generally in the areas 3 A and 3 B of FIG. 2 and illustrate the cooperation between the divider piece and a clip;
FIG. 4A is a perspective view of a dividing clip constructed in accordance with a first embodiment and illustrated in an open or support position;
FIG. 4B is a side elevation view of the dividing clip of FIG. 4A in a hooked position;
FIG. 5 illustrates a second possible embodiment of a dividing clip of the present invention;
FIGS. 6A-6C illustrate a third possible embodiment of a dividing clip of the present invention; and
FIGS. 7A-7C illustrate a fourth possible embodiment of a dividing clip of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring now to the drawings in more detail and initially to FIG. 1 , numeral 10 generally designates a card assembly apparatus constructed in accordance with an embodiment of the present invention. In this illustrated example, the apparatus 10 includes a display section or panel or tray 12 for coupling to and support on a display fixture (not shown). The display fixture may be any standard display fixture as is known in the art. As illustrated, the display section 12 includes two permanent levels 14 for displaying greeting cards 16 . As illustrated in FIG. 2 , each level 14 is defined by a ledge 18 , upon which an L-shaped row section 20 is supported. Each row section 20 includes a front wall 22 and a bottom wall 24 . Each front wall 22 is of a sufficient height to contain a greeting card 16 , while still allowing a portion thereof to be visible above the front wall 22 . Though not necessary, the row sections 20 , and in particular the front wall 22 , are preferably transparent, such that the full face of the cards 16 can be viewable. Each level 14 of the display section 12 also includes a rear wall 26 against which the greeting cards 16 would normally rest. The greeting cards 16 are supported on the bottom wall 24 of the row sections 20 .
To provide for the ability to change the display arrangement, the illustrated display section 12 also includes a plurality of convertible rows 28 that are capable of being moved between a use or display position and a storage or non-use position. As illustrated in FIG. 1 , the display section 12 includes four convertible rows 28 , two to form an upper row and two to form a lower row. Alternatively, single convertible rows 28 could run the width of the display section 12 , such that only two convertible rows 28 would be provided. As illustrated, the upper left convertible row 28 is provided in the display position, while the upper and lower right convertible rows 28 are in the storage position. The lower left convertible row 28 has been illustrated in FIG. 1 in a position close to the storage position.
Each convertible row 28 includes a front divider 30 and a bottom divider 32 . The front and bottom dividers 30 , 32 are connected by a joint 34 that permits the two dividers 30 , 32 to move relative to one another to create the two positions. In the display position, the front divider 30 is pulled out away from the rear wall 26 of the display section 12 . Such a position allows the bottom divider 32 of the convertible row 28 to be generally perpendicular to the rear wall 26 of the display section 12 , thereby providing another level or row to the overall display section 12 . Thus, in the configuration illustrated in FIG. 1 , the top row of the display section 12 is able to display greeting cards 16 at its set or permanent level 14 and additional greeting cards 16 on a level provided by the convertible row 28 . The front divider 30 of the convertible row 28 acts similarly to the front wall 22 of the row section 20 , and serves to support the greeting card 16 . The convertible row 28 will be further described herein below.
The display section 12 preferably also includes a plurality of divider or support clips 36 . In the prior art, divider clips are clipped on the front piece (e.g., front wall 22 ) of a card row to horizontally separate different types of greeting cards 16 . In the present invention, the divider clips 36 may also be used to support the convertible row 28 and maintain it in either the display or storage positions. Multiple embodiments of divider clips 36 of the present invention are illustrated and will be further described below.
When a convertible row 28 is no longer desired for use in displaying a row of greeting cards 16 , it may be collapsed and the pushed back against the rear wall 26 , as illustrated by the convertible rows 28 on the right side of the display section 12 of FIG. 1 . The convertible rows 28 may be moved from the display position to the storage position by folding the convertible row 28 at the joint 34 and moving the front divider 30 back against the rear wall 26 . This position and alternate embodiments are described in more detail below.
Turning now to FIG. 2 , a cross-sectional, side elevation view of the card assembly apparatus 12 in FIG. 1 is shown. In this view, two convertible rows 28 are shown. The upper convertible row 28 is illustrated in the display position, with the bottom divider 32 generally perpendicular to the rear wall 26 . As will be further discussed below, a proximal edge 38 of the bottom divider 32 of the convertible row 28 is rotatably received in a horizontal channel 40 in the rear wall 26 of the display section 12 . The bottom divider 32 of the convertible row 28 supports the greeting card 16 , thereby providing another row to the set permanent row or level 14 immediately below that is also displaying a greeting card 16 . A portion of that greeting card 16 is displayed over the front wall 22 and a top edge 42 thereof rests against the front of the front divider 30 of the upper convertible row 28 .
The upper divider clip 36 , which is adjacent to the upper convertible row 28 in the display position, is in its open or support position. A movable portion 44 of the divider clip 36 extends downward and provides support for the bottom divider 32 of the convertible row 28 . This serves to stabilize and support the convertible row 28 when displaying greeting cards 16 .
The lower convertible row 28 of FIG. 2 is illustrated in the storage position. The bottom divider 32 of the convertible row 28 has been rotated downwardly and moved to an orientation where it is closer to parallel to the rear wall 26 of the display section 12 , thereby allowing the convertible row 28 to collapse and rest against the back of the permanent row or level 14 . By being collapsible, the convertible row 28 , when not desired for displaying an additional row of cards 16 , does not need to be removed from the display section 12 . Such a configuration thus avoids the need to remove a divider and store it until an additional row is needed. Here, in the bottom portion of FIG. 2 , only the set row of the display section 12 , formed by the row section 20 , is being used for displaying a greeting card 16 .
When the convertible row 28 is in the storage position, the divider clip 36 adjacent to it is adjusted so that it presses against the convertible row 28 , holding it in place against the rear wall 26 of the display section 12 . Note that a divider clip 36 may be used adjacent a convertible row 28 whether it is in the display or storage position, and is adjusted accordingly As will be discussed in greater detail below, an adjustable divider clip, such as divider clip 36 , allows for more flexibility when determining which position a convertible row 28 is to be used. One skilled in the art will appreciate that various embodiments of divider clips may be used, and will be discussed in more detail below.
Referring now to FIGS. 3A and 3B , enlarged views of the divider clips 36 from FIG. 2 are provided, in accordance with embodiments of the present invention. In FIG. 3A , where the convertible row 28 is in the display position, the divider clip 36 is in its open or support position. The divider clip 36 has a body portion 46 with a notch 48 therein. The notch 48 is sized to receive an upper edge 50 of the front wall 22 of a row section 20 , as illustrated. The notch 48 may also receive the upper edge 50 of the front divider 30 if the divider clip 36 is placed on the convertible row 28 when it is in its display position to separate cards 16 placed thereon. The notch 48 may also include a raised rib 52 therein to assist with retaining the divider clip 36 on the front wall 22 or front divider 30 , as the case may be. While a notch 48 has been shown, one skilled in the art will appreciate that any method of attaching the divider clip 36 to the front of the display section 12 may be used in accordance with this invention.
The body portion 46 is connected with the movable portion 44 via an arm 54 . The arm 54 is preferably flexible such that it may be bent between the illustrated support and hooked positions. In that regard, the divider clip 36 may be made of a plastic and formed by a molding process. In such an arrangement, the arm may be naturally biased to a position intermediate the illustrated support and hooked positions. In this way, the arm 54 provides lift and secure engagement to the convertible row 28 when it is in the support position.
To assist with secure engagement with the convertible row 28 , the movable portion 44 is provided with a nock 56 in its outer periphery 58 . The nock 56 is intended to receive a lower edge 60 of the front divider 30 of the convertible row 28 , as illustrated in FIG. 3A . In this arrangement, the clip 36 holds the convertible row 28 in the display position by preventing downward and rearward movement of the front divider 30 . Downward pressure on the bottom divider 32 , caused by the weight of the front divider 30 and any greeting cards 16 placed in the convertible row 28 , is transferred through the clip to the front wall 22 . Further, the body portion 46 spaces the front divider 30 from the front wall 22 and prevents forward rotation of the front divider 30 .
To further prevent unintended movement of the convertible row 28 from the display position to the storage position, friction arrangement is provided. In that regard, the proximal edge 38 of the bottom divider 32 is provided with a generally cylindrical tube portion 62 . The tube portion 62 has a longitudinal slot 64 therein adjacent a stop flange 66 . When the tube portion 62 is received in the channel 40 of the rear wall 26 of the display section 12 , a longitudinal ridge 68 is received in the slot 64 when the bottom divider 32 is in a generally horizontal position, as illustrated in FIG. 3A and which corresponds with the convertible row 28 being in its display position. The ridge 68 in the slot 64 discourages rotational movement of the tube portion 62 in a direction where the ridge 68 is moved out of the slot 64 , as such requires the tube portion 62 to be compressed, as illustrated in FIG. 3B . This is helpful when the convertible row 28 is first placed in the display position before the divider clips 36 can be hooked on to the bottom of the convertible row 28 . The stop flange 66 discourages rotational movement of the tube portion 62 in a direction past that needed for the display position.
In FIG. 3B , where the convertible row 28 is in the storage position, the divider clip 36 is in its hooked position. In this position, the arm 54 is generally perpendicular to the rear wall 26 of the display section 12 and preferably presses against the convertible row 28 to keep it collapsed and in the storage position. To maintain the divider clip 36 in the hooked position, the divider clip 36 , in this embodiment, includes a projection 70 that extends outwardly from a side of the arm 54 and is received in an aperture 72 of a tab 74 that extends from the body portion 46 of the divider clip 36 , as best illustrated in FIGS. 4A and 4B . Alternate embodiments of divider clips are illustrated and will be described below.
FIGS. 4A and 4B illustrate alternate views of the first embodiment of the divider clip 36 . In this illustrated embodiment, the divider clip 36 comprises a singular piece of material. FIG. 4A shows the divider clip 36 is in its open or support position that corresponds with the convertible row 28 being in the display position, as discussed above. FIG. 4B shows the divider clip 36 is in its hooked position that corresponds with the convertible row 28 being in the in a storage position. As can be seen, the projection 70 is received in the aperture 72 to secure the movable portion 44 in a location to abut the front divider 30 of a convertible row 28 to maintain it in a storage position.
The divider clip 36 may also be provided with a recess portion 75 in the body portion 46 adjacent to and of a corresponding shape as the notch 48 . As illustrated in FIG. 4A , the notch may be part of a clipping member 77 that extends laterally outward from the body portion 46 . The recess portion is adjacent a proximal end 79 of the clipping member and is designed to receive a distal end 81 of a clipping member 77 of another divider clip 36 placed adjacent thereto. This arrangement allows for a plurality of divider clips 36 to be coupled together for easy storage and to support the ease/speed of installation of the divider clips 36 during a reset/conversion of a display or a reduction/increase in the number of rows.
Referring now to FIG. 5 , an alternative embodiment of a divider clip 36 is illustrated, in accordance with the present invention. The divider clip 36 has a body portion 76 with a clipping member 78 for attaching the divider clip 36 to a front wall 22 or front divider 30 . The divider clip further includes an adjustable portion 80 , which connects to the body portion 76 of the divider clip 502 via a bend 82 . The bend 82 functions similar to the arm 54 and biases the adjustable portion 80 to the position illustrated. The divider clip 36 further includes a hook 84 extending from a lower portion of the body potion 76 and having a notch 86 .
In this embodiment, the divider clip 36 is illustrated in a position for use when the convertible row 28 is in the storage position. The adjustable portion 80 extends away from the body portion 76 of the divider clip 36 to press against the front divider 30 , which itself rests against the rear wall 26 of the display section 12 , as described above. When a convertible row 28 is used in the display position, the bend 82 will flex, and the adjustable portion 80 will be moved back into a correspondingly shaped cutout 88 . The lower edge 60 of a front divider 30 will then rest or otherwise be secured in the notch 86 of the hook 84 .
Turning now to FIGS. 6A-6C , a third possible embodiment of a divider clip 36 is shown, in accordance with the present invention. Here, the divider clip 36 includes a fixed portion 90 and a rotatable portion 92 . These portions 90 , 92 are connected at joint 94 , about which the rotatable portion 92 pivots. The fixed portion 90 includes a clipping mechanism 96 for attaching the clip 36 to a front wall 22 or front divider 30 . When a convertible row 28 is in a display position, the divider clip 36 oriented to the position illustrated in FIGS. 6A and 6C , where the rotatable portion 92 is generally parallel to the fixed portion 90 . In this arrangement, a ledge 98 extends outwardly from a lower edge 100 of the rotatable portion 92 and is used to support the lower edge 60 of the front divider 30 of the convertible row 28 , as discussed above with respect to FIG. 3A . FIG. 6B illustrates the rotatable portion 92 rotated to be generally perpendicular to the fixed portion 90 , which is the position of the divider clip 36 when the convertible row 28 is in a storage position.
FIGS. 7A-7C illustrate a fourth possible embodiment of a divider clip 36 , where the divider clip includes two separate pieces: a clipping portion 102 , which includes a clipping mechanism 104 , and an adjustable portion 106 , which slides on the clipping portion 102 . Flaps 108 secure the fixed portion 102 against a back 110 of the adjustable portion 106 . When a convertible row 28 is in a display position, the divider clip 36 is oriented to the configuration illustrated in FIG. 7A . Here, both the clipping portion 102 and the adjustable portion 106 are generally parallel to each other. A ledge 112 extends outwardly from a lower edge 114 of the adjustable portion 106 and is used to support the lower edge 60 of the front divider 30 of the convertible row 28 , in a manner similar to that discussed above with respect to FIG. 6A . The ledge 112 thereby supports the convertible row 28 and works to maintain it in the display position. FIG. 7B illustrates how these pieces 102 , 106 fit together when used in connection with a convertible row 28 in the display position.
When the convertible row 28 is in a storage position, the divider clip 700 may be reconfigured to the arrangement illustrated in FIG. 7C . In this illustrated example, the adjustable portion 106 is secured to the clipping portion 102 by rotating it approximately 90° and receiving the clipping portion 102 in a transverse opening 116 in the adjustable portion 106 that is defined by the flaps 108 and sides 118 and 120 ( FIG. 7A ).
Many variations can be made to the illustrated embodiments of the present invention without departing from the scope of the present invention. Such modifications are within the scope of the present invention. For example, the convertible rows 28 can span the entire width of the display section 12 . Similarly, while the joint 34 is illustrated as constructed in the illustrated manner, other versions of the joint that permit movement between the front divider 30 and the bottom divider 32 (such as a hinge type mechanism) are possible and within the scope of the present invention. Additionally, the display sections 12 can be molded with features or apertures in the rear of the section to facilitate coupling of the display section 12 to a display fixture. It should be noted that the increase of the row depth when a convertible row 28 is collapsed allows for the display of product having an increased product depth. Further, while the present invention has been described in connection with the display of greeting cards, the present invention is not limited to such a narrow use. Non-card products can be displayed as well. Other modifications would be within the scope of the present invention.
From the foregoing it will be seen that this invention is one well adapted to attain all ends and objects hereinabove set forth together with the other advantages which are clear following the complete disclosure above and which are inherent to the methods and apparatuses described herein. It will be understood that certain features and subcombinations are of utility and may be employed without reference to other features and subcombinations. This is contemplated by and is within the scope of the invention.
Since many possible embodiments may be made of the invention without departing from the scope thereof, it is to be understood that all matter herein set forth or shown in the accompanying drawings is to be interpreted as illustrative of applications of the principles of this invention, and not in a limiting sense.
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When displayed, greeting cards are typically organized on a display fixture having multiple rows or levels upon which to sit the cards. Each row then has a front wall to hold in the card, yet is short enough to still view a portion of the greeting card above the wall. Because display fixtures are manufactured to have a specified amount of rows or levels at a specified depth, in order to adjust the specifications of a display fixture, other pieces may be used, for example, by attaching to the display fixture a convertible row to add another level or tier between set rows of the display fixture. By providing another row using a convertible row, another set of greeting cards may be displayed between cards displayed on other rows of the original display fixture, increasing the density of the overall display. Further, when an extra row is not desired, such a convertible row may be pushed flush against the back of the display fixture, while still attached, allowing the full depth of the row of the display fixture to be used.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This is a continuation of application Ser. No. 665,593, filed Mar. 10, 1976, and abandoned after the filing of this application. Application Ser. No. 665,593 was, in turn, a continuation-in-part of then copending application Ser. No. 438,156, filed Jan. 31, 1974, and issued Apr. 6, 1976, as U.S. Pat. No. 3,948,894.
BACKGROUND OF THE INVENTION
This invention relates to anti-inflammatory 5,6-diaryl-1,2,4-triazines. More particularly, this invention relates to topically-active anti-inflammatory 5,6-diaryl-1,2,4-triazines.
Inflammation is an essentially protective and normal response to injury, although the etiology and pathogenesis of many inflammatory conditions remain obscure. In general, anti-inflammatory agents are employed primarily to relieve the symptoms of inflammation. In such symptomatic therapy, topically-applied anti-inflammatory agents present special problems. Inflammatory conditions calling for the topical application of an anti-inflammatory agent are almost exclusively treated with steroids. Topically-applied steroids, however, may carry considerable systemic toxicity. Thus, the need continues for safer, better tolerated topically-active anti-inflammatory agents.
SUMMARY OF THE INVENTION
In accordance with the present invention, 5,6-diaryl-1,2,4-triazines are provided having the formula, ##STR2## wherein R is hydrogen or -(X) n R 1 , in which X is either O or S, n is an integer which is either 0 or 1, and R 1 is C 1 -C 8 alkyl, C 7 -C 8 aralkyl, C 3 -C 8 cycloalkyl, or C 4 -C 8 (cycloalkyl)alkyl; and R 2 and R 3 independently are C 1 -C 3 alkoxy or di(C 1 -C 3 alkyl)amino; with the proviso that when R 2 and R 3 both are methoxy, R cannot be H or methylthio; and the pharmaceutically-acceptable acid addition salts of basic members thereof.
The compounds of the present invention are useful as anti-inflammatory agents. In particular, all of such compounds are especially useful as topically-active anti-inflammatory agents in warm-blooded mammals, such as guinea pigs, mice, rats, dogs, monkeys, humans, and the like. In addition, those compounds wherein X is O or S and n is 1 are useful as intermediates in the preparation of anti-inflammatory 3-amino-5,6-diaryl-1,2,4-triazines which are disclosed an claimed in copending and commonly-assigned application Ser. No. 438,156, filed Jan. 31, 1974, by William B. Lacefield, now U.S. Pat. No. 3,948,894.
DETAILED DESCRIPTION OF THE INVENTION
The term "C 1 -C 8 alkyl" includes methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, tert-butyl, pentyl, isopentyl, 1-methylbutyl, 1-ethylpropyl, neopentyl, tert-pentyl, 1,2-dimethylpropyl, hexyl, isohexyl, 2-ethylbutyl, 1-ethyl-1-methylpropyl, heptyl, 2-ethyl-1-methylbutyl, 2,4-dimethylpentyl, octyl, 2-ethylhexyl, 1,1-diethylbutyl, and the like.
The term "C 7 -C 8 aralkyl" includes benzyl, 2-phenylethyl, p-methylbenzyl, m-methylbenzyl, o-methylbenzyl, and the like.
The term "C 3 -C 8 cycloalkyl" includes cyclopropyl, 2-butylcyclopropyl, cyclobutyl, 2-ethyl-3-methylcyclobutyl, cyclopentyl, 3-isopropylcyclopentyl, cyclohexyl, 1-methylcyclohexyl, 2,5-dimethylcyclohexyl, cycloheptyl, 5-methylcycloheptyl, cyclooctyl, and the like.
The term "C 4 -C 8 (cycloalkyl)alkyl" includes cyclopropylmethyl, 3-cyclopropyl-2-methylbutyl, 3-(2-methylcyclobutyl)propyl, 2-cyclopentylethyl, 2-methylcyclohexylmethyl, cycloheptylmethyl, and the like.
The term "C 1 -C 3 alkoxy" includes methoxy, ethoxy, propoxy, and isopropoxy. The term "C 1 -C 3 alkyl" includes methyl, ethyl, propyl, and isopropyl.
Illustrative of the triazine compounds which are provided by the present invention are the following:
5,6-bis(4-ethoxyphenyl)-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-1,2,4-triazine,
5,6-bis(4-dipropylaminophenyl)-1,2,4-triazine,
5-(4-diethylaminophenyl)-6-(4-methoxyphenyl)-1,2,4-triazine,
5,6-bis(4-methoxyphenyl)-3-methyl-1,2,4-triazine,
3-ethyl-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
5,6-bis(4-methoxyphenyl)-3-propyl-1,2,4-triazine,
3-isopropyl-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
3-tert-butyl-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
3-(1,2-dimethylpropyl)-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
3-heptyl-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-methyl-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-ethyl-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-propyl-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-isopropyl-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-hexyl-1,2,4-triazine,
3-ethyl-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
3-(1-methylbutyl)-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
3-neoheptyl-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
5,6-bis(4-isopropoxyphenyl)-3-methyl-1,2,4-triazine,
3-sec-butyl-5,6-bis(4-isopropoxyphenyl)-1,2,4-triazine,
5,6-bis(4-isopropoxyphenyl)-3-octyl-1,2,4-triazine,
5-(4-methoxyphenyl)-3-methyl-6-(4-propoxyphenyl)-1,2,4-triazine,
6-(4-ethoxyphenyl)-5-(4-isopropoxyphenyl)-3-(2,3,4-trimethylpentyl)-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-methyl-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-ethyl-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-propyl-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-isopropyl-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-isopentyl-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-(2-ethylhexyl)-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-methyl-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-ethyl-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-propyl-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-isopropyl-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-(2,2,3-trimethylbutyl)-1,2,4-triazine,
5,6-bis(4-dipropylaminophenyl)-3-methyl-1,2,4-triazine,
3-sec-butyl-5,6-bis(4-dipropylaminophenyl)-1,2,4-triazine,
5,6-bis(4-dipropylaminophenyl)-3-(2-ethylbutyl)-1,2,4-triazine,
5,6-bis(4-diisopropylaminophenyl)-3-ethyl-1,2,4-triazine,
5,6-bis(4-diisopropylaminophenyl)-3-tert-pentyl-1,2,4-triazine,
5,6-bis(4-diisopropylaminophenyl)-3-(2,2,4-trimethylpentyl)-1,2,4-triazine,
6-(4-diisopropylaminophenyl)-5-(4-dimethylaminophenyl)-3-neoheptyl-1,2,4-triazine,
5-(4-diisopropylaminophenyl)-6-(4-ethoxyphenyl)-3-methyl-1,2,4-triazine,
3-benzyl-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
5,6-bis(4-methoxyphenyl)-3-(m-methylbenzyl)-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-(2-phenylethyl)-1,2,4-triazine,
3-(1-phenylethyl)-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
5,6-bis(4-isopropoxyphenyl)-3-(o-methylbenzyl)-1,2,4-triazine,
3-benzyl-5-(4-methoxyphenyl)-6-(4-propoxyphenyl)-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-(p-methylbenzyl)-1,2,4-triazine,
5-(4-diethylaminophenyl)-6-(4-diisopropylaminophenyl)-3-(2-phenylethyl)-1,2,4-triazine,
3-benzyl-6-(4-diethylaminophenyl)-5-(4-ethoxyphenyl)-1,2,4-triazine,
3-cyclopropyl-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
3-cyclopentyl-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
3-cyclobutyl-5-(4-ethoxyphenyl)-6-(4-methoxyphenyl)-1,2,4-triazine,
3-cyclooctyl-5,6-bis(4-dimethylaminophenyl)-1,2,4-triazine,
5,6-bis(4-dipropylaminophenyl)-3-(2-ethylcyclopropyl)-1,2,4-triazine,
5-(4-diethylaminophenyl)-6-(4-dipropylaminophenyl)-3-(2-ethylcyclobutyl)-1,2,4-triazine,
3-cycloheptyl-6-(4-dipropylaminophenyl)-5-(4-methoxyphenyl)-1,2,4-triazine.
3-(2-cyclohexylethyl)-5,6-bis(4-ethoxyphenyl)-1,2,4-triazine,
3-cyclobutylmethyl-5,6-bis(4-isopropoxyphenyl)-1,2,4-triazine,
5-(4-ethoxyphenyl)-6-(4-isopropoxyphenyl)-3-(2-methylcyclohexylmethyl)-1,2,4-triazine,
3-cyclopropylmethyl-5,6-bis(4-diethylaminophenyl)-1,2,4-triazine,
5,6-bis(4-dipropylaminophenyl)-3-[2-(2-methylcyclobutyl)ethyl]-1,2,4-triazine,
3-cycloheptylmethyl-5,6-bis(4-diisopropylaminophenyl)-1,2,4-triazine,
3-(1-cyclohexylethyl)-5-(4-diethylaminophenyl)-6-(4-dimethylaminophenyl)-1,2,4-triazine,
3-cyclopentylmethyl-5-(4-diethylaminophenyl)-6-(4-ethoxyphenyl)-1,2,4-triazine,
3-methoxy-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
3-ethoxy-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
5,6-bis(4-methoxyphenyl)-3-propoxy-1,2,4-triazine,
3-isopropoxy-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
3-hexyloxy-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
3-(1,2-diethylbutoxy)-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-methoxy-1,2,4-triazine,
3-ethoxy-5,6-bis(4-ethoxyphenyl)-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-propoxy-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-isopropoxy-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-neopentyloxy-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-(1-ethyl-2-methylbutoxy)-1,2,4-triazine,
3-methoxy-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
3-ethoxy-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
3-propoxy-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
3-hexyloxy-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
3-ethoxy-5,6-bis(4-isopropoxyphenyl)-1,2,4-triazine,
3-(1-ethylbutoxy)-5,6-bis(4-isopropoxyphenyl)-1,2,4-triazine,
3-(2-ethylhexyloxy)-5,6-bis(4-isopropoxyphenyl)-1,2,4-triazine,
6-(4-ethoxyphenyl)-5-(4-isopropoxyphenyl)-3-(2,2,3-trimethylbutoxy)-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-methoxy-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-ethoxy-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-propoxy-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-isopropoxy-1,2,4-triazine,
3-butoxy-5,6-bis(4-dimethylaminophenyl)-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-isoheptyloxy-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-methoxy-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-ethoxy-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-propoxy-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-isopropoxy-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-pentyloxy-1,2,4-triazine,
5,6-bis(4-dipropylaminophenyl)-3-methoxy-1,2,4-triazine,
3-tert-butoxy-5,6-bis(4-dipropylaminophenyl)-1,2,4-triazine,
5,6-bis(4-dipropylaminophenyl)-3-neoheptyloxy-1,2,4-triazine,
5,6-bis(4-diisopropylaminophenyl)-3-methoxy-1,2,4-triazine,
3-butoxy-5,6-bis(4-diisopropylaminophenyl)-1,2,4-triazine,
5,6-bis(4-diisopropylaminophenyl)-3-(1-ethyl-1-methylpropoxy)-1,2,4-triazine,
5-(4-diisopropylaminophenyl)-6-(4-dimethylaminophenyl)-3-methoxy-1,2,4-triazine,
6-(4-diethylaminophenyl)-3-ethoxy-5-(4-methoxyphenyl)-1,2,4-triazine,
3-benzyloxy-5,6-bis(4-ethoxyphenyl)-1,2,4-triazine,
5,6-bis(4-isopropoxyphenyl)-3-(2-phenylethoxy)-1,2,4-triazine,
5-(4-ethoxyphenyl)-3-(o-methylbenzyloxy)-6-(4-propoxyphenyl)-1,2,4-triazine
3-benzyloxy-5,6-bis(4-dimethylaminophenyl)-1,2,4-triazine,
5-(4-diethylaminophenyl)-6-(4-diisopropylaminophenyl)-3-(1-phenylethoxy)-1,2,4-triazine,
6-(4-dipropylaminophenyl)-5-(4-methoxyphenyl)-3-(m-methylbenzyloxy)-1,2,4-triazine,
3-cycloheptyloxy-5,6-bis(4-ethoxyphenyl)-1,2,4-triazine,
3-cyclobutyloxy-5,6-bis(4-isopropoxyphenyl)-1,2,4-triazine,
3-cyclohexyloxy-5-(4-ethoxyphenyl)-6-(4-propoxyphenyl)-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-(2-methylcyclopentyloxy)-1,2,4-triazine,
3-cyclobutyloxy-5,6-bis(4-diisopropylaminophenyl)-1,2,4-triazine,
3-cyclohexyloxy-6-(4-diethylaminophenyl)-5-(4-dimethylaminophenyl)-1,2,4-triazine,
5-(4-dipropylaminophenyl)-6-(4-ethoxyphenyl)-3-(2-ethyl-3-methylcyclopentyloxy)-1,2,4-triazine,
5,6-bis(4-methoxyphenyl)-3-(2-methylcyclobutylmethoxy)-1,2,4-triazine,
3-(3-methylcyclopentylmethoxy)-5,6-bis(4-propoxyphenyl)-1,2,4-triazine.
3-cyclohexylmethoxy-5,6-bis(4-dimethylaminophenyl)-1,2,4-triazine,
3-cyclopropylmethoxy-5,6-bis(4-dipropylaminophenyl)-1,2,4-triazine,
5-(4-diethylaminophenyl)-6-(4-dimethylaminophenyl)-3-[2-(2-ethylcyclobutyl)ethoxy]-1,2,4-triazine,
3-(4-cyclopropylbutoxy)-6-(4-dipropylaminophenyl)-5-(4-isopropoxyphenyl)-1,2,4-triazine,
3-ethylthio-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
5,6-bis(4-methoxyphenyl)-3-propylthio-1,2,4-triazine,
3-isopropylthio-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
3-butylthio-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
5,6-bis(4-methoxyphenyl)-3-neoheptylthio-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-methylthio-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-ethylthio-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-propylthio-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-isopropylthio-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-(3-methylpentylthio)-1,2,4-triazine,
5,6-bis(4-ethoxyphenyl)-3-octylthio-1,2,4-triazine,
3-methylthio-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
3-ethylthio-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
5,6-bis(4-propoxyphenyl)-3-propylthio-1,2,4-triazine,
3-isopropylthio-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
3-(1,2-dimethylpropylthio)-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
3-heptyloxy-5,6-bis(4-propoxyphenyl)-1,2,4-triazine,
5,6-bis(4-isopropoxyphenyl)-3-methylthio-1,2,4-triazine,
5,6-bis(4-isopropoxyphenyl)-3-pentylthio-1,2,4-triazine,
6-(4-isopropoxyphenyl)-3-methylthio-5-(4-propoxyphenyl)-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-methylthio-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-ethylthio-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-propylthio-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-isopropylthio-1,2,4-triazine,
5,6-bis(4-dimethylaminophenyl)-3-isoheptylthio-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-methylthio-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-ethylthio-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-propylthio-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-isopropylthio-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-pentylthio-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-(1,1-dimethylhexylthio)-1,2,4-triazine,
5,6-bis(4-dipropylaminophenyl)-3-ethylthio-1,2,4-triazine,
3-(1,2-dimethylpropylthio)-5,6-bis(4-dipropylaminophenyl)-1,2,4-triazine,
5,6-bis(4-dipropylaminophenyl)-3-(1-ethyl-2-methylbutylthio)-1,2,4-triazine
5,6-bis(4-diisopropylaminophenyl)-3-ethylthio-1,2,4-triazine,
5,6-bis(4-diisopropylaminophenyl)-3-isobutylthio-1,2,4-triazine,
5,6-bis(4-diisopropylaminophenyl)-3-(2-methylpentylthio)-1,2,4-triazine,
6-(4-diethylaminophenyl)-5-(4-diisopropylaminophenyl)-3-isohexylthio-1,2,4-triazine,
5-(4-dimethylaminophenyl)-6-(4-isopropoxyphenyl)-3-(2-isopropyl-3-methylbutylthio)-1,2,4-triazine,
3-benzylthio-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
6-(4-isopropoxyphenyl)-5-(4-methoxyphenyl)-3-(2-phenylethylthio)-1,2,4-triazine,
5,6-bis(4-dipropylaminophenyl)-3-(p-methylbenzylthio)-1,2,4-triazine,
6-(4-diethylaminophenyl)-5-(4-dipropylaminophenyl)-3-(o-methylbenzylthio)-1,2,4-triazine,
3-benzylthio-5-(4-dimethylaminophenyl)-6-(4-methoxyphenyl)-1,2,4-triazine,
3-(2-isopropylcyclopentylthio)-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
3-(2-ethylcyclobutylthio)-5,6-bis(4-isopropoxyphenyl)-1,2,4-triazine,
3-cyclobutylthio-6-(4-ethoxyphenyl)-5-(4-methoxyphenyl)-1,2,4-triazine,
3-cyclopropylthio-5,6-bis(4-dimethylaminophenyl)-1,2,4-triazine,
5,6-bis(4-diethylaminophenyl)-3-(2-ethylcyclohexylthio)-1,2,4-triazine,
3-cyclopentylthio-5-(4-dimethylaminophenyl)-6-(4-dipropylaminophenyl)-1,2,4-triazine,
6-(4-dipropylaminophenyl)-5-(4-ethoxyphenyl)-3-(2-methylcyclopropylthio)-1,2,4-triazine,
3-(3-methylcyclohexylmethylthio)-5,6-bis(4-methoxyphenyl)-1,2,4-triazine,
3-(2-cyclobutylethylthio)-5,6-bis(4-ethoxyphenyl)-1,2,4-triazine,
3-cycloheptylmethylthio-6-(4-isopropoxyphenyl)-5-(4-propoxyphenyl)-1,2,4-triazine,
3-cyclopropylmethylthio-5,6-bis(4-dimethylaminophenyl)-1,2,4-triazine,
5,6-bis(4-dipropylaminophenyl)-3-[2-(1-methylcyclopentyl)ethylthio]-1,2,4-triazine,
5-(4-diethylaminophenyl)-6-(4-dipropylaminophenyl)-3-(2,3-dimethylcyclopentylmethylthio)-1,2,4-triazine,
3-(2-cyclobutylbutylthio)-6-(4-dimethylaminophenyl)-5-(4-methoxyphenyl)-1,2,4-triazine, and the like, and the pharmaceutically-acceptable acid addition salts of the basic triazines.
The preferred triazines are those wherein R 2 and R 3 in the above-defined formula are C 1 -C 3 alkoxy. More preferably, R 2 and R 3 will be the same, and most preferably are methoxy. With respect to the substituent in the 3-position, the preferred groups are C 1 -C 8 alkyl (R is --(X) n R 1 , n is 0, and R 1 is C 1 -C 8 alkyl), C 1 -C 8 alkoxy (R is --(X) n R 1 , n is 1, X is O and R 1 is C 1 -C 8 alkyl), and C 2 -C 8 alkylthio (R is --(X) n R 1 , n is 1, X is S, and R 1 is C 2 -C 8 alkyl). More preferably, the 3-substituent is C 1 -C 8 alkyl or C 1 -C 8 alkoxy. Most preferably, the 3-substituent is C 1 -C 3 alkyl or C 1 -C 3 alkoxy.
Examples of such preferred, more preferred, and most preferred triazines are included in the above list of illustrative triazines.
The compounds of the present invention are prepared by a variety of methods known to those having ordinary skill in the art. Starting materials and intermediates also are prepared by known methods. The preparation of 5,6-diaryl-1,2,4-triazines is described generally by J. G. Erickson in "The 1,2,3- and 1,2,4-Triazines, Tetrazines and Pentazines," The Chemistry of Heterocyclic Compounds, Vol. 10, Interscience Publishers, Inc., New York, N.Y., 1956, Chapter II, pp. 44-84. The 5,6-diaryl-1,2,4-triazines which are unsubstituted in the 3-position can be prepared by the catalytic reduction of the corresponding 3-chlorotriazines.
The specific procedure employed to prepare a given 3-substituted-5,6-diaryl-1,2,4-triazine in part is dependent upon the substituent in the 3-position. For example, 3-alkyl-, 3-aralkyl-, 3-cycloalkyl-, and 3-(cycloalkyl)alkyl-5,6-diaryl-1,2,4-triazines can be prepared directly by the cyclization of acylhydrazones of α-diketones by ammonium acetate in hot acetic acid under controlled conditions; see, e.g., C. M. Atkinson and H. D. Cossey, J. Chem. Soc., 1962, 1805 [Chem. Abstr., 57:4662i (1962)]. Such triazines also can be prepared from 3-chloro-5,6-diaryl-1,2,4-triazines by the procedure of E. C. Taylor and S. F. Martin [J. Amer. Chem. Soc., 94, 2874 (1972)] which involves the nucleophilic displacement of chlorine by a Wittig reagent which may be generated in situ from an alkyl-, aralkyl-, cycloalkyl-, or (cycloalkyl)alkyltriarylphosphonium halide.
3-Chloro-5,6-diaryl-1,2,4-triazines also can be employed to prepare the 3-alkoxy, 3-aralkoxy, 3-cycloalkoxy-, 3-(cycloalkyl)alkoxy-, 3-alkylthio-, 3-aralkylthio-, 3-cycloalkylthio-, and 3-(cycloalkyl)alkylthio-5,6-diaryl-1,2,4-triazines via the nucleophilic displacement of chlorine by the appropriate alcohol or thiol. The 3-alkylthio-, 3-aralkylthio-, 3-cycloalkylthio-, and 3-(cycloalkyl)alkylthio- compounds can be converted to the 3-alkoxy-, 3-aralkoxy-, 3-cycloalkoxy-, and 3-(cycloalkyl)alkoxy-5,6-diaryl-1,2,4-triazines, again via nucleophilic displacement by the appropriate alcohol. The 3-alkylthio-, 3-aralkylthio-, 3-cycloalkylthio, and 3-(cycloalkyl)alkylthiotriazines in many cases can be prepared by treating the appropriate 3-mercapto-5,6-diaryl-1,2,4-triazine with the appropriate hydrocarbyl halide in the presence of base, particularly when the hydrocarbyl halide is primary or secondary.
3-Chloro-5,6-diaryl-1,2,4-triazines are readily obtained by treating the appropriate 3-hydroxytriazine with phosphorus oxychloride. 3-Hydroxy- and 3-mercapto-5,6-diaryl-1,2,4-triazines in turn can be prepared by condensing an appropriate benzil with semicarbazide or thiosemicarbazide, respectively.
The required benzils are prepared by the oxidation of the corresponding benzoins with copper sulfate in pyridine; see H. T. Clarke and E. E. Driger, Org. Synthesis, Coll. Vol. I, 87 (1941). The benzoins are prepared by the condensation of aromatic aldehydes with cyanide ion; see W. S. Ide and J. S. Buck, Org. Reactions, 4, 269 (1948).
Another approach to the compounds of the present invention involves the use of benzils having substituents which can be displaced to give the desired R 2 or R 3 substituent. For example, the halogen on the phenyl ring at the 5-position in 5-(4-halophenyl)-6-aryl-1,2,4-triazines can be displaced with an alcohol or a dialkylamine to give the corresponding 5-(4-alkoxyphenyl)- or 5-(4-dialkylaminophenyl)- compound, respectively.
The use of two different aromatic aldehydes in the benzoin synthesis leads to unsymmetrical benzils. That is, in a benzil of the formula, ##STR3## wherein R 2 and R 3 are as described hereinbefore, R 2 and R 3 are different. The use of an unsymmetrical benzil may result in the preparation of a mixture of triazine isomers. For example, the condensation of 4-dimethylamino-4'-methoxybenzil with thiosemicarbazide gives a mixture of 5-(4-dimethylaminophenyl)-6-(4-methoxyphenyl)-1,2,4-triazine-3-thiol and 6-(4-dimethylaminophenyl)-5-(4-methoxyphenyl)-1,2,4-triazine-3-thiol
It will be recognized by those skilled in the art that mixtures of triazine isomers are separable by known methods, such as fractional crystallization and chromatography. The isomer separation may be effected upon intermediate mixtures or delayed until the final product stage.
Certain of the 5,6-diaryl-1,2,4-triazines described herein are sufficiently basic to form acid addition salts, especially when the triazine contains one or more dialkylamino groups on the phenyl rings. "Pharmaceutically-acceptable" acid addition salts are well known to those skilled in the art and in general are formed by reacting in a mutual solvent a stoichiometric amount of a suitable acid with a basic triazine. Such salts should not be substantially more toxic to warm-blooded animals than the traizines. While the choice of a salt-forming acid is not critical, in some instances a particular acid may result in a salt having special advantages, such as ready solubility, ease of crystallization, and the like. Representative and suitable acids include, among others, the following: hydrochloric, hydrobromic, hydriodic, sulfuric, nitric, phosphoric, methanesulfonic, p-toluenesulfonic, and the like.
A modification of the method of Winder was used to measure the anti-inflammatory activites of the compounds of the present invention; see C. V. Winder, et al., Arch. Int. Pharmacodyn., 116, 261 (1958). Albino guinea pigs of either sex, weighing 225-300 grams, were shaved on the back and chemically depilated (Nair® Lotion Hair Remover, Carter Products, N.Y., N.Y.) 18-20 hours before exposure to ultraviolet light. The animals, in groups of four and bearing identifying ear tags, were treated by applying to an area of skin of about 12 cm. 2 a solution of test compound dissolved in 0.1 cc. of ethanol. The control treatment consisted of administering only the drug vehicle, ethanol, to a group of four animals. Groups of four animals each were given different treatment levels of test compound to obtain dose responses. Random order and blind administration of the test compounds were employed; drug identification was not made until after all animals were graded. Immediately prior to drug application, the animals were exposed in groups of four to a high-intensity ultraviolet light for a measured period of time (usually 4-7 seconds). The ultraviolet light source, a Hanovia Lamp (Kroymayer-Model 10), was placed in contact with the skin of the animal's back. A gummed notebook paper reinforcement was affixed to the lamp lens to provide an unexposed area of contrast for grading the erythema. Beginning one hour after exposure and thereafter at half-hour intervals for another 11/2 hours, the degree of resulting erythema was graded by an arbiturary scoring system based upon the degree of contrast and redness formed. Anti-inflammatory agents delay the development of the erythema and usually have their greatest effect at the initial grading periods. The scores were, therefore, weighted by factors of 4, 3, 2, and 1 at the 1.0, 1.5, 2.0, and 2.5 hour scoring times, respectively. The erythema was graded as follows:
______________________________________Erythema Scoring SystemScore Appearance of Exposed Area______________________________________0 No redness and no contrast1 Slight redness with a faint reinforcement outline2 Slight to moderate redness with a distinct outline3 Marked redness with a distinct circular outline______________________________________
Total scores from each treatment group of four guinea pigs were compared to the control treatment, and the percent inhibition was calculated as follows: ##EQU1##
A dose-response graph was obtained by plotting dose versus percent inhibition, the points representing the average of each treatment group of four guinea pigs. The dose (ED 50 ) in micrograms per 12 cm. 2 (mcg./12 cm. 2 ) which produced a 50% inhibition of the erythemic response for the particular compound tested was obtained in several instances by extrapolation. Table I below summarizes the results obtained from testing representative compounds of the invention by the foregoing method. The plotted or calculated ED 50 for the particular compound tested, where available, is given in the last column of Table I.
Table I______________________________________Erythemic response inhibition of 5,6-Diaryl-1,2,4-triazines ##STR4## InhibitionR.sub.1 X n R.sub.2 R.sub.3 Dose.sup.a %.sup.b ED.sub.50.sup.a______________________________________CH.sub.3 -- 0 OCH.sub.3 OCH.sub.3 -- -- 2.4C.sub.2 H.sub.5 -- 0 OCH.sub.3 OCH.sub.3 -- -- 4CH.sub.3 O 1 OCH.sub.3 OCH.sub.3 -- -- 7C.sub.2 H.sub.5 O 1 OCH.sub.3 OCH.sub.3 -- -- 3.1CH.sub.3 S 1 OCH.sub.3 OCH.sub.3 -- -- 9C.sub.2 H.sub.5 S 1 OCH.sub.3 OCH.sub.3 -- -- 21.3CH(CH.sub.3).sub.2 S 1 OCH.sub.3 OCH.sub.3 100 35 --C.sub.6 H.sub.13 S 1 OCH.sub.3 OCH.sub.3 -- -- 37.4CH.sub.2 C.sub.6 H.sub.5 S 1 OCH.sub.3 OCH.sub.3 100 49 --______________________________________ .sup.a In mcg./12 cm..sup.2 .sup.b % Inhibition compared with control
The toxicities of representative compounds of the present invention, determined as the dose (LD 50 ) in milligrams per kilogram (mg./kg.) of animal body weight which is lethal to 50 percent of mice treated orally, typically are greater than about 1000 mg./kg., and in some cases are greater than about 1500 mg./kg.
In the utilization of the compounds of this invention, one (or more) of the anti-inflammatory triazines is topically administered to a warm-blooded mammal in an amount sufficient to provide at least about 1 mcg./12 cm. 2; such administration can be repeated periodically as needed. Because of the relatively low order of toxicity of such triazines, the maximum level of application is limited only by the esthetics of the mode of administration. As a practical matter, however, such triazines normally need not be administered at a level much above about 10 3 mcg./12 cm. 2 , although levels of about 10 5 mcg./12 cm. 2 or higher can be employed, if desired.
The topical administration of the anti-inflammatory compounds can be made according to any of the well known prior art procedures. Thus, such administration can utilize aerosols, creams, emulsions, lotions, ointments, solutions, and the like. In each case, the compounds to be employed are utilized in combination with one or more adjuvants suited to the particular mode of application. For example, ointments and solutions for topical administration can be formulated with any of a number of pharmaceutically-acceptable carriers, including ethanol, animal and vegetable oils, mixtures of waxes, solid and liquid hydrocarbons, glycols, and the like. Thus, a typical ointment composition comprises the following ingredients per gram of ointment:
______________________________________ mg.______________________________________Triazine 0.1-100Polyethylene gylcol 300 450-700 (N.F.)Polyethylene gylcol 4000 300-450 (U.S.P.)______________________________________
The concentration of the anti-inflammatory triazine in the final topical preparation is not critical. In general, such concentration can range from about 0.001 percent to about 50 percent (w/w or w/v), or higher.
The following examples further illustrate the preparations of the compounds of the present invention.
EXAMPLE 1
Preparation of 5,6-Bis(4-methoxyphenyl)-3-methyl-1,2,4-triazine
(A) 3-Hydroxy-5,6-bis(4-methoxyphenyl)-1,2,4-triazine
Two moles, 540 g., of anisil (4,4'-dimethoxybenzil), 222 g. (2 moles) of semicarbazide hydrochloride, 180 g. (2.2 moles) of sodium acetate, and 2.5 liters of acetic acid were heated at reflux overnight. The cooled reaction mixture was poured into 5 liters of water. The crude solid product was collected by filtration, washed with water, and recrystallized from acetic acid, giving 434 g. of 3-hydroxy-5,6-bis(4-methoxyphenyl)-1,2,4-triazine, m.p. about 272°-274° C.
Analysis: C 17 H 15 N 3 O 3 : Calc: C, 66.01; H, 4.89; N, 13.58: Found: C, 65.92; H, 5.04; N, 13.66.
(B) 3-Chloro-5,6-bis(4-methoxyphenyl)-1,2,4-triazine
Ten grams of 3-hydroxy-5,6-bis(4-methoxyphenyl)-1,2,4-triazine and 50 ml. of phosphorous oxychloride were heated at reflux for 1.5 hours. The cooled mixture was poured onto crushed ice and the resultant mixture was extracted with diethyl ether. The extract was washed successively with 2 percent sodium hydroxide and water until the washings were neutral. The ether extract was dried over anhydrous sodium sulfate and evaporated. The residue was taken up in ether, filtered, and the filtrate was evaporated to yield 9.0 g. of 3-chloro-5,6-bis(4-methoxyphenyl)-1,2,4-triazine, m.p. about 130°-132° C.
Analysis: C 17 H 14 ClN 3 O 2 : Calc: C, 62.30; H, 4.31; Cl, 10.82; N, 12.82: Found: C, 62.50; H, 4.48; Cl, 10.53; N, 12.99.
(C) 5,6-Bis(4-methoxyphenyl)-3-methyl-1,2,4-triazine
To a slurry of 11.7 g. (0.33 mole) of methyltriphenylphosphonium bromide in 150 ml. of dry tetrahydrofuran at -35° C. was added, over a 15-minute period, 20 ml. (0.033 mole) of n-butyl lithium. The reaction mixture was stirred for one hour. To the reaction mixture at -35° to -40° C. was added over a 10-minute period a solution of 5.7 g. (0.0165 mole) of 3-chloro-5,6-bis(4-methoxyphenyl)-1,2,4-triazine in 50 ml. of tetrahydrofuran. The reaction mixture was allowed to warm to ambient temperature and was stirred overnight. A solution of 1.05 g. (0.0165 mole) of sodium carbonate in 50 ml. of water was added dropwise to the reaction mixture which then was heated at reflux for three hours. The reaction mixture was cooled, poured over ice, and extracted with diethyl ether. The diethyl ether extract was washed with water, dried over anhydrous sodium sulfate, and concentrated. The concentrate was chromatographed over silica gel, with three fractions being collected. After evaporation of solvent, the third fraction solidified, m.p. about 109°-113° C. The solid was identified as 5,6-bis(4-methoxyphenyl)-3-methyl-1,2,4-triazine by nuclear magnetic resonance analysis, mass spectrographic analysis, and elemental microanalysis.
Analysis: C 18 H 17 N 3 O 2 : Calc: C, 70.34; H, 5.58; N, 13.67: Found: C, 70.42; H, 5.66; N, 13.33.
EXAMPLE 2
Preparation of 3-Ethyl-5,6-bis(4-methoxyphenyl)-1,2,4-triazine
3-Ethyl-5,6-bis(4-methoxyphenyl)-1,2,4-triazine, m.p. about 73°-75.5° C., was prepared by the method of Example 1(C) using the appropriate phosphonium bromide, except that work-up after diethyl ether extraction was carried out as follows: The diethyl ether extract was washed, dried, and concentrated as in Example 1(C), giving a solid residue which was dissolved in warm petroleum ether/ethyl acetate. The solution was cooled and the solid which precipitated was isolated by filtration. The filtrate solidified and was slurried in petroleum ether. The mixture was filtered and the solid thus obtained (second solid) was recrystallized from petroleum ether/ethyl acetate. The second solid was identified as 3-ethyl-5,6-bis(4-methoxyphenyl)-1,2,4-triazine by nuclear magnetic resonance analysis, mass spectrographic analysis, and elemental microanalysis.
Analysis: C 19 H 19 N 3 O 2 : Calc: C, 71.01; H, 5.96; N, 13.08: Found: C, 71.30; H, 6.01; N, 13.10.
EXAMPLE 3
Preparation of 3-Ethylthio-5,6-bis(4-methoxyphenyl)-1,2,4-triazine
(A) 3-Mercapto-5,6-bis(4-methoxyphenyl)-1,2,4-triazine
One hundred grams of anisil (4,4'-dimethoxybenzil) were added to 600 ml. of acetic acid and the mixture was heated to about 100° C. with stirring. Thiosemicarbazide, 68.4 g., was added and the mixture was heated at reflux for about an hour. The mixture was cooled and the solid product was collected by filtration. The solid was washed successively with acetic acid and water. The product was filtered and air dried to yield 96.3 g. of 3-mercapto-5,6-bis(4-methoxyphenyl)-1,2,4-triazine, m.p. about 233°-236° C.
Analysis: C 17 H 15 N 3 O 2 S: Calc: C, 62.75; H, 4.65; N, 12.91; S, 9.85: Found: C, 62.61; H, 4.57; N, 12.66; S, 9.73.
(B) 3-Ethylthio-5,6-bis(4-methoxyphenyl)-1,2,4-triazine
To a mixture of 10 g. (0.031 mole) of 3-mercapto-5,6-bis(4-methoxyphenyl)-1,2,4-triazine in 200 ml. of ethanol was added a solution of 1.3 g. (0.032 mole) of sodium hydroxide in 25 ml. of water. The mixture was stirred until a clear solution was obtained. To the solution was added dropwise over a 10-minute period a solution of 3.4 g. (0.032 mole) of ethyl bromide in 10 ml. of ethanol. The reaction mixture was stirred for 30 minutes. The mixture was poured over ice and extracted with diethyl ether. The diethyl ether extract was washed with water and dried over anhydrous sodium sulfate. The diethyl ether was distilled to give a solid residue which was recrystallized from petroleum ether/ethyl acetate to give 6.7 g. of 3-ethylthio-5,6-bis(4-methoxyphenyl)-1,2,4-triazine, m.p. about 118°-120° C.
Analysis: C 19 H 19 N 3 O 2 S: Calc: C, 64.57; H, 5.42; S, 9.07: Found: C, 64.78; H, 5.24; S, 9.00.
EXAMPLES 4-6
The following compounds were prepared by the method of Example 3(B), using the appropriate alkyl halide (given in parenthesis after the compound name):
3-isopropylthio-5,6-bis(4-methoxyphenyl)-1,2,4-triazine (from isopropyl iodide), m.p. about 109°-111° C.
Analysis: C 20 H 21 N 3 O 2 S: Calc: C, 65.37; H, 5.76; S, 8.73: Found: C, 65.65; H, 5.53; S, 8.63.
3-hexylthio-5,6-bis(4-methoxyphenyl)-1,2,4-triazine (from hexyl bromide), m.p. about 92°-94° C., 7 g.
Analysis: C 23 H 27 N 3 O 2 S: Calc: C, 67.45; H, 6.65; S, 7.83; N, 10.26: Found: C, 67.66; H, 6.71; S, 8.00; N, 10.26.
3-benzylthio-5,6-bis(4-methoxyphenyl)-1,2,4-triazine (from benzyl chloride), m.p. about 128°-130° C., 10.3 g.
Analysis: C 24 H 21 N 3 O 2 S: Calc: C, 69.38; H, 5.09; S, 7.72: Found: C, 69.37; H, 5.19; S, 7.37.
EXAMPLE 7
Preparation of 3-Methoxy-5,6-bis(4-methoxyphenyl)-1,2,4-triazine
(A) Procedure A
Sodium, 3.0 g. (0.13 mole), was added piecewise under a nitrogen atmosphere to 100 ml. of dry methanol, followed by the addition of a slurry of 31.6 g. (0.1 mole) of 5,6-bis(4-methoxyphenyl)-3-methylthio-1,2,4-triazine in methanol. The reaction mixture was heated at reflux overnight. The reaction mixture was cooled and filtered. The filter cake and filtrate were extracted with diethyl ether. The diethyl ether was concentrated, giving a solid, m.p. >220° C. The solid was taken up in diethyl ether and the insoluble material was removed by filtration. The filtrate was dried over anhydrous sodium sulfate and concentrated to give a solid residue which was recrystallized from petroleum ether to give 3-methoxy-5,6-bis(4-methoxyphenyl)-1,2,4-triazine, m.p. about 105°-108° C.
Analysis: C 18 H 17 N 3 O 3 : Calc: C, 66.86; H, 5.30; N, 13.00: Found: C, 67.26; H, 5.97; N, 11.69.
(B) Procedure B
Sodium, 0.91 g. (0.04 mole), was added piecewise under a nitrogen atmosphere to 100 ml. of dry methanol, followed by the portionwise addition of 11.6 g. (0.036 mole) of 3-chloro-5,6-bis(4-methoxyphenyl)-1,2,4-triazine. The reaction mixture was heated at reflux for three hours, cooled, and stirred overnight. The reaction mixture was cooled and filtered. The filtrate was concentrated and the solid residue was crystallized from petroleum ether/ethyl acetate to give 8.5 g. of 3-methoxy-5,6-bis(4-methoxyphenyl)-1,2,4-triazine, m.p. about 135°-137° C.
Analysis: C 18 H 17 N 3 O 3 : Calc: C, 66.86; H, 5.30; O, 14.86; N, 13.00: Found: C, 66.84; H, 5.52; O, 14.86; N, 12.79.
EXAMPLE 8
The following compound was prepared by the method of Example 8(B), using ethanol in place of methanol:
3-ethoxy-5,6-bis(4-methoxyphenyl)-1,2,4-triazine, m.p. about 120°-122° C., 7.1 g.
Analysis: C 19 H 19 N 3 O 3 : Calc: C, 67.64; H, 5.68; O, 14.23; N, 12.46: Found: C, 67.92; H, 5.56; O, 14.43; N, 12.38.
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5,6-Diaryl-1,2,4-triazines, topically-active anti-inflammatory agents, having the formula, ##STR1## wherein R is hydrogen or -(X) n R 1 , in which X is either O or S, n is an integer which is either 0 or 1, and R 1 is C 1 -C 8 alkyl, C 7 -C 8 aralkyl, C 3 -C 8 cycloalkyl, or C 4 -C 8 (cycloalkyl)alkyl; and R 2 and R 3 independently are C 1 -C 3 alkoxy or di(C 1 -C 3 alkyl)amino; with the proviso that when R 2 and R 3 both are methoxy, R cannot be H or methylthio; and the pharmaceutically-acceptable acid addition salts of basic members thereof.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] The present invention relates generally to wall covering borders and layer sheets of wall covering that are attached to a wall without wallpaper paste or other type of adhesive, and more particularly to wall covering borders and wall covering in general that are attached to a wall by placing them into a channel or clip.
[0003] 2. Description of Prior Art
[0004] Wall coverings are used to provide a decoration for walls. These coverings offer an alternative from painting by providing more decorative and design options. Wall coverings can also be used as borders or trim on walls, providing a touch of color or design on an otherwise plain wall surface. However, wall coverings, either full or borders, must be pasted or adhered to walls making them a permanent decoration. The result is that, when a wall covering is removed, the wall itself is often damaged, requiring it to be patched and repainted or recovered. Changing wallpaper, either as a trim or for a larger portion of a wall, is difficult since the old paper must be removed which is a time consuming and tedious process, and is generally frowned upon by the owners of residences, rental units, stores, offices or cottages where such changes are more likely to occur (or at least be more desirable) due to the change in tenants. Thus, owners of rental homes, apartments, offices and stores usually will not permit the renters or temporary dwellers to apply new wall coverings or change existing ones. There is a desire of building owners in particular, and of others who are responsible for changes in wall design, to have a pasteless wall paper system for changing wall paper without having to scrape off or otherwise remove old wallpaper before installing new wall paper. In addition, there is a desire for those decorating walls to have a fast and inexpensive way to change wall paper. Further, it is difficult to apply traditional wall coverings or wall borders to textured or non-smooth walls.
SUMMARY OF THE INVENTION
[0005] The present invention provides a solution to the problems of the prior art with a pasteless wall covering system in which wall covering becomes easily installable, removable, changeable and reusable without damaging walls. This invention will allow apartment and other rental property owners, such as store and office owners, to encourage tenants to change wall decorations to suit individual tenant's tastes, and will also enable tenants to easily install and change wall decorations on non-smooth or textured wall surfaces. The invention has particular advantages for wall covering borders but it can be used for larger sections of wall coverings as well. Further, it could be used with non-paper wall coverings such as fabric, carpeting, etc.
[0006] In accordance with a preferred embodiment of the present invention, a conventional wall covering border is attached to a semi-rigid paper type stock, or a decoration is printed onto a semi-rigid paper type stock, creating a semi-rigid wall covering border. Likewise, the semi-rigid paper stock can itself carry the decoration and form the border. A holder for the semi-rigid wall covering border is created by scoring and folding a channel that is stapled or otherwise attached to the wall surface at the desired wall covering border location.
[0007] An object of this invention is to provide an article that serves as a wall covering border or wall covering and is easy to install and change.
[0008] A further object of this invention is to provide an article that serves as a wall covering border or wall covering and is interchangeable.
[0009] A further object of this invention is to provide an article that serves as a wall covering border or wall covering and does not damage the wall surfaces when removed.
[0010] Yet another object of this invention is to provide an article that serves as a wall covering border or wall covering and can go over smooth or textured surfaces.
[0011] Yet another object of this invention is to provide an article that serves as a wall covering border or wall covering and is reusable.
[0012] Yet another object of this invention is to provide an article that serves as a wall covering border or wall covering and is inexpensive.
[0013] Yet another object of this invention is to provide an article that serves as a wall covering border or wall covering and has no pattern matching required.
[0014] Yet another object of this invention is to provide an article that serves as a wall covering border or wall covering and is supplied in a continuous roll.
[0015] Still another object is to provide a wall paper system for providing a pasteless or adhesiveless wall paper that can be easily and quickly changed.
[0016] These and other objects will become apparent from the following description of a preferred embodiment taken together with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
[0017] The invention may take physical form in certain parts and arrangement of parts, a preferred embodiment of which will be described in detail in the specification and illustrated in the accompanying drawings which form a part hereof, and wherein:
[0018] [0018]FIG. 1 is an end perspective view of a wall covering border in a holder;
[0019] [0019]FIG. 2 is an end view of the wall covering border in the holder of FIG. 1;
[0020] [0020]FIG. 2 a is a top view of the holder prior to folding the channels;
[0021] [0021]FIG. 3 is a side view of a two layer or two member wall covering border;
[0022] [0022]FIG. 3 a is a side view of a one piece wall covering border;
[0023] [0023]FIG. 4 is a side view of the two piece wall covering border in a holder;
[0024] [0024]FIG. 5 is a perspective view of the wall covering border in a holder,
[0025] [0025]FIG. 6 is a perspective view of the wall covering border in a holder,
[0026] [0026]FIG. 7 is a front perspective view of an interior or exterior corner;
[0027] [0027]FIG. 8 is a top view of the wall covering border corner piece; and
[0028] [0028]FIG. 9 is a front perspective view of a wall covering border in a holder on a wall.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0029] Referring now to the drawings wherein the showings are for the purpose of illustrating the preferred embodiment of the invention only, and not for the purpose of limiting same, FIG. 1 and FIG. 2 show a wall covering border 2 in a holder 4 . The holder 4 can be can preferably be made of PVC or other materials, can be flexible or made of flexible materials, and can preferably have a matte finish that does not reflect light. The length of the holder can be as short as about three feet. A preferred length can be between six and thirty feet. The holder 4 has a top longitudinal side 6 , a bottom longitudinal side 8 , a front surface 10 and a back surface 12 . The longitudinal sides 6 , 8 of the holder 4 are folded over twice to form channels, top channel 16 and bottom channel 18 , each having a base 20 a, 20 b, and a channel or fold lip 22 a, 22 b with a fold or channel edge 24 a, 24 b, extending along the length of the holder 4 . The channels 16 , 18 hold the wall covering border 2 when it is installed on the wall. As shown in FIG. 2 a, the holder can be scored with score lines 26 in the front surface 10 so that it can be stored and distributed without channels and folded to create the channels 16 , 18 at the installation site.
[0030] Numerous attachments means can be used to attach the back surface 12 of the holder 4 to a wall. Such means include hook and latch systems such as Velcro®, adhesives, double faced tape, staples, or glue. In a preferred embodiment, the top channel lip 22 a is larger than the bottom channel lip 22 b. In a preferred embodiment, the channel lips 22 a, 22 b, are biased in an inward direction, that is, the channel lips have “memory”, so that they press against the wall paper border, holding the border firmly in place.
[0031] [0031]FIG. 3 shows the wall covering border 2 which is comprised of a top member 28 and a bottom member 30 . The top member 28 can preferably be made of wall covering material, which can be from 2″ to 30″ wide, and, in one preferred embodiment, from 6¼″ to 6¾″ wide. The bottom member 30 can be made of a semi-rigid paper stock. The paper stock, or alternative material, should be flexible enough so that wall covering border 2 can be changed from a flat position to a roll for storing and transporting. The bias of the roll could help keep it in place in the holder. For the bottom member 30 , a material having one side covered with pressure sensitive adhesive can be used to so that the bottom member 30 can be inexpensively and simply attached to the top member 28 . In the alternative, as shown in FIG. 3 a, the decoration can be placed directly on a semi-rigid paper stock 32 .
[0032] [0032]FIG. 4 shows a second embodiment, wherein the holder 40 is separated into two pieces, each “J” shaped and having a back 42 , an upper wall 44 and a front or top 46 . A channel 48 is formed between the top 46 and the back 42 of the holder 40 , there being two channels 48 for each assembly. FIG. 5 shows another embodiment, wherein the holder 50 can preferably be made of molded foam, channeled wood or other moldable, semi-rigid material. In the alternative, the holder 50 can be made of rigid or semi-rigid PVC with clear edges, similar to the material found in vertical blinds. The front 52 of the holder 50 can be rounded or angled. A pair of opposing channels 54 are formed between the front 52 and the back 56 of the holder 50 .
[0033] Another embodiment of the invention is shown in FIG. 6 in which the holder 60 , attached to a wall 62 , is the hook-type material of a hook and latch connecting system, such as Velcro, and the latch material 64 is attached to the back of the wall covering border 2 . In the alternative, the holder 60 could be made of double faced adhesive tape.
[0034] [0034]FIG. 7 shows a corner piece 70 , which can be used at the junction of walls, typical inside corners as well as outside corners. These corner pieces can be made of rigid PVC vinyl, wood, foam, plastic or other materials. The holder 4 and wall covering border 2 can be applied to each wall forming the juncture and the corner piece 70 can be inserted into the corner, abutting holder. In the embodiment shown in FIG. 7, the corner piece can contain slots 72 into which the wall covering border 2 can be inserted. In the alternative, the wall covering border may abut the corner piece. In a preferred embodiment, the wall covering border 2 and holder 4 may be bent to wrap the corner; no special corner piece would be necessary.
[0035] [0035]FIG. 8 shows a corner piece 80 which can be used in a non-square corner, that is, a corner that is not 90°. This corner piece 80 has a center score-line 82 along which it can be bent or folded, creating the desired corner angle. In addition, a channel 84 is formed between the top 86 , the side 88 and the back 90 of the corner piece 80 , there being two channels 84 for each corner piece 80 . The top 86 and the side 88 of the channel 84 do not extend the entire length of the wall covering border holder; instead, each terminates before reaching the score-line 82 , enabling the corner piece to bend and form the corner angle. There are vertical score-lines 92 along which the corner piece can be folded to create the top and the side of the channel.
[0036] Installation of the current invention is easy. In the embodiment shown in FIGS. 1 and 2, channels 16 , 18 are created by folding the holder 4 along the scored lines 26 . In all of the embodiments, the holder 4 , 40 , 50 , 60 is attached to the wall using fasteners such as clips, staples, or adhesives such as pressure sensitive adhesives and double faced tape. Key shaped holes can be made in the backs of the holder having an enlarged bottom portion and a narrow top portion. A screw or other fastener can be inserted in a wall with its top end extending outwardly from the wall, and the back of the holder can be placed so that the head of the fastener extends through the enlarged bottom portion hole. The holder can then be released so that the fastener supports the holder through the upper edge of the narrow portion of the hole. Once the holder is secured on the wall, the wall covering border 2 is unrolled and inserted into the holder 4 , preferably by sliding it into the channel 16 , 18 , 48 , 54 along the wall. Corner pieces, which can be made of rigid PVC vinyl, wood, foam or plastic, can be used at the junction of walls. These corner pieces can contain slots into which the wall covering border can be inserted. Corner pieces can be used in typical inside corners as well as outside corners; in both cases, the channel 16 , 18 , 48 , 54 and wall covering border 2 can be applied to each wall forming the juncture. The wall covering border 2 may wrap the corner, if it is pliable enough.
[0037] Changing the wall paper is very easy. The user simply grasps the end portion of the wall paper and withdraws it from the holder, and inserts a replacement wall paper by forcing it between the front and back of the holder.
[0038] The invention has been described with particular emphasis on the preferred embodiments. It should be appreciated that these embodiments are described for purposes of illustration only, and that numerous alterations and modifications may be practiced by those skilled the art without departing from the spirit and scope of the invention. It is intended that all such modifications and alterations be included insofar as they come within the scope of the invention or the equivalents thereof.
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The present invention provides a pasteless wall covering system in which wall covering becomes easily installable, removable, changeable and reusable without damaging walls. A wall covering border is attached to, or made from, a semi-rigid paper stock and is held on the wall by a holder with channels. The holder can be created by scoring and folding a top and bottom channel. The holder can be attached to the wall by stapling, adhesives or other attachment means.
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CROSS-REFERENCE TO RELATED APPLICATION
[0001] This application claims priority to earlier filed U.S. provisional application Ser. No. 60/759,606 filed on Jan. 17, 2006, the entire contents of which is incorporated herein by its reference. The electrical energy harvesting power sources disclosed herein are described in detail in U.S. patent application Ser. Nos. 10/235,997 and 11/116,093, each of which are incorporated herein by their reference.
GOVERNMENTAL RIGHTS
[0002] This invention was made with Government support under Contract No. DAAE30-03-C1077, awarded by the U.S. Army. The Government may have certain rights in this invention.
BACKGROUND OF THE INVENTION
[0003] 1. Field of the Invention
[0004] The present invention relates generally to power supplies, and more particularly, to power supplies for projectiles, which generate power due to an acceleration of the projectile.
[0005] 2. Prior Art
[0006] Fuzing of munitions is necessary to initiate a firing of the munition. Currently, there is no reliable and simple mechanism for differentiating an accidental drop of a munition from a firing acceleration, to prevent an accidental drop from initiating a fuzing of the munition. Similarly, there is a need to reliably validate firing and start of the flight of a munition. For rounds with booster rockets, this capability can provide the means to validate firing, firing duration and termination. Munitions further require the capability to detect target impact, to differentiate between hard and soft targets and to provide a time-out signal for unexploded rounds. Lastly, in order to recover unexploded rounds (munitions) it would be desirable for the munition to have the capability to notify a recovery crew.
SUMMARY OF THE INVENTION
[0007] The power sources/generators/supplies disclosed in U.S. patent application Ser. Nos. 10/235,997 and 11/116,093 are based on the use of piezoelectric elements. Such power sources are designed to harvest electrical energy from the firing acceleration as well as from the aerodynamics induced motions and vibration of the projectile during the entire flight. The energy harvesting power sources can withstand firing accelerations of over 100,000 Gs and can be designed to address the power requirements of various fuzes, communications gear, sensory devices and the like in munitions.
[0008] The electrical energy harvesting power sources are based on a novel approach, which stores mechanical energy from the short pulse firing accelerations, and generates power over significantly longer periods of time by vibrating elements, thereby increasing the amount of harvested energy by orders of magnitude over conventional methods of directly harvesting energy from the firing shock. With such power sources, electrical power is also generated during the entire flight utilizing the commonly present vibration disturbances of various kinds of sources, including the aerodynamics disturbances or spinning. Such power sources may also be used in a hybrid mode with other types of power sources such as chemical reserve batteries to satisfy any level of power requirements in munitions.
[0009] While the piezoelectric power generators are generally suitable for many applications, they are particularly well suited for low to medium power requirements, particularly when safety and very long shelf life are critical factors.
[0010] The electrical energy harvesting power sources for munitions are based on a novel use of stacked piezoelectric elements. Piezoelectric elements have long been used in accelerometers to measure acceleration and in force gages for measuring dynamic forces, particularly when they are impulsive (impact) type. In their stacked configuration, the piezoelectric elements have also been widely used as micro-actuators for high-speed and ultra-accuracy positioning applications with low voltage input requirement and for high-frequency vibration suppression. The piezoelectric elements have also been used as ultrasound sources and for the generation and suppression of acoustic signals and noise.
[0011] In the present application, the electrical energy harvesting power sources are used for powering fuzing electronics as acceleration and motion sensors, acoustic sensors, micro-actuation devices, etc., that could be used to enhance fusing safety and performance. As such, the developed electrical energy harvesting power sources, in addition to being capable of replacing or at least supplementing chemical batteries, have significant added benefits in rendering fuzing safer and enhancing its operational performance. Fir example, the piezoelectric-based electrical energy harvesting power sources can provide the following safety and performance enhancing capabilities:
1. Capability to detect accidental drops and differentiate them from the firing acceleration. 2. Capability to validate firing and start of the flight. For rounds with booster rockets, this capability will provide the means to validate firing, firing duration and termination. 3. Capability to detect target impact. 4. Capability to differentiate between hard and soft targets. 5. Capability to provide time-out signal for unexploded rounds. 6. In an unexploded round, the capability to detect acoustic and vibration wake-up signals generated by a recovery crew and respond to the same via an RF or acoustic signal or the like.
[0018] Accordingly, a system is provided for use with a munition for detecting a target impact of the munition. The system comprising: a power supply having a piezoelectric material for generating power from a vibration induced by the munition; and a processor operatively connected to the power supply for monitoring an output from the power supply and determining whether the output of power from the power supply has dropped below a predetermined threshold.
[0019] If the output of the power supply has dropped below the predetermined threshold, the processor can further disable the round from being internally detonated.
[0020] Also provided is a method for detecting a target impact of a munition. The method comprising: providing the munition with a power supply having a piezoelectric material for generating power from a vibration induced by the munition; monitoring an output from the power supply; and determining whether the output of power from the power supply has dropped below a predetermined threshold.
[0021] The method can further comprise, if the output of the power supply has dropped below the predetermined threshold, disabling the round from being internally detonated.
BRIEF DESCRIPTION OF THE DRAWINGS
[0022] These and other features, aspects, and advantages of the apparatus and methods of the present invention will become better understood with regard to the following description, appended claims, and accompanying drawings where:
[0023] FIG. 1 illustrates a schematic cross section of an exemplary power generator for fuzing of a munition.
[0024] FIG. 2 illustrates a schematic view of a system of harvesting electric charges generated by the power generator of FIG. 1 .
[0025] FIG. 3 illustrates a longitudinal acceleration (firing force, which is equal to the longitudinal acceleration times the mass of the round) versus time plot for a fired munition.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0026] In the methods and apparatus disclosed herein, the spring end of a mass-spring unit is attached to a housing (support) unit via one or more piezoelectric elements, which are positioned between the spring end of the mass-spring and the housing unit. A housing is intended to mean a support structure, which partially or fully encloses the mass-spring and piezoelectric elements. On the other hand, a support unit may be positioned interior to the mass-spring and/or the piezoelectric elements or be a frame structure that is positioned interior and/or exterior to the mass-spring and/or piezoelectric elements. The assembly is provided with the means to preload the piezoelectric element in compression such that during the operation of the power generation unit, tensile stressing of the piezoelectric element is substantially avoided. The entire assembly is in turn attached to the base structure (e.g., gun-fired munitions). When used in applications that subject the power generation unit to relatively high acceleration/deceleration levels, the spring of the mass-spring unit is allowed to elongate and/or compress only within a specified limit. Once the applied acceleration/deceleration has substantially ended, the mass-spring unit begins to vibrate, thereby applying a cyclic force to the piezoelectric element, which in turn is used to generate electrical energy. The housing structure or the base structure or both may be used to provide the limitation in the maximum elongation and/or compression of the spring of the mass-spring unit (i.e., the amplitude of vibration). Each housing unit may be used to house more than one mass-spring unit, each via at least one piezoelectric element.
[0027] In the following schematic the firing acceleration is considered to be upwards as indicated by arrow 113 .
[0028] In FIG. 1 , power generation unit 100 includes a spring 105 , a mass 110 , an outer shell 108 , a piezoelectric (stacked and washer type) generator 101 , one socket head cap screw 104 and a stack of Belleville washers 103 (each of the washers 103 in the stack is shown schematically as a single line). Piezoelectric materials are well known in the art. Furthermore, any configuration of one or more of such materials can be used in the power generator 100 . Other fasteners, which may be fixed or removable, may be used and other means for applying a compressive or tensile load on the piezoelectric generator 101 may be used, such as a compression spring. The piezoelectric generator 101 is sandwiched between the outer shell 108 and an end 102 of the spring, and is held in compression by the Belleville washer stack 103 (i.e., preloaded in compression) and the socket head cap screw 104 . The mass 109 is attached (e.g., screwed, bonded using adhesives, press fitted, etc.) to another end 106 of the spring 105 . The piezoelectric element 101 is preferably supported by a relatively flat and rigid surface to achieve a relatively uniform distribution of force over the surface of the element. This might be aided by providing a very thin layer of hard epoxy or other similar type of adhesives on both contacting surfaces of the piezoelectric element. The housing 108 may be attached to the base 107 by the provided flange 111 using well known methods, or any other alternative method commonly used in the art such as screws or by threading the outer housing and screwing it to a tapped base hole, etc. The mass 109 is provided with an access hole 110 for tightening the screw 104 during assembly. Between the free end 106 of the spring and the base 107 (or if the mass 109 projects outside the end 106 of the spring, then between the mass 109 and the base 107 ) a gap 112 is provided to limit the maximum expansion of the spring 105 . Alternatively, the gap 112 may be provided by the housing 108 itself. The gap 112 also limits the maximum amplitude of vibration of the mass-spring unit.
[0029] During firing of a projectile (the base structure 107 ) containing such power generation unit 100 , the firing acceleration is considered to be in the direction 113 . The firing acceleration acts on the mass 109 (and the mass of the spring 105 ), generating a force in a direction opposite to the direction of the acceleration that tends to elongate the spring 105 until the end 106 of the spring (or the mass 109 if it is protruding from the end 106 of the spring) closes the gap 112 . For a given power generator 100 , the amount of gap 112 defines the maximum spring extension, thereby the maximum (tensile) force applied to the piezoelectric element 101 . As a result, the piezoelectric element is protected from being damaged by tensile loading. The gap 112 also defines the maximum level of firing acceleration that is going to be utilized by the power generation unit 100 .
[0030] When the firing acceleration has ended, i.e., after the projectile has exited the gun barrel, the mechanical (potential) energy stored in the elongated spring is available for conversion into electrical energy. This can be accomplished by harvesting the varying voltage generated by the piezoelectric element 101 as the mass-spring element vibrates. The spring rate and the maximum allowed deflection determine the amount of mechanical energy that is stored in the spring 105 . The effective mass and spring rate of the mass-spring unit determine the frequency (natural frequency) with which the mass-spring element vibrates. By increasing (decreasing) the mass or by decreasing (increasing) the spring rate of the mass-spring unit, the frequency of vibration is decreased (increased). In general, by increasing the frequency of vibration, the mechanical energy stored in the spring 105 can be harvested at a faster rate. Thus, by selecting appropriate spring 105 , mass 109 and gap 112 , the amount of electrical energy that can be generated and the rate of electrical energy generation can be matched with the requirements of a projectile.
[0031] In FIG. 1 , the spring 105 is shown to be a helical spring. The preferred helical spring, however, has three or more equally spaced helical strands to minimize the sideways bending and twisting of the spring during vibration. In general, any other type of spring may be used as long as they provide for vibration in the direction of providing cyclic tensile-compressive loading of the piezoelectric element.
[0032] The power generation unit 100 of FIG. 1 is described herein by way of example only and not to limit the scope or spirit of the present invention. Other embodiments described in U.S. patent application Ser. Nos. 10/235,997 and 11/116,093 can also be used in the applications described below as well as any other type of power generation unit which harvests electrical energy from a vibrating mass due to the acceleration of a projectile/munition as well as from the aerodynamics induced motions and vibration of the projectile during the entire flight.
[0033] The schematic of FIG. 2 shows a typical system of harvesting electric charges generated by the piezoelectric element of the energy harvesting power generation unit 100 as the mass-spring element of the power source begins to vibrate upon exiting the gun barrel. Electronic conditioning circuitry 202 , well known in the art, would, for example, convert the oscillatory (AC) voltages generated by the piezoelectric element to a DC voltage and then regulate it and provide it for direct use or for storage in a storage device 204 such as a capacitor or a rechargeable battery as shown in the schematic of FIG. 2 . The piezoelectric output is connected by wires 203 to the electronic converter/regulator/charger 202 , the output of which is connected to the storage device (a capacitor or rechargeable battery) 204 by wires 205 , or is used to directly run a load 206 via wires 207 . A processor 208 is also provided for processing information from the output of the power generation unit 100 . Although the processor 208 is shown connected by way of wiring 209 to the electronic conditioning circuitry 202 , it can be connected to or integral with any of the shown components such that it is operative to process the output or output information from the power generation unit 100 .
[0000] Accidental Drop Detection and Differentiation from Firing
[0034] During the firing, the force exerted by the spring element of the power generation unit 100 generates a charge and thereby a voltage across the piezoelectric element that is proportional to the acceleration level being experienced. The generated voltage is proportional to the applied acceleration since the applied acceleration works on the mass of the spring-mass element of the energy harvesting power source (in fact the mass of the piezoelectric element itself as well), thereby generating a force proportional to the applied acceleration level.
[0035] In certain situations and particularly in the presence of noise and at relatively low acceleration levels, the mass-spring system of the power generation unit 100 begins to vibrate and generates an oscillatory (AC) voltage with a DC bias, which is still proportional to the level of acceleration that is applied to the munitions. Hereinafter, when vibratory motion is present, the piezoelectric voltage output is intended to indicate the level of the aforementioned DC bias.
[0036] The level of voltage produced by the piezoelectric element is therefore proportional to the level of acceleration that is experienced by the munitions in the longitudinal (firing) direction. This information is obviously available as a function of time. A typical such longitudinal acceleration (firing force, which is equal to the longitudinal acceleration times the mass of the round) versus time plot may look as shown in FIG. 3 . From this plot, the processor 208 may calculate information such as the peak acceleration (impulsive force) level and the acceleration (firing force) duration, Δt, can be measured. The processor 208 can be dedicated for such calculations or used for controlling other functions of the munition. The plot information can also be used to calculate the average acceleration (firing force) level and the total applied impulse (the area under the force versus time curve of FIG. 3 or the product of the average firing force times the time duration). The amount of impulse that the round is subjected to in its longitudinal (firing) direction is thereby known. In practice, the processor may be used onboard the munitions (or the generally present fuzing processor could be used) to make the above time and voltage (acceleration or firing force) measurements and perform the indicated calculations and provide the safety and fuzing decision making capabilities that are indicated in the remainder of this disclosure.
[0037] However, a round is subjected to such input impulses in its longitudinal direction during its firing as well as during accidental dropping. The level of input impulse due to accidental dropping of the round is, however, orders of magnitude smaller than that of firing.
[0038] For example, consider a situation in which a round is dropped on a very rigid concrete slab, generating around 15,000 G of acceleration in the longitudinal direction (here, it is assumed that the round is dropped perfectly on its base, resulting in the highest possible longitudinal impact acceleration). Assuming that the elastic deformation that occurs during the impact is in the order of 0.1 mm, a conservative estimate of the impact duration with a constant acceleration of 15,000 Gs becomes about 0.04 msec. Now, even if we assume a similar acceleration profile in the gun barrel, but spread it over a time duration of 8 msec (close to what is experienced in many large caliber guns), then the impulse experienced during the firing is (8/0.04) or 200 times larger than that experienced during a drop over a hard surface. This is obviously a conservative estimate and the actual ratio can be expected to be much higher since in most situations, the round is not expected to land perfectly on its base and on a very hard surface and that the firing acceleration is expected to be significantly larger than those experienced in an accidental drop.
[0039] The above example clearly shows that by measuring the impact impulse, accidental drops can be readily differentiated from the firing acceleration by the processor 208 . This characteristic of the present piezoelectric based power generation units 100 can be readily used to construct a safety feature to prevent arming of the fuzing during accidental drops and/or to take some other preventive measures. This safety feature can be readily implemented in the electrical energy collection and regulation electronics of the power source or in the fuzing electronics (e.g., the processor 208 can have an input into the electrical energy collection and regulation electronics 202 of the power source or in the fuzing electronics to prevent fuzing when the calculated impact pulse is below a predetermined threshold value indicative of a firing).
[0000] Firing Validation and Booster firing
[0000] and Duration Time and Total Impulse
[0040] As was described in the previous section on accidental drop detection and differentiation from firing, the firing impulse as well as its acceleration profile and time duration can be readily measured and/or calculated from the output of the piezoelectric elements of the power generation units 100 by the processor 208 . Similarly, the completion of the firing acceleration cycle and the start of the free flight are readily indicated by the piezoelectric element. In the presence of firing boosters, their time of activation; the duration of booster operation, and the total exerted impulse on the round can also be determined by the processor 208 from the output of the power generation unit 100 .
[0041] As a result, the piezoelectric based power generation units provide the means to validate firing; determine the beginning of the free flight; and when applicable, validate booster firing and its duration.
[0000] Target Impact Detection
[0042] During the flight, the munition/projectile is decelerated by aerodynamic drag. Projectiles are commonly designed to produce minimal drag. As a result, the deceleration in the axial direction is fairly low. In addition, there may also be components of vibratory motions present in the axial direction. Axially oriented piezoelectric based power generation units 100 can also be very insensitive to lateral accelerations, which are also usually fairly small except for high spinning rate projectiles.
[0043] When impact occurs (assuming that the impact force is at least partially directed in the axial direction), the piezoelectric elements of the power generation units 100 experience the resulting input impact, including the time of impact, the impact acceleration level, peak impact acceleration (force) and the total impact impulse. As a result, the exact moment of impact can be detected and/or calculated by the processor 208 from the output of the power generation unit 100 .
[0044] In addition, when desired, lateral impact time, level and total impulse may be similarly detected by employing at least one such piezoelectric based power generation unit 100 in the lateral directions, noting that at least two piezoelectric power sources directed in two different directions in the lateral plane are required to provide full lateral impact information. Alternatively, a single power generation unit 100 can be provided which is aligned offset from an axial direction so as to have a vibration component in the axial direction and a vibration component in the lateral direction. Such laterally directed power sources are generally preferable for harvesting lateral vibration and movements, such as those generated by small yawing and pitching motions of the round.
[0000] Hard and Soft Target Detection
[0045] When the munition impacts the target, ground or another object, the munition's deceleration profile can be measured from the piezoelectric element output voltage during the impact period and peak deceleration level, impact duration, impact force and total impulse can then be calculated as previously described using the processor 208 . This information can then be used to determine if a relatively hard or soft target has been hit, noting that the softer the impacted target, the longer would be the duration of impact, peak impact deceleration (force). The opposite will be true for harder impacted targets. This information is very important since it can be used by the fuzing system to make a decision as to the most effective settings.
[0046] It is worth noting at this point that the hard or soft target detection and decision making, in fact all the aforementioned detection and decision making processes, are expected to be made nearly instantly by the power source electrical energy collection and regulation electronics or the fuzing electronics by employing, for example, threshold detecting switches to set appropriate flags.
[0000] Time-out Signal for Unexploded Rounds
[0047] Once a munition has landed and is not detonated, whether due to faulty fuzing or other components or properly made decision against detonation, the piezoelectric based power generation unit 100 will stop generating electrical energy once its initial vibratory motion at the time of impact has died out. The electrical power harvesting electronics and/or the fuzing electronics can utilize this event, if followed by target impact, to initiate detonation time-out circuitry. For example, the power source and/or fuzing electronics can be equipped with a time-out circuit that would disable the detonation circuitry and/or components to make it impossible for the round to be internally detonated. The time-out period can be programmed, for example, while loading fuzing information before firing, and/or may be provided by built-in leakage rate from capacitors assigned for this purpose.
[0048] Wake-Up Signal Detection and Detection Beacon Provision
[0049] Consider the situation in which a round has landed without detonation and its detonation window has timed-out. Then at some point in time, a recovery crew may want to attempt to safely recover the unexploded rounds. The present piezoelectric based power generation unit 100 can readily be used to transmit an RF or other similar beacon signals for the recovery crew to use to locate the projectile. This may, for example, be readily accomplished through the generation of acoustic signals that are produced by the dropping or hammering of weights on the ground or by detonating small charges in the suspect areas. The acoustic waves will then cause the piezoelectric elements of the power source to generate a small amount of power to initiate wake-up and transmission of the RF or similar beacon signal.
[0050] When appropriate, the acoustic signal being transmitted by the recovery crew could be coded. In addition, this feature of the power generation unit 100 provides the means for the implementation of a variety of tactical detonation scenarios. As an example, multiple rounds could be fired into an area without triggering detonation, awaiting a detonation signal from a later round, which is transmitted by a coded acoustic signal during its own detonation.
[0051] While there has been shown and described what is considered to be preferred embodiments of the invention, it will, of course, be understood that various modifications and changes in form or detail could readily be made without departing from the spirit of the invention. It is therefore intended that the invention be not limited to the exact forms described and illustrated, but should be constructed to cover all modifications that may fall within the scope of the appended claims.
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A method is provided for detecting a target impact of a munition. The method including: providing the munition with a power supply having a piezoelectric material for generating power from a vibration induced by the munition; monitoring an output from the power supply; and determining whether the output of power from the power supply has dropped below a predetermined threshold.
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CROSS-REFERENCE TO PRIOR APPLICATION
[0001] This application claims the benefit under 35 USC §119(e) of U.S. provisional application serial No. 60/402,418 filed Aug. 8, 2002 and is a divisional of U.S. application Ser. No. 10/638,282 filed Aug. 7, 2003.
BACKGROUND OF THE INVENTION
[0002] 1.0 Field of Invention
[0003] This invention relates to contraceptive intrauterine devices (IUDs) and methods of preventing conception.
[0004] 2.0 Description of the Related Art
[0005] Reproductive medicine is lagging in contraception technologies at a time when the world population is about to include the largest proportion of people of reproductive age ever. This invention introduces Nitinol thin film, a recent major advancement in material science and micro-electro-mechanic technology, to help resolve longstanding limitations in existing contraceptive intrauterine devices.
[0006] Intrauterine contraceptive devices (IUDs) are objects inserted into the uterus to prevent conception. Introducing an object into the uterus for birth control is an ancient discovery that has evolved to become the modern IUD. The use of such devices is based on the fact that the presence of a foreign object in the uterus discourages conception. IUDs have been invented of numerous and varied solid shapes and configurations. The most well known shapes are the ring, the “S”, the coil or spiral, the “T” and the “T” with its transversal arms bent down. These devices are configured to occupy a significant portion of the uterine fundus in order to prevent expulsion through the cervical os, a lumen of a few millimeters in diameter.
[0007] Existing IUDs are most commonly inserted using an insertion tube and a complementary plunger. Prior to insertion, the extended arms of the “T” are manually inserted into the upper end of the insertion tube The tube is of sufficient diameter and malleability to constrain the extended arms of the device in a folded position during insertion. The loaded tube is pushed through the cervical os into the uterine cavity. When the desired position is achieved, the tube is withdrawn to release the IUD while the inner plunger is manually held stationary. Withdrawal of the insertion tube allows the arms of the “T” to unfold inside the uterus.
[0008] The required manual placement of the IUD in the insertion tube is disadvantageous because it is cumbersome, time consuming, and increases the possibilities of compromising the sterile field. Moreover, where the IUD must be positioned by human manipulation, there exists a hazard of erroneous placement that could reduce contraceptive effectiveness and may be a source of injury to the patient. Approximately 1 in 500 insertions of existing rigid IUDs cause perforation.
[0009] IUDs of some configurations must be positioned in the insertion tube by drawing back on the “tail,” i.e., the string attached to the IUD for removal from the uterus. Such a method, however, is undesirable for an IUD having a “T” configuration since the arms would be drawn upwards. In some devices the folding of the IUD or placement in the insertion tube occurs after the initial placement of the insertion tube in the uterus, resulting in less control on placement position.
[0010] Attempts have been made to reduce the size of convention solid IUDs to allow use by younger women, but reducing size and surface area result in a less effective contraceptive and an increased rate of expulsion. The challenges in adapting these devices for use by nulliparous women include reducing size to reduce trauma and adverse reactions, while maintaining a large enough inert or medicated surface area to maximize effectiveness and a size sufficient to resist expulsion. These problems have limited the use of existing IUDs, especially in younger women.
[0011] The use of Nitinol is already well established in other areas of medicine and thin film devices are being developed to replace or expand these applications. For example, thin film devices are successfully used in neuro- and neurovascular surgery, where miniaturization, flexibility, and compliance are imperative to reach small vessels and to remove clots and block aneurisms.
OBJECTS AND SUMMARY OF THE INVENTION
[0012] It is a general object of the invention to provide a new and improved reversible contraceptive device and method for intrauterine use in humans and other mammals
[0013] Another object to provide a device and method of use of the type described which is relatively smaller, safer, less intrusive, easier to insert and remove, more comfortable, and less expensive to manufacture than currently available IUDs.
[0014] In its general concept, the invention provides contraceptive IUD devices, and methods of use, made from thin-film, shape memory alloy materials exhibiting superplasticity and shape memory at the internal body temperatures of humans and other mammals.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] FIG. 1 is a perspective view of a device in accordance with one embodiment of the invention.
[0016] FIG. 2 is a perspective view of a device in accordance with another embodiment.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0017] The contraceptive devices of the invention are comprised of thin films of a shape memory alloy (SMA), such as TiNi (also known as Nitinol). TiNi thin film is ˜5 microns thick and has shape memory at human body temperature. At lower temperatures, the material is in its martensitic state, is highly ductile, and can withstand large deformations. At higher temperatures, such as that of the human body, the material undergoes a phase transformation to a more rigid austenitic state in which it is not easily deformed.
[0018] The contraceptive thin film IUD is a micro-fabricated three-dimensional object. FIG. 1 shows generally at 10 a thin film IUD device of frusto-conical shape in accordance with one preferred embodiment of the invention. FIG. 2 shows generally at 20 a thin film IUD device in a generally U-shape in accordance with another preferred embodiment. The invention contemplates that many other three-dimensional geometric shapes can be used for the device as long as the portions of the device surfaces make contact with the uterus wall sufficient to cause irritation of the wall. The irritation is believed to be the physiological reaction which prevents the mammal's egg from attaching to the wall, which would otherwise result in pregnancy. The uterus wall reacts and essentially “thinks” that conception has taken place when it has not.
[0019] Micro-electro-mechanical (MEM) techniques developed recently at TiNi Alloy Co permit the fabrication of seamless thin film three-dimensional structures that were impossible to fabricate in the past. Since this TiNi alloy film has a “body temperature phase transformation”, then once inserted and released into the uterine cavity (temperatures ˜37° C.), the thin film contraceptive expands within the uterus so that the film makes contact with the uterine walls with sufficient force to maintain its predetermined shape. The inherent elasticity of the thin film will also enable it to comply and move with the walls during contraction and relaxation of the uterine muscles.
[0020] By virtue of the characteristics of TiNi shape memory alloy, the IUD can be folded or rolled at low temperatures and introduced into the uterus within a very narrow tube, i.e. a catheter of less than 1 mm diameter. Once inside the uterus, the contraceptive foil is released from the catheter. The inherent properties of the shape memory alloy allow the IUD to automatically unfold and adopt a desired shape. The thin film contraceptive IUD can be manufactured, sterilized and pre-packed inside a catheter, minimizing contamination risks. The thin film IUDs can be micro-fabricated with appendages or tails. These would not be placed extracervically but would remain inside the uterus or cervix. Material for adding radio-opaque features to the contraceptive can also be used. A comparison between a regular IUD insertion tube and that used for a thin film contraceptive device is illustrated in FIG. 1 .
[0000] Fabrication of the Device
[0021] In the invention three-dimensional shapes of thin films are fabricated using the general teachings of Busch et. al. U.S. Pat. No. 5,061,914, the disclosure of which is incorporated by this reference. Multiple layers of TiNi thin film and sacrificial material are sputter deposited sequentially on a polished and oxidized silicon wafer. The sacrificial material can be chromium, aluminum, copper, or TiCuSil, a material obtained through Wesgo Metals. Chromium is preferentially used as a sacrificial layer.
[0022] A thin chromium layer is sputter deposited on the oxidized silicon wafer using RF sputtering at argon pressure of about 2 milliTorr. The thickness of the deposited thin film can be 500 A or more. A thin layer of TiNi is sputter deposited on top of the chromium layer using DC sputtering at an argon pressure of about 2 milliTorr. The thickness of the deposited TiNi layer can be from 1 to 40 microns. A thin chromium layer is then sputter deposited on top of the device layer. Typical thickness of this layer is about 1000 A. This layer acts as a protective layer for the underlying TiNi layer during subsequent lithography steps and provides a sacrificial layer that in the final steps of fabrication is dissolved away chemically in order to selectively create a pocket between the two device layers.
[0023] Three-dimensional thin film shapes as shown in FIG. 1 require two photo masks (mask 1 and mask 2 ) with appropriate pattern designs. The design of mask 1 determines the final three-dimensional shape of the device; e.g., solid triangles for cones, rectangles for cylinders, semicircles for hemispheres, etc. Mask 2 contains designs for fenestration or any other surface patterns that may be needed for the final device. Mask 1 is used to pattern the top sacrificial layer deposited on the wafer described above.
[0024] Micro-photolithography techniques are then followed. A thin layer of positive photo resist liquid is spin-coated on the above wafer at about 4000 rpm and baked at 90° C. in a clean room convection oven. Using an ultraviolet light mask aligner, the wafer and mask 1 are aligned and the photo resist layer is UV exposed though the mask plate which transfers the patterns from mask 1 on to the photo resist layer. The wafer with exposed photo resist is immersed in developer solution to selectively remove the exposed sections of the photo resist thus creating windows in the photo resist layer on the wafer. When immersed in a chemical etchant, these windows in the photo resist allow for the selective etching of the chromium layer. After patterning, the photo resist layer is chemically dissolved away by immersing in a solvent.
[0025] The wafer is loaded back into the sputtering chamber that is taken to high vacuum. In the chamber, the top exposed surface is sputter-etched to remove any contamination. Sputter-etch is a process similar to sputtering except that in the case of sputter-etch the argon ions are accelerated to the substrate surface rather than the target surface. Highly energetic argon ions when operated in “sputter-etch” mode also remove the undesired thin native oxide layer on the surface, which may have formed during the lithography process. Following sputter-etch, another layer of TiNi film followed by another layer of chromium are sputter deposited on the substrate. The resulting TiNi film is heat-treated at 500° C. in vacuum for crystallization so that the material exhibits the properties of shape memory and superelasticity.
[0026] Photo resist is spin coated again to pattern the layers with designs in mask 2 using the photolithography steps described above. In this step, after etching the top chromium layer, the underlying TiNi layers are also chemically etched with the same mask design in order to define the device's outer features. This is followed by the complete removal of the photo resist layer. To separate the devices from the surface of the substrate, the whole wafer with patterned layers is immersed in a chemical etchant to completely dissolve the sacrificial layer. The etchant for this purpose should etch the sacrificial material selective to the device layer. This etching not only separates the devices from the substrate surface but also selectively creates an empty pocket between the two TiNi layers by etching away the chromium layer from between.
[0027] A pattern of fenestrations 14 ( FIG. 1 ) or 22 ( FIG. 2 ) can be formed in the TiNi layer. To create fenestration patterns, the photo resist layer is patterned using mask 2 , which contains the necessary fenestration patterns. The basic process sequence to fabricate thin film devices with fenestration patterns is the same as the one described above except for the added designs on mask 2 . As described above, after patterning the photo resist layer with fenestration patterns, the chromium and TiNi layers are patterned by chemical etching.
[0028] The released multi-layered thin film devices from the above steps are in planar form which may be of various size and shapes: triangular, rectangular, semicircular etc. These multi-layered thin film devices may then be transformed into their corresponding three-dimensional shapes 12 ( FIG. 1 ) by inserting a stainless steel mandrel into the pocket between the TiNi layers and re-annealing them at 500° C. in vacuum. Re-annealing of the thin film device with an inserted mandrel causes shape-setting according to the shape of the mandrel. Conical and hemispherical thin film devices with appended tentacle-type tails 16 or ridges 18 ( FIG. 1 ), or grooves 24 ( FIG. 2 ) may also be fabricated using the same processes.
[0029] In planar deposition of TiNi to produce three-dimensional structures, multiple layers, are deposited by planar sputtering, with intermediate sacrificial layers patterned selectively, producing structures that can be opened to produce cones, cylinders, and other shapes. Multiple alternating layers of TiNi film and Cr sacrificial layers are applied by sputtering alternatively from a TiNi target, patterning, depositing a sacrificial layer from a Cr target, patterning a second time, and depositing a second TiNi layer. The number of TiNi layers is not limited to two: more complex structures may be formed by iteration of this sequence.
[0030] During fabrication of three-dimensional nitinol thin film structures, a metal such as copper is added as an integral part of the device. This is accomplished either by electroplating or by sputter deposition depending on the design of the finished film contraceptive product. The tails 16 (or strings, ribbons etc.) can be formed in the device as integral features rather than attached or welded onto it. The tails can function as features for retrieval of the device, similar to the regular IUD tail, or as the medicated or contraceptive agent (copper) carrier.
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Contraceptive intrauterine devices made of thin film shape memory alloy materials. The devices are formed in three-dimensional shapes which contact uterus tissue of a human or other mammal to prevent conception. In certain embodiments, structural features such as tails, fenestrations, ridges or grooves are formed on the devices to enhance the contraceptive effect.
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This invention relates to a variable volume air valve which can be incorporated in a plenum directly attached to an air supply terminal in a heating, ventilation and air conditioning system.
BACKGROUND
Variable volume air conditioning systems are well known in tile industry and are commonly used in different kinds of buildings where zoning is required to maintain desired comfort conditions in a plurality of rooms that are served by a single air handling and air conditioning apparatus. The variable volume system and its variations are described in Chapter 2 of American Society of Heating, Refrigeration and Air Conditioning Engineers Inc. (ASHRAE) handbook; Heating, Ventilating and Air Conditioning Systems and Equipment, 1992 Edition. These systems comprise the following as the essential elements:
an air handling and air conditioning apparatus;
a main supply duct to convey conditioned air to the vicinity of the zones served by the air conditioning apparatus;
a plurality of variable air volume (VAV) boxes comprising dampers and actuators, connected to the main supply duct via branches;
distribution ductwork, connected to downstream of VAV boxes to convey conditioned air to a single or a plurality of air terminals located in each zone;
provision for noise reduction in the form of acoustical duct lining of the distribution ductwork or a silencer downstream of each VAV box;
A plurality of zone thermostats, one for each zone, located in one of the rooms within each zone; and
An automatic control system for each VAV box, which may be pneumatic, electric, electronic or digital electronic, to respond signals from the zone thermostat and to reposition the damper in the VAV box, increasing or decreasing the air volume (air flow rate) into the zone. The control system may also receive and respond to signals from a building automation system. Additionally, it may also control reheat or perimeter heating apparatus.
The dampers in VAV boxes are generally round or rectangular single blade type, commonly referred to as butterfly dampers. Rectangular multi-blade dampers are used less commonly, due to their higher cost. When throttling to adjust air volume, these dampers reduce pressure by inducing geometric flow separation and turbulence in the air stream. Through lifts mechanism the total pressure is dissipated into heat. In the mean time, turbulence interaction with damper blades and duct walls and pressure perturbations with frequencies within audible range are perceived as noise by the occupants. The noise level, or more precisely the sound power level is a function of damper geometry, blade position, pressure drop across the damper and air flow rate. A method of predicting this damper noise is given in ASHRAE handbook; HVAC applications, 1991 edition. To attenuate this noise, silencers or acoustically lined distribution ductwork are usually employed downstream of the dampers.
To achieve the best possible temperature comfort, ideally each room should be made an independently controlled zone. However, due to the cost and impracticality of using a VAV box, acoustically lined ductwork or a silencer and distribution ductwork for each room, this is rarely done. The usual practice is to lump a number of rooms of similar cooling/heating characteristics into a single zone, and locate the zone thermostat in one of these rooms. However, there are always variations in room loads and occupants'preferences, therefore this grouping does not always work satisfactorily.
To avoid the compromise mentioned above, during the last few years, a different type of air terminal design has been developed, which incorporates a volume control damper within the air terminal itself, thus eliminates the VAV box. Air volume al each terminal can be controlled individually, therefore each room can be made an individual zone by installing a room thermostat to control the damper inside the air terminal. However, there are two major drawbacks associated with this scheme, as follows:
The first drawback is related to the damper noise. In order to operate at acceptable noise levels, these systems must restrict the pressure drop across the damper within the air terminal (The higher the pressure drop across the damper, the higher the noise). A common method to accomplish this is to control the duct static pressure by means of a separate damper located in a branch duct serving a plurality of such terminals, modulated in response to downstream duct static pressure. The inlet pressure at the terminal is limited to about 60 Pascals. Thus the noise is kept within acceptable limits. Unfortunately, this solution introduces the additional cost and complexity of a pressure regulating damper, a pressure sensor, a control loop and acoustic treatment downstream of the pressure regulating damper.
The second drawback is the difficulty in applying pressure independent controls. Incorporating an air velocity sensor into every branch serving such an air terminal is expensive and impractical, therefore presently systems using this type of terminals do not employ pressure independent controls. Pressure fluctuations at the terminal inlet result in changes in air flow rate, which in turn may cause temperature fluctuations in the room.
BRIEF SUMMARY OF THE INVENTION
I have found that, the two major drawbacks mentioned above can be overcome by a new variable volume air valve that does not create appreciable turbulence, thus generates little noise. This air valve can be used well above 60 Pascals inlet static pressure, eliminating the need for upstream pressure regulation and sound attenuation in most applications. Further, due to its unique shape and method of operation, which will be described in full detail below, the air flow rate through the variable air valve can be measured easily and accurately by measuring the differential pressure at the inlet and outlet of the variable volume air valve and using the valve position input.
The operating principle of the invention can be summarized as follows: The variable volume air valve receives supply air from a main supply duct, and directs the air into an acoustically lined plenum through at least one converging nozzle. The nozzle has a very high aspect ratio (length versus width), and the inflowing air flow is accelerated into a thin sheet of high velocity stream. In accordance with the flow theory, the air velocity at the tip of the nozzle is proportional to the square root of pressure difference between inlet of the variable volume air valve and inside of the plenum. The high velocity air stream discharging from the nozzle rapidly entrains the surrounding air inside the plenum, and its velocity drops considerably within a short distance from the tip of the nozzle. The kinetic energy of the slower but larger mass of the primary and the entrained air is quickly dissipated through friction with acoustically lined plenum walls. The air then flows into the room through a supply terminal attached to the plenum. During the entire process, minimum turbulence, therefore minimum noise is generated. Baffle plates, with or without acoustic lining may be used inside the plenum to promote friction and further attenuate any noise generated at the nozzle. For a given static pressure in the supply duct, the air flow into the plenum can be adjusted very linearly by changing the width, thus the area of the nozzle.
BRIEF DESCRIPTION OF DRAWINGS
FIG. 1 is a combined elevation and section showing a typical supply air duct, an air terminal, and a thermostat arrangement using the invention in a heating, ventilation, air conditioning system;
FIG. 2 is an isometric view of the variable air valve, its plenum and the supply air terminal as an assembly;
FIG. 3 is a section through the preferred embodiment and its plenum along the section line 3--3;
FIG. 4 is a front view of the inlet ring of the variable air valve with respect to air flow direction;
FIG. 5 shows a cross-section of one of the spokes of the inlet ring along the section line 5--5;
FIG. 6 is a front view of the middle ring;
FIG. 7 is a front view of the end plate;
FIG. 8 is a section through a second embodiment of the invention wherein the middle ring is omitted to save cost;
FIG. 9 is a section through a third embodiment of the invention which employs a pneumatic actuator instead of an electric motor;
FIG. 10 is a section through a fourth embodiment of the invention which employs pneumatic actuation as in the third embodiment but the middle ring is omitted to save cost; and
FIG. 11 is a front view of the inlet ring of the third and fourth embodiments of the invention with a static pressure probe attached.
DETAILED DESCRIPTION
The invention will now be described in detail in reference to the drawings briefly described above.
In reference to FIG. 1, the preferred embodiment of the variable volume air valve 1 is installed in a plenum 2 which is directly on top of, and attached to a supply air terminal 3. The air terminal can be a linear slot diffuser, a square or a round diffuser, or any suitable diffuser. A branch duct 4, preferably a piece of flexible duct connects the variable volume air valve 1 to a supply duct 5. An electronic controller is located in a control box 6 attached to the plenum. The electronic controller features one or more microcontrollers which communicate with the room thermostat 7, a building automation system and control the variable volume air valve 1 and perimeter heating valve 8. Preferred communication medium is a single pair of twisted wire, although other media such as coaxial cable, fibre optic cable, even electromagnetic waves can be employed. The control box requires a power supply, which is not shown for sake of simplicity.
In reference to FIG. 2, the variable volume air valve 1 is shown in its plenum 2 which is attached to a linear supply air terminal 3. The supply air terminal may be supported by the T-bars of the suspended ceiling. The plenum may further be supported from the building structure. A duct collar 9 is connected to a branch duct 4 as shown in FIG. 1. In reference to FIG. 3, the variable volume air valve 1 comprises four major components; an inlet ring 10, a main shaft 13, a middle ring 14 and an end plate 19 with gear and motor housing 22. The inlet ring 10 which ultimately supports all other components of the variable air valve 1 is rigidly attached to and supported by the duct collar 9. The duct collar itself is attached removably to the plenum 2 by fasteners, such as sheet metal screws. In this fashion the variable volume air valve 1 may be quickly removed from the plenum 2 for inspection and servicing. The inlet ring 10 has a minimum of two, preferably three spokes 11 and a hollow hub 12. The upstream end of the main shaft 13, relative to the air flow direction indicated by arrows, is rigidly attached to the hub 12 of the inlet ring 10, and does not rotate. The middle ring, comprising a minimum of two, preferably three spokes 15, a hub 16 and a sleeve 17 is mounted on the main shaft 13 and is free to slide along the main shaft 13. The sleeve 17 is made of a material with low coefficient of friction, such as filled plastic. A compression spring 18 pushes the middle ring 14 away from the inlet ring 10. The end plate 19 comprising a motor and gear housing 22 and a sleeve 20 made of a low friction material is mounted on the main shaft 13, downstream of the middle ring 14. An additional compression spring 21 pushes the end plate 19 away from the middle ring 14 so that, provided the two compression springs 18, 21 are of equal length and spring constant, the middle ring 14 will always automatically assume a halfway position between the inlet ring 10 and the end plate 19.
The spokes 11 of the inlet ring 10 and the middle ring have an airfoil cross-section, as shown in FIG. 5, to reduce pressure drop and minimize creation of turbulence.
In reference to FIG. 3, the downstream end of the main shaft 13 with respect to air flow direction is screw threaded. The motor and gear housing 22 contains an electric motor 23, a reduction gear train 24 and a captive nut 25 which is also the last driven gear in the gear train. The captive nut 25 is in contact with the sleeve 20 of the end plate through a thrust ball bearing 26 and thus limits the movement of the end plate 19 towards the downstream end of the main shaft 13 under the spring force. The captive nut 25 rides along the main shaft 13 when rotated by the motor 23 and the gear train 24 and thus moves the end plate 19 towards or away from the inlet ring 10 depending on the direction of rotation. The end plate 19, and the motor and gear housing 22 are prevented from rotating about the main shaft 13 axis due to the gear reaction force by a torque arm 27, and a shorter torque shaft 28 and the two rollers 29. One end of the torque arm 27 is rigidly attached to the downstream end of the main shaft 13 whereas the other end rigidly supports the torque shall 28, which is parallel to the main shaft 13. The two rollers 29 are located within the motor and gear housing 22, their axis being in a plane vertical to the main shaft 13 axis. The rollers 29 are rotatably attached to the motor and gear housing 22 and ride along the torque shaft 28 as the end plate 19 moves relative to the main shaft 13, transferring the gear reaction force to the torque shaft 28.
A position sensing device 30, such as a optical encoder or a hall effect revolution counter, is located within the motor and gear housing 22 and provides an input liar the electronic controller indicative of the position of the end plate relative to the main shaft 13, thus also indicative of the width of the nozzles 31, 32 that form between the rims of the inlet ring 10 and the middle ring 14 and between the rims of the middle ring 14 and the end plate 19 respectively.
The thrust ball bearing 26 has V shaped grooves and is always loaded by the force of the compression springs 18, 21. These V-grooves and the spring force help align the axis of the end plate with the axis of the captive nut 25.
Operating principle of the air valve is as follows: In reference to FIG. 3, the rims of the inlet ring 10, the middle ring 14 and the end plate 19 form two converging nozzles 31, 32 through which air flows into the plenum in a radial direction relative to the axis of the main shaft 13. The static pressure is converted into velocity pressure as the entering air is accelerated to a theoretical final velocity which may be calculated according to the following formula given in ASHRAE Handbook, Fundamentals, 1993 for standard air at 1.204 kg/m 3 density: ##EQU1## Where V is the velocity of air leaving the nozzle in m/s and P is the velocity pressure in Pascals, which is equal to the total pressure difference between the inlet and a point inside the plenum, assuming negligible pressure loss in the nozzle itself. Static pressure regain is also negligible due to the shape of the nozzles. The nozzles 31, 32 have very high aspect ratio (Length versus width), especially when the end plate 19 is moved closer to the inlet ring 10. The thin sheet of air flowing through the nozzles 31, 32 rapidly entrains the surrounding air, and within a short distance, the flow velocity is reduced to a fraction of the velocity at the tip of the nozzle. The kinetic energy of the air stream, on the other hand, remains about the same, since it has been transferred to a much larger mass of air moving at a slower speed. However, this energy can be quickly dissipated through friction with the acoustically lined plenum 2 walls. There is no part located in the high velocity air stream to create turbulence, thus noise. Any turbulence created in the slower moving air stream is much less severe, and so is the resulting noise. The nozzles 31, 32 are deliberately positioned away from the plenum 2 walls to prevent impingement of flow on the walls, thereby reducing its capacity to entrain surrounding air.
The air flow rate through the variable volume air valve can be measured and calculated by the electronic controller as follows: A pressure sensor located in the control box 6 sends a signal corresponding to the pressure difference between its high pressure port and the low pressure port. The high pressure port is connected to the total pressure probes 33 that are attached to, or form a part of the inlet ring 10. The low pressure port opens to a corner of the plenum where the air velocity is low. The electronic controller keeps track of the position of the end plate 19 by counting motor 23 or gear 24 revolutions in each direction of rotation, therefore it "knows" the nozzle width, thus nozzle area of the nozzles 31, 32. From the differential pressure signal, the air velocity is calculated according to the formula given above. Flow area multiplied by flow velocity gives the air flow rate.
Since the differential pressure is measured across the nozzles 31, 32, the signal level is always higher compared to a differential pressure signal that can be obtained by a pitot tube or impact probe located in the branch duct serving the plenum. This is because the nozzle area is much smaller compared to the branch duct cross sectional area where the pitot tube or impact tube would normally be installed. Further, as the variable volume air valve throttles, the air velocity in the branch duct decreases, and the pitot tube or impact probe signal would decrease too, whereas the differential pressure signal across the nozzles will not change as long as the inlet pressure does not change. This higher signal level allows more accurate measurements, or alternatively, less sensitive therefore less expensive pressure sensors may be employed for the same air flow rate measurement accuracy.
During the cooling mode, in reference to FIG. 1, the room thermostat 7 sends a signal corresponding to actual room temperature, and an error signal corresponding to the difference between its set point and the actual room temperature. The electronic controller compares the error signal with a previously received error signal, and calculates the error change. Using the error signal and the error change, the controller calculates the required correction to the present air flow rate, then re-positions the end plate 19 to obtain the new air flow rate. The control action is essentially proportional-integral type.
A temperature sensor within the plenum 2 monitors the supply air temperature. If the supply air temperature is higher than the room temperature, heating mode is automatically selected, and control action of the variable volume air valve is reversed. If the room temperature set point cannot be maintained at the maximum allowed flow rate, a reheat or perimeter heating system, if there is one, is activated and controlled by the signals from the electronic controller.
Building operators can communicate with the air valve electronic controller through the building automation system to set maximum, minimum allowable air flow rates, and to read current air flow rate. Another method is to plug in a portable computer or a similar instrument into the room thermostat and communicate with the air valve controller.
It should be understood that file scope of tiffs invention is not limited to the specific geometrical shape illustrated in FIGS. 3, 4, 5, 6 and 7. To reduce manufacturing costs, the middle ring 14, its sleeve 17 and one of the compression springs 21 may be omitted. This second embodiment of the air valve is illustrated in FIG. 8. The result of this modification is reduced nozzle aspect ratio, longer distance for equivalent air flow velocity reduction, and higher operating noise, which may be tolerated in less critical applications, or in systems where the inlet static pressures are lower.
Further, pneumatic actuation may be used instead of the electric motor to move the end plate relative to the inlet ring. A third embodiment of the invention is shown in FIG. 9. In reference to FIG. 9, a pneumatic piston 34 is rigidly attached to the downstream end of the main shaft 13. There is no external threading on the downstream end of the main shaft 13. In reference to FIG. 3, the motor and gear housing 22, the torque arm 27 and the torque shaft 28, and the rollers 29 are also omitted. In reference to FIG. 9, a ring shaped sleeve 35 is rigidly attached to the end plate 19 and together they form a pneumatic cylinder. A flexible diaphragm 36 seals the clearance between the piston 34 and the cylinder formed by the end plate 19 and the sleeve 35. The outer edge of the diaphragm 36 is compressed and held in place between the end plate 19 and the sleeve 35. The inner edge of the diaphragm 36 is compressed and held in place between two smaller sleeves 39, 40 which are secured to the end plate by a lock nut 41. This third embodiment is controlled by an industry standard, pressure independent pneumatic VAV box controller, also known as velocity controller, in conjunction with an industry standard pneumatic room thermostat. To provide a static pressure signal for the pneumatic VAV box controller, a static pressure probe 38, in the form of a ring shaped tube with a multiple of small holes drilled at selected locations to give a stable pressure signal, is pressed into slots in the spokes 11 of the inlet ring 10. FIG. 11 shows the front view of the inlet ring 10 with the static pressure probe 38 inserted in the slots of the spokes 11. One end of the static pressure probe is sealed, the other end is connected to the corresponding port on the pneumatic VAV box controller with pneumatic tubing. Similarly, the total pressure probes are connected to a corresponding port on the pneumatic VAV box controller. Electronic controllers are not used, and communications with a building automation system is not possible. The pneumatic VAV box controller receives a signal from the room thermostat, another signal from the total pressure probes from the total pressure probes 33 and a third signal from the static pressure probe 38, and generates a pneumatic output signal corresponding to a new valve setting. Upon increasing output signal value, the control air under pressure is admitted into the cylinder through a pneumatic tube 37, pushing the end plate 19 away from the piston 34, towards the inlet ring 10, resulting in reduced nozzle area. Reverse happens on a reduction in decreasing output signal value. The operating principle and method are similar to those of the first embodiment.
A fourth embodiment of the invention is shown in FIG. 10. The fourth embodiment employs pneumatic actuation as described above for the third embodiment, and further omits, in reference to FIG. 9, the middle ring 14, its sleeve 17 and one of the compression rings 21 to reduce manufacturing costs. The result of this modification is similar to that of the second embodiment, as described earlier.
The inlet and middle rings, and the end plate can be manufactured of preferably die cast or permanent mold cast aluminum or zinc alloy, or may be injection molded of a suitable plastic. All other parts can be manufactured of any suitable material and process.
The present invention has been shown and described with respect to four exemplary embodiments. However, other embodiments based on the principles of file present invention should occur to those of ordinary skill in the art. Such embodiments are intended to be covered by the claims.
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An apparatus for temperature control in a room by adjusting supply air flow rate in response to a room thermostat in a ducted air conditioning system where a plurality of rooms are supplied by a single air handling unit. The apparatus may be installed in a plenum which is directly mounted on an air supply terminal. The apparatus is connected to a main supply duct with a branch duct, and as a result of its favorable geometry and throttling method, operates at low noise levels. The apparatus employs high aspect ratio converging nozzles to allow incoming air accelerate into a thin sheet of high velocity air stream. Air flow rate is adjusted simply by changing tile nozzle area. This high velocity air stream entrains surrounding air within the plenum and slows down. Its energy is dissipated through friction with acoustically lined plenum walls. In tiffs process, little noise generated. The apparatus, due to its special shape, allows accurate measurement of air flow rate. The apparatus incorporates a control system for adjusting the air flow rate in response to a room thermostat. The control system may further comprise means for controlling supplementary heaters or heating valves.
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FIELD OF THE INVENTION
[0001] This invention relates to compact solid state lasers.
BACKGROUND OF THE INVENTION
[0002] Femtosecond lasers are usually more complicated than other lasers emitting continuouswave, Q-switched, or picosecond radiation. One reason for this is that femtosecond generation requires laser materials with a spectrally broad emission band, in comparison for example to the well-known laser material Nd:YAG, leaving a limited number of laser materials suitable for femtosecond generation. Additionally, femtosecond lasers need some group velocity dispersion compensation, which usually requires additional intra cavity elements, such as a prism pair, thereby adding complexity to the system. An example of a femtosecond laser is the green-pumped Ti:sapphire laser. More compactness is obtained by directly diode pumping suitable laser materials, such as Nd:glass, Cr:LiSAF, Yb:glass, etc (see for example in D. Kopf, et al., “Diode-pumped modelocked Nd:glass lasers using an A-FPSA”, Optics Letters, vol. 20, pp. 1169-1171, 1995; D. Kopf, et al., “Diode-pumped 100-fs passively modelocked Cr:LiSAF using an A-FPSA”, Optics Letters, vol. 19, pp. 2143-2145, 1994; C. Honninger, et al., “Femtosecond Yb:YAG laser using semiconductor saturable absorbers”, Optics Letters, vol. 20, pp. 2402-2405, 1995). These laser systems, however, are not perfectly compact in the sense that they usually use two laser diodes as pump sources that are imaged into the laser crystal using imaging optics. The latter are relatively large in size and could still be made considerably more compact. Furthermore, the resonator comprises two arms that have to be aligned accurately with respect to each other and with respect to the pump beam, respectively, resulting in a number of high-accuracy adjustments to be performed. Quite commonly, focusing lenses with a focal length of 75 mm or longer are used to focus the pump light into the laser crystal through one of the curved cavity mirrors, following a delta-type laser cavity scheme. Such a cavity scheme essentially does not allow for straight-forward size reduction of the pump optics. Another approach (see for example S. Tsuda, et al., “Low-loss intracavity AlAs/AlGaAs saturable Bragg reflector for femtosecond mode locking in solid-state lasers”, Optics Letters, vol. 20, pp. 1406-1408, 1995) places the laser medium at the end of the laser cavity, thereby allowing for more compact pump focusing optics with a potentially shorter working distance and reducing the number of adjustments required. However, since one cavity end is taken by the laser medium, both the semiconductor element (semiconductor saturable absorber mirror, SESAM) and the prism sequence for dispersion compensation need to be placed toward the other end of the laser resonator. Since the spot size on the SESAM needs to be small enough for saturation in that setup, the focusing mirror towards that cavity end does not leave enough room for a prism pair to compensate for the group velocity dispersion. However a total of four prisms had to be implemented for that purpose.
SUMMARY OF THE INVENTION
[0003] The invention comprises a compact solid state laser. The laser medium is positioned at or close to one end of the laser cavity and pumped by at least one pump source or laser diode. The pumping can be done by one or two laser diodes including imaging optics of compact size (10 cm or less), respectively, due to the arrangement of the cavity end and pumping optics, and is suitable for achieving reasonable gain even from low-gain laser materials. For femtosecond operation, the laser resonator is laid out such that both a semiconductor saturable absorber mirror and a prism pair are located toward the other end of the cavity, and the laser mode on the SESAM and the prism sequence length fulfill the requirements that have to be met for stable femtosecond generation. It is another object of the invention to provide a semiconductor saturable absorber mirror (SESAM) having a structure which comprises a plurality of alternating gallium arsenide (GaAs) and aluminum arsenide (AlAs) or Aluminum gallium arsenide (AlGaAs) layers, each layer having an optical thickness corresponding substantially to one quarter wavelength, a gallium arsenide (GaAs) substrate at a first face of said plurality of alternating layers, a gallium arsenide (GaAs) or AlGaAs structure integrating an absorber layer at a second face of said plurality of alternating layers, and plurality of dielectric layers at a face of said gallium arsenide (GaAs) opposite the one in contact with said second face, whereby the overall structure shows resonant behaviour. Such a SESAM may be implemented into a solid state laser as described above. It is a further object of the invention to provide a special setup for a solid state laser, wherein the laser comprises a laser gain medium, pumping means for pumping said laser gain medium, a laser cavity with a semiconductor saturable absorber mirror (SESAM) at one end of said cavity, and wherein said cavity contains a prism pair followed by a telescope.
BRIEF DESCRIPTION OF THE DRAWINGS
[0004] The invention and its advantages shall become more apparent from reading the following description of the preferred embodiments, given purely by way of non-limiting illustrative examples with reference to the appended drawings, in which:
[0005] [0005]FIG. 1 is a schematic representation of a laser gain setup according to a preferred embodiment of the invention;
[0006] [0006]FIG. 2 is a schematic representation of an unfolded propagation of the laser mode cavity of a femtosecond cavity;
[0007] [0007]FIG. 3 is a schematic representation of an implementation of the cavity of FIG. 2 forming a small-size setup;
[0008] [0008]FIGS. 4 a and 4 b are schematic representations of implementations of the cavity of FIG. 2 with a relatively larger prism sequence, followed by an intracavity telescope and the cavity end.
[0009] [0009]FIG. 5 shows an example of a semiconductor saturable absorber structure which can be used in combination with prism sequences.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0010] The general setup of a compact, ultra-fast laser according to a preferred embodiment of the invention shall be described with reference to FIG. 1. The gain section of the laser setup comprises a laser gain medium 1 which is located in the vicinity of a first end of a laser cavity (see laser cavity mode axis 2 ). The laser gain medium 1 can even be the laser cavity end itself if one side 3 of the laser material is coated for reflectivity at the laser wavelength. A flat-brewster-cut laser medium may be used, where the flat side is coated for reflectivity at the laser wavelength and for high transmission at the wavelength of the pump laser diode 4 used in the setup. The laser diode beam is preferably collimated in the (vertical) fast-divergent axis by means of a cylindrical micro lens attached close to the laser diode 4 so that the pump beam 5 diverges at a reduced vertical divergence angle. The pump laser diode 4 can be for example a 100 micron wide laser diode emitting at a power of 1 or more Watts at a wavelength of 800 nm. It serves to pump a laser medium such as Nd:glass. A collimating lens 6 and focusing lens 6 ′ are used to re-image the pump beam into the laser medium 1 . Imaging elements including the microlens, and lenses 6 and 6 ′ may be replaced by any imaging optics of similar compactness and imaging properties. Because of the potentially short working distance between lens 6 ′ and the laser medium 1 , the pump elements 4 , 6 , 6 ′ can cover as short a distance, on the order of 10 cm or less.
[0011] The setup uses a second pump source comprising a laser diode 7 , collimating lens 8 , prism 9 , focusing lens 10 , and dichroic mirror 11 . The pump beam of laser diode 7 is first collimated with lens 8 and then enters prism 9 . When the beam emerges from the prism 9 , it has been expanded in the tangential plane, as indicated in FIG. 1. This results in a smaller spot in air after focusing lens 10 . One or the other of these laser diodes, or both combined, may produce a pump intensity of 10 kW per square centimeter or more. When entering the laser medium 1 through the Brewster face, however, the spot will be expanded again due to the Brewster face refraction. Therefore the prism 9 is used to pre-compensate the expansion due to the Brewster face, which results in similar spot sizes within the laser medium 1 from both pump sources. Additionally, the prism 9 is used to compensate for the beam axis angle due to the Brewster face of the laser medium. The pump source comprising laser diode 7 , lens 8 , prism 9 , and lens 10 can have a degree of compactness similar to that of the first pump source, assuming that dichroic mirror 11 is placed close enough to the laser medium 1 , reducing the working distance between the lens 10 and the laser medium. The dichroic mirror 11 is highly transmissive for the pump wavelength of laser diode 7 and highly reflective for the laser wavelength. In this way, the resonator mode 2 is directed from the laser medium 1 towards a curved cavity mirror 12 and some further plane folding mirrors 13 and 13 ′, etc., for example. When the focus spot of the pump sources 4 and 7 is chosen to be located within the laser medium 1 , this pump arrangement is suitable for pumping low-gain laser materials such as Nd:glass, Cr:LiSAF, Yb:glass, Yb:YAG, Yb:KGW, etc (low-gain meaning less gain than Nd:YAG). This pump arrangement can therefore be used for pumping broad emission band laser materials suitable for femtosecond generation. It may however also be used for pumping any solid state laser material for other purposes including continuous wave, Q-switched, or picosecond operation.
[0012] For a femtosecond laser setup, above setup can be combined with the laser mode shown in FIG. 2, which illustrates an example of an unfolded propagation of the laser mode throughout a possible femtosecond cavity. The lenses indicate curved cavity mirrors that refocus the cavity mode. Laser medium 1 in the vicinity of one cavity end 3 ′ has a mode radius on the order of 30×45 um (microns). The cavity end 3 ′ may be a mirror with characteritsic features similar to thoses of the coated side 3 of the laser material in FIG. 1. Curved mirror 12 (whose radius of curvature is for example 200 mm) is located some 120 mm away from the laser medium 1 , and therefore re-images the cavity mode into a waist 14 . The cavity mode then further diverge to a spot size that is on the order of 2-3 mm in diameter at another cavity mirror 15 (whose radius of curvature is for example 600 mm) after a distance 16 of around 1400 mm. The relatively large mode diameter at cavity mirror 15 results in a small mode diameter 16 a at the laser cavity end which contains a SESAM (semiconductor saturable absorber mirror) 17 . An example of a design for a suitable SESAM is given in D. Kopf, et al., “Diode-pumped femtosecond solid state lasers based on semiconductor saturable absorbers”, SPIE Proceedings, “Generation, Amplification and Measurement of Ultrashort Laser Pulses III”, 28-30 January 1996, San Jose, Calif., The International Society for Optical Engineering). This laser cavity has a large working distance of around 400 mm between element 15 and 17 such that it can contain a prism pair 18 , 18 ′ (shown schematically, see also FIG. 4 b ) consisting of two SF10 Brewster prisms that are separated by some 350 mm for sufficient group velocity dispersion compensation. The cavity of FIG. 2 can be folded with plane highly reflective mirrors at any location as required to fit the setup into small boxes. One example of a final small-size setup is shown in FIG. 3. Here the surface 3 of the laser medium 1 is made partially transmissive for the laser wavelength such that a fraction of the intracavity power is outcoupled and furthermore separated from the incident pump beam by dichroic mirror 3 b, resulting in laser output beam 3 c. Prism sequences that are considerably longer than those in above setup can be achieved at the expense of a larger spot size at the end of the prism sequence.
[0013] [0013]FIGS. 4 a and 4 b illustrate such examples of prism sequences. For such longer prism sequences 19 , for example 500-1000 mm long or longer, the spot size 20 at the SESAM could be too large for achieving saturation at femtosecond operation as required for stable ultra fast performance. To solve this problem, it can be useful to extend the cavity by a telescope 21 . In this way, the mode size reduces according to the telescope factor to a mode size 21 ′ (FIG. 4 a ), where the SESAM is positioned. Simultaneously, the parallelism between two dispersed beams 22 and 22 ″ is preserved after the telescope, and corresponding beams 23 and 23 ′ (FIG. 4 a ) are perpendicular to the end mirror (which is the SESAM) 24 as required for the lasing condition and for obtaining negative group velocity dispersion from the prism sequence 19 . Prism sequences of considerable length can also be used in combination with a special SESAM structure such that saturation is obtained at lower energy densities for stable ultra fast laser operation.
[0014] [0014]FIG. 5 shows an example of such a semiconductor saturable absorber structure, representing the layers along the surface normal to its surface. Firstly, 30 pairs of layers of alternating gallium arsenide (GaAs) and aluminium arsenide (AlAs) layers 43 each with an optical thickness corresponding to a quarter wavelength are applied onto a gallium arsenide (GaAs) substrate 48 . This can be achieved by means of growth process using molecular beam epitaxy (MBE). However, other known epitaxy processes and usual in this field are also suitable. The GaAs/AlAs pairs of layers are transparent for the laser wavelength of 1064 nm and result, in the example of FIG. 5, in a Bragg mirrorlike coating structure with a high reflection factor close to 100% with a wavelength of 1064 nm if the thickness of GaAs is selected at approx. 72.3 nm and that of AlAs at approx. 88 nm, each corresponding to about an optical quarter wavelength. Then, a further GaAs layer 44 integrating an approx. 10 nm thin absorber layer of indium gallium arsenide (InGaAs) material is assembled onto this standard GaAs/AlAs Bragg mirror structure. The optical total thickness of this GaAs layer with integrated absorber layer 47 corresponds to half a wavelength, that is the physical film thickness is approx. 145 nm. The indium content of the absorber layer 47 is determined so that an absorption is obtained at the laser wavelength of 1064 nm, that is the band-edge is approx. 1064 nm or a few 10 nm higher than the laser wavelength, e.g. at 1064-1084 nm. This corresponds to an indium content of about 25 percent. With higher intensity and pulse energy density, a saturation of the absorption of this absorber layer 47 occurs, i.e. it is lower. In the case of particularly thin layers of less than 20 nm thickness, by additionally finely adjusting the indium content, the exciton peak near the band edge, generated by the exciton absorption behaviour of thin layers to be quantizised, can be adjusted exactly to the laser wavelength, resulting again in an even more pronounced saturable absorption at that wavelength. Finally, another three or more pairs of dielectric layers transparent for the layer wavelength are applied, beginning with that layer 45 having a higher index of refraction n=2.02 and continuing with that layer 46 having a lower index of refraction of 1.449 at a wavelength of 1064 nm. The process of electron beam coating, widespread in the optical coating field, is suitable to achieve this. Other optical coating processes, such as for example ion beam sputtering, are also suitable and can have the advantage of resulting in lower losses. As optical layer materials, those with an index of refraction of 1.449 and 2.02 at a wavelength of 1064 nm were used. However, a large number of other materials can be used as long as adhesion to GaAs and transparency at the laser wavelength are ensured. Because the three or more final dielectric pairs have a reversed order in terms of their index of refraction, with respect to the order of the refractive indexes of the layers underneath, the structure is at resonance. By virtue of the resonant saturable absorber mirror structure, this device has a saturation fluence which can be on the order of a few microjoules per square centimeter (depending on the number of dielectric top layers), which is considerably lower than those of existing SESAMs, and can therefore be well suited for femtosecond or pulsed laser generation from setups where the laser mode on the saturable absorber device is usually too large for saturation. Thanks to the resonant structure, one single or a low number of single thin saturable absorber layers introduce an increased saturable absorption for the overall device in comparison to those structures which do not use a resonant structure. When the saturable absorber layers introduce strain due to a lattice mismatch (which is the case for Indium Gallium Arsenide within GaAs), this structure helps reduce strain without reducing the saturable absorption effect for the overall device, resulting in less material defects and in improved long-term properties of the device.
[0015] While there has been described herein the principles of the invention, it is to be clearly understood to those skilled in the art that this description is made only by way of example and not as a limitation to the scope of the invention. Accordingly, it is intended, by the appended claims, to cover all modifications which fall within the spirit and scope of the invention.
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The solid state laser comprises a laser gain medium, pumping means for pumping the laser gain medium, and a laser cavity having a first end and a second end, wherein the laser gain medium is at, or in the vicinity of, said first end of said cavity. A semiconductor saturable absorber mirror (SESAM) can be placed at the second end of the cavity. The laser gain medium can comprise at least one face for receiving pumping energy from the pumping means, the face being made reflective at a laser frequency of the laser, so that it can form the first end of the laser cavity. The resulting setup can used for generating femtosecond laser pulses.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation application of, and claims priority under 35 U.S.C. § 120 to, U.S. application Ser. No. 11/394,691, filed on Mar. 31, 2006, now U.S. Pat. No. 7,288,319 which is a continuation of Ser. No. 10/402,068, now U.S. Pat. No. 7,053,134, filed on Mar. 28, 2003, which is a continuation of U.S. application Ser. No. 10/116,330, filed on Apr. 4, 2002, now abandoned each of which is incorporated herein by reference in its entirety.
TECHNICAL FIELD
The invention relates generally to forming a chemically cross-linked particle and more particularly to forming a chemically cross-linked particle of a desired shape and diameter.
BACKGROUND INFORMATION
Polymeric microspheres (i.e., microspheres formed at least in part from a polymer) are used in medical and industrial areas. These microspheres may be used as drug delivery agents, tissue bulking agents, tissue engineering agents, and embolization agents, for example. Accordingly, there are a variety of methods directed towards preparing polymeric microspheres. Typical methods include dispersion polymerization of the monomer, potentiometric dispersion of dissolved polymer within an emulsifying solution followed by solvent evaporation, electrostatically controlled extrusion, and injection of dissolved polymer into an emulsifying solution through a porous membrane followed by solvent evaporation.
Additional methods of preparing polymeric microspheres include vibratory excitation of a laminar jet of monomeric material flowing in a continuous liquid medium containing a suitable suspending agent, irradiation of slowly thawing frozen monomer drops, emulsification and evaporation, emulsification and evaporation using a high shear air flow, and continuous injection of dissolved polymer into a flowing non-solvent through a needle oriented in parallel to the direction of flow of the non-solvent.
SUMMARY OF THE INVENTION
The present invention facilitates production of microspheres having small diameters in a manner that is generally independent of viscosity and density. This is accomplished through the use of an uncross-linked polymer precursor in solid form, and a mechanical technique of compacting the precursor into a desired shape.
Accordingly, in one aspect, the invention involves a method of forming a chemically cross-linked particle of a desired shape and diameter. The method includes providing an uncross-linked resin (e.g., polyvinyl alcohol) in particulate form, agglomerating the resin into a mass of a desired shape with a desired diameter, compressing the mass, and cross-linking the mass to thereby form the chemically cross-linked particle. An advantage of the present invention is the ability to avoid melting the resin in order to attain the desired shape. This is useful, for example, in connection with thermally unstable polymers.
In one embodiment, the method further includes adding a binding agent (such as a starch or a sugar) to the resin and later removing the binding agent by exposing the particle to a solvent formulated to selectively dissolve the binding agent. The binding agent serves to hold the mass of uncross-linked resin particles together in the desired shape until the mass is cross-linked. In other embodiments, the binding agent comprises a polymer having a melting temperature lower than the melting temperature of the resin. In this way, the polymer becomes part of the chemically cross-linked particle.
In another embodiment, the method further includes cross-linking the mass by exposing the mass to actinic energy such as an electron beam, ultraviolet radiation, or gamma radiation.
In still another embodiment, the method further includes cross-linking the mass by exposing the particle to a gaseous cross-linking agent.
In yet another embodiment, the method further includes agglomerating the resin into a mass in the shape of a sphere with a diameter of less than 600 microns.
In another aspect, the invention involves a method of forming a chemically cross-linked particle of a desired shape and diameter. The method includes providing an uncross-linked resin in particulate form, adding a binding agent to the resin, and agglomerating the resin into a mass. The method further includes heating the mass to a temperature that is both above the melting point of the binding agent and below the melting point of the resin, compressing the mass into a desired shape with a desired diameter, and cooling the mass to a temperature below the melting point of the binding agent. The mass is then cross-linked to form the chemically cross-linked particle.
In one embodiment, cross-linking the mass includes exposing the mass to actinic energy, such as an electron beam, ultraviolet radiation, or gamma radiation.
In another embodiment, cross-linking the mass includes exposing the mass to a gaseous cross-linking agent.
In still another embodiment, the method further includes removing the binding agent by heating the chemically cross-linked particle to a temperature above the melting point of the binding agent. The binding agent is thereby melted out of the chemically cross-linked particle.
In yet another embodiment, the method further includes removing the binding agent by exposing the particle to a solvent formulated to selectively dissolve the binding agent.
The foregoing and other objects, aspects, features, and advantages of the invention will become more apparent from the following description and from the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings, like reference characters generally refer to the same parts throughout the different views. Also, the drawings are not necessarily to scale, emphasis instead generally being placed upon illustrating the principles of the invention.
FIG. 1 is an illustrative flow diagram depicting the steps of forming a chemically cross-linked particle of a desired shape and diameter according to one embodiment of the invention.
FIG. 2 is an illustrative flow diagram depicting the steps of forming a chemically cross-linked particle of a desired shape and diameter according to another embodiment of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring to FIG. 1 , in one embodiment, the method of forming a chemically cross-linked particle of a desired shape and diameter is a mechanical process rather than a chemical process. First, an uncross-linked resin or polymer in particulate form is provided (Step 102 ). In one embodiment, the resin is a polyvinyl alcohol resin in particulate form having an average diameter of approximately 75 microns, such as a 99% hydrolyzed polyvinyl alcohol (e.g., product #341584 from Aldrich Chemical or Gohsenol NM-11 from Nippon Synthetic Chemical Industry Co.). In other embodiments, polymers such as polyvinyl acetate, vinyl polymers, polyamides, polyureas, polyurethranes, methacrylates, polyvinyl alcohols, or polymers having a pendant ester group that is easily cross-linked (or derivatives thereof) can be used. For many applications (e.g., embolics), the polymer is desirably hydrophilic.
A binding agent is then mixed with the resin particles (Step 104 ). The binding agent serves to hold the resin particles together before they are cross-linked. In some embodiments, the binding agent is a starch or a sugar (e.g., sucrose). In other embodiments, other materials such as alginates, polysaccharides, proteins, carrageenan, or vegetable gums, for example, can be used as binding agents. In still other embodiments, the binding agent can be a blend of one or more of the above synthetic or naturally occurring materials.
After the uncross-linked resin is mixed with the binding agent, the resin particles are agglomerated into a mass of a desired shape with a desired diameter (Step 106 ). In one embodiment, the resin particles are forced into a mold (using conventional plastic injection molding techniques) conforming to the desired shape and diameter. In another embodiment, the resin particles are pressed into the desired shape and diameter using conventional compression equipment. In still another embodiment, a punch is used to punch the desired shape out of a solid sheet of the resin. In yet another embodiment, a combination of static electricity and mechanical vibration or agitation is applied to the uncross-linked resin to cause the uncross-linked resin to agglomerate. In another embodiment, the uncross-linked resin particles are agglomerated by being put into a suspension and rotated. Rotation forces the resin particles to collide with each other and form a mass that can thereafter be cross-linked. The size of the mass is selected by controlling the rate of rotation. As the rotation speed increases, so does the number of resin particle collisions. However, the forces acting to pull the agglomerated mass apart also increase. The final size of the mass is a function of rotation speed and the force acting to pull the mass apart.
Preferably, the technique used to form the particle involves, or is followed by, some form of compression in order to ensure that the resin particles stay together in the desired shape, such as a sphere (Step 108 ). For example, molding can involve pneumatic, hydraulic, or other compression of the resin-filled mold form. Rotation generally provides adequate compression force.
After the mass is compressed, it is cross-linked to form the chemically cross-linked particle (Step 110 ). In some embodiments, cross-linking the mass is accomplished by exposing the mass to actinic energy, such as an electron beam, ultraviolet radiation, or gamma radiation. In other embodiments, cross-linking the mass is accomplished by exposing the mass to a gaseous cross-linking agent such as formaldehyde, glutaraldehyde, or an acid, for example. Polyvinyl alcohol and other polymers can be cross-linked using any of these techniques.
After the mass is chemically cross-linked and a chemically cross-linked particle is formed, the binding agent may be removed from the particle by exposing the particle to a solvent (Step 112 ) formulated to selectively dissolve the binding agent. For example, a polar solvent (e.g., water or alcohol) can be used to dissolve the binding agents discussed above.
Referring to FIG. 2 , in another embodiment, the binding agent is a polymer with a melting temperature that is lower than the melting temperature of the resin. First, an uncross-linked resin or polymer in particulate form is provided (Step 202 ). Next, a binding agent is added to the resin ( 204 ). After the uncross-linked resin is mixed with the binding agent, the resin particles are agglomerated into a mass of a desired shape with a desired diameter (Step 206 ).
Exemplary binding agents useful in connection with this embodiment include Methocell methoylcellulose, hydroxypropyl methylcellulose, Ethocell Standard and Premium (organic solvent soluble) from Dow Chemical Co., Avicel PH-001 and Avicell PH-002 microcrystalline cellulose (water soluble) from Asahi Kasei Corp, potassium alginates, sodium alginates, or PEG 1400 (polyethylene glycol), for example. The agglomerated mass of binding agent and resin is heated to a temperature above the binding-agent melting point but below the resin melting point (Step 208 ). After the mass is heated, it is compressed (Step 210 ). Compression ensures that the resin particles stay together in the desired shape, such as a sphere, for example. After the mass is compressed, it is cooled (Step 212 ). Upon cooling, the binding agent resolidifies and the shape imparted to the mass remains “set.”
After the mass is cooled, it is then cross-linked to form the chemically cross-linked particle (Step 214 ). The binding agent may remain in the particle during and following cross-linking of the resin. In some embodiments, cross-linking the mass is accomplished by exposing the mass to actinic energy, such as an electron beam, ultraviolet radiation, or gamma radiation. hi other embodiments, cross-linking the mass is accomplished by exposing the mass to a gaseous cross-linking agent such as formaldehyde or glutaraldehyde, for example. After the mass is cross-linked, the resulting particle can be again heated to a temperature above the binding-agent melting point so that the binding agent can be melted out of the particle (Step 216 ). The binding agent may also be removed from the particle by exposing the particle to a solvent formulated to selectively dissolve the binding agent. For example, a polar solvent (e.g. water or alcohol) can be used to dissolve some of binding agents discussed above.
Variations, modifications, and other implementations of what is described herein may occur to those of ordinary skill in the art without departing from the spirit and scope of the invention. Accordingly, the invention is not to be defined only by the preceding illustrative description.
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Chemically cross-linked polymeric particles are formed using mechanical rather than chemical processes, facilitating production of small-diameter particles in a manner largely independent of the viscosity or density of the polymer. For example, an uncross-linked resin may be provided in particulate form, agglomerated, and compressed into a mass of a desired shape with a desired diameter, and subsequently cross-linked.
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CROSS REFERENCE TO RELATED CASE
This application is a division of application Ser. No. 165,784 filed July 3, 1980, now U.S. Pat. No. 4,356,651 issued Oct. 26, 1982, which is in turn a continuation-in-part of application Ser. No. 82,162 filed Oct. 5, 1979, now U.S. Pat. No. 4,351,275. Ser. No. 354,099 (Solids Quench Boiler and Process) and Ser. No. 375,730 (Solids Quench Boiler and Process) are related to the subject application.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates generally to quenching furnace effluent. More particularly, the invention relates to a process and apparatus for quenching effluent cracked in a furnace using inert solid particles to provide the reaction heat. The invention is particularly adapted for embodiment in an apparatus and process for use in the Thermal Regenerative Cracking (TRC) process, as described in U.S. Pat. No. 4,061,562 to McKinney et al and U.S. Pat. No. 4,097,363 to McKinney et al.
2. Description of the Prior Art
In the technology of thermally cracking hydrocarbon feedstocks to produce olefins, it has long been necessary to stop the reaction of the cracked effluent by rapidly cooling the effluent. Various techniques and apparatus have been provided to facilitate quenching. Both direct quench, wherein a fluid material is introduced directly into the effluent stream, and indirect quench, wherein, heat exchange is performed by heat transfer through the walls separating the hot and cold side of the exchanger are commonly employed. An illustration of the indirect heat exchanger is shown in U.S. Pat. No. 3,583,476 (Herman N. Woebcke et al).
Process and equipment have been recently developed to crack hydrocarbons in tubular reactors employing solid-gas contact. The solids are essentially inert particulate materials which are heated to high temperatures and intimately mixed with the hydrocarbon feedstock to provide the heat necessary to crack the hydrocarbon.
The existing solid-gas contact processes employing inert particulate solids to provide the heat necessary for reaction typically separate the particulate solids from the gas before quench occurs. An illustration is seen in patent application Ser. No. 055,148 filed July 6, 1979 (Gartside et al), now U.S. Pat. No. 4,288,235 issued Sept. 8, 1981.
However, in the noncatalytic temperature dependent endothermic reaction processes, systems have been developed to quench the entire products stream after the requisite reaction period. The problem is that with heavy feedstocks at high severities, short residence times are desirable. The combination of heavy feedstock, high severity and short residence times impose severe operating problems on the heat recovery devices.
In connection with a current TRC installation, a 90% separation occurs in the primary separator. This is followed by an oil quench to 1300° F., and a cyclone to remove the remainder of the solids. The mix is then quenched again with liquid to 600° F. Thus, all the available heat from the reaction outlet temperature to 600° F. is rejected to a circulating oil stream. Steam is generated from this oil at 600 psig, 500 F. The subject invention is used to avoid exchanger fouling when cracking heavy feeds at low steam dilutions and high severities in the TRC. However, instead of an oil quench, a circulating solids stream could be used to quench the effluent. As in the reaction itself, the coke would be deposited preferentially on the solids thus avoiding fouling. These solids can be held at 800° F. or above, thus permitting the generation of high pressure steam (1500 psig+) which increases the overall thermal efficiency of the process. The oil loop can not operate at these temperatures due to instabilities (too many light fractions are boiled off, yielding on oil that is too viscous).
SUMMARY OF THE INVENTION
It is an object of the present invention to provide a solid quench system and apparatus capable of quenching the composite cracked effluent and particulate solids discharged from the reactor fed with heavy feed stocks and operated at high severity and short residence times.
It is another object of the present invention to generate 1,500 psig steam under any operating conditions imposed by the reactor.
It is a further object to provide a solids quench system uniquely suited for rapid quench of furnace effluent generated by noncatalytic temperature dependent endothermic systems utilizing particulate solids to provide the heat for cracking.
Thus, a process and apparatus have been provided to quench the stream of effluent and particulate solids discharged from a tubular reactor heated by the particulate solids in a TRC installation. The process and apparatus operate to introduce particulate solids into the effluent stream and also pass the effluent-particulate solids mixture in indirect heat exchange relationship with steam. In one embodiment a fluid bed quench riser is used to introduce the additional particulate solids into the stream and a quench exchanger close coupled to the quench riser is provided to effect the indirect heat exchange. The quench exchanger has a plurality of concentrically arrayed tubes extending longitudinally to the exchanger axis over which the stream of effluent and particulate solids pass in indirect heat exchange relationship.
In the process of quenching, the effluent from the reactor with entrained particulate solids enters the fluidized bed quench riser and by an eductor effect draws particulate solids, at a temperature much lower than the effluent temperature, into the quench boiler. The effluent and particulate solids pass in heat exchange relationship with steam in the tubes on the cold side of the quench exchanger and are cooled to the desired quench gas outlet temperature. Concomitantly, high pressure steam is generated in the cold side of the quench exchanger.
Apparatus for separating the particulate solids from the quench gas is provided downstream of the quench exchanger. A return leg for the separated solids to be delivered to the fluidized bed quench riser and outlet for the cracked gas are also included in the system.
In an alternative embodiment the quench riser is not used. The quench boiler is provided with the same plurality of concentrically arrayed longitudinal tubes, however the particulate solids are introduced directly into the reactor outlet tube at the entry end of the quench boiler.
DESCRIPTION OF THE DRAWINGS
The invention will be better understood when viewed with the following drawings wherein:
FIG. 1 is a schematic diagram of a TRC system and process according to the prior art.
FIG. 2 is a sectional elevational view of the solids quench boiler using the quench riser;
FIG. 3 is a detailed cross sectional elevational view of the quench exchanger of the system;
FIG. 4 is a cross sectional plan view taken through line 4--4 of FIG. 3; and
FIG. 5 is a detailed drawing of the reactor outlet and fluid bed quench riser particle entry area.
FIG. 6 is an elevational view of an embodiment in which particulate solids are delivered directly to the reactor outlet tube at the entry end of the quench boiler.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The solids quench boiler process and apparatus of the present invention are suitable for use in any application wherein a very rapid rate of quenching is required and the generation of high pressure steam is desirable without accumulation of tar or coke on the boiler tube surface, and thus the subject invention is particularly well adapted for use in the Thermal Regenerative Cracking (TRC) process.
Referring to FIG. 1, in the prior art TRC process and system, thermal cracker feed oil or residual oil, with or without blended distillate heavy gas, entering through line 10 and hydrogen entering through line 12 pass through hydrodesulfurized zone 14. Hydrosulfurization effluent passes through line 16 and enters flash chamber 18 from which hydrogen and contaminating gases including hydrogen sulfide and ammonia are removed overhead through line 20, while flash liquid is removed through line 22. The flash liquid passes through preheater 24, is admixed with dilution steam entering through line 26 and then flows to the bottom of thermal cracking reactor 28 through line 30.
A stream of hot regenerated solids is charged through line 32 and admixed with steam or other fluidizing gas entering through line 34 prior to entering the bottom of riser 28. The oil, steam and hot solids pass in entrained flow upwardly through riser 28 and are discharged through a curved segment 36 at the top of the riser to induce centrifugal separation of solids from the effluent stream. A stream containing most of the solids passes through riser discharge segment 38 and can be mixed, if desired, with make-up solids entering through line 40 before or after entering solids separator-stripper 42. Another stream containing most of the cracked product is discharged axially through conduit 44 and can be cooled by means of a quench stream entering through line 46 in advance of solids separator-stripper 48.
Stripper steam is charged to solids separators 42 and 48 through lines 50 and 52, respectively. Product streams are removed from solids separators 42 and 48 through lines 54 and 56, respectively, and then combined in line 58 for passage to a secondary quench and product recovery train, not shown. Coke-laden solids are removed from solids separators 42 and 48 through lines 60 and 62, respectively, and combined in line 64 for passage to coke burner 66. If required, torch oil can be added to burner 66 through line 68 while stripping steam may be added through line 70 to strip combustion gases from the heated solids. Air is charged to the burner through line 69. Combustion gases are removed from the burner through line 72 for passage to heat and energy recovery systems, not shown, while regenerated hot solids which are relatively free of coke are removed from the burner through line 32 for recycle to riser 28. In order to produce a cracked product containing ethylene and molecular hydrogen, petroleum residual oil is passed through the catalytic hydrodesulfurization zone in the presence of hydrogen at a temperature between 650° F. and 900° F., with the hydrogen being chemically combined with the oil during the hydrocycling step. The hydrosulfurization residual oil passes through the thermal cracking zone together with the entrained inert hot solids functioning as the heat source and a diluent gas at a temperature between about 1300° F. and 2500° F. for a residual time between about 0.05 to 2 seconds to produce the cracked product and ethylene and hydrogen. For the production of ethylene by thermally cracking a hydrogen feed at least 90 volume percent of which comprises light gas oil fraction of a crude oil boiling between 400° F. and 650° F., the hydrocarbon feed, along with diluent gas and entrained inert hot gases are passed through the cracking zone at a temperature between 1300° and 2500° F. for a residence time of 0.05 to 2 seconds. The weight ratio of oil gas to fuel oil is at least 0.3, while the cracking severity corresponds to a methane yield of at least 12 weight percent based on said feed oil. Quench cooling of the product immediately upon leaving the cracked zone to a temperature below 1300° F. ensures that the ethylene yield is greater than the methane yield on a weight basis.
As seen in FIG. 2, in lieu of quench zone 44, 46 (see FIG. 1) of the prior art, the composite solids quench boiler 2E of the subject invention is comprised essentially of a quench exchanger 4E, a fluid bed-quench riser 6E, a cyclone separator 8E with a solids return line 10E to the fluid bed-riser 6E and a line 14E for the delivery of gas to the fluid bed-quench riser.
The quench exchanger 4E as best seen in FIGS. 3 and 4, is formed with a plurality of concentrically arranged circular tubular arrays extending parallel to the longitudinal axis of the quench exchanger 4E. The outer circle of tubes 16E form the outside wall of the quench exchanger 4E. The tubes 16E are joined together, preferably by welding, and form a pressure-tight membrane wall which is in effect, the outer wall of the quench exchanger 4E. The inner circles of tubes 18E and 20E are spaced apart and allow for the passage of effluent gas and particulate solids therearound. The arrays of tubes 16E, 18E and 20E are manifolded to an inlet torus 24E to which boiler feed water is delivered and an upper discharge torus 22E from which high pressure steam is discharged for system service. The quench exchanger 4E is provided with an inlet hood 26E and an outlet hood 28E, to insure a pressure tight vessel. The quench exchanger inlet hood 26E extends from the quench riser 6E to the lower torus 24E. The quench exchanger outlet hood 28E extends from the upper torus 22E and is connected to the downstream piping equipment by piping such as an elbow 30E which is arranged to deliver the cooled effluent and particulate solids to the cyclone separator 8E.
The fluid bed quench riser 6E is essentially a sealed vessel attached in sealed relationship to the quench exchanger 4E. The fluid bed-quench riser 6E is arranged to receive the reactor outlet tube 36E which is preferably centrally disposed at the bottom of the fluid quench riser 6E. A slightly enlarged centrally disposed tube 38E is aligned with the reactor outlet 36E and extends from the fluid bed-quench riser 6E into the quench exchanger 4E. In the quench exchanger 4E, the centrally disposed fluid bed-quench riser tube 38E terminates in a conical opening 40E. The conical opening 40E is provided to facilitate nonturbulent transition from the quench riser tube 38E to the enlarged opening of the quench exchanger 4E. It has been found that the angle of the cone θ, best seen in FIG. 3, should be not greater than 10 degrees.
The fluid bed 42E contained in the fluid bed quench riser 4E is maintained at a level well above the bottom of the quench riser tube 38E. A bleed line 50E is provided to bleed solids from the bed 42E. Although virtually any particulate solids can be used to provide the quench bed 42E, it has been found in practice that the same solids used in the reactor are preferably used in the fluidized bed 42E. Illustrations of the suitable particulate solids are FCC alumina solids.
As best seen in FIG. 5, the opening 48E through which the fluidized particles from the bed 42E are drawn into the quench riser tube 38E is defined by the interior of a cone 44E at the lower end of the quench riser tube 38E and a refractory cone 46E located on the outer surface of the reactor outlet tube 36E. In practice, it has been found that the refractory cone 46E can be formed of any refractory material. The opening 48E, defined by the conical end 44E of the quench riser tube 38E and the refractory cone 46E, is preferably 3-4 square feet for a unit of 50 MMBTU/HR capacity. The opening is sized to insure penetration of the cracked gas solid mass velocity of 100 to 800 pounds per second per square foot is required. The amount of solids from bed 42E delivered to the tube 38E is a function of the velocity of the gas and solids entering the tube 38E from the reactor outlet 36E and the size of the opening 48E.
In practice, it has been found that the Thermal Regenerative Cracking (TRC) reactor effluent will contain approximately 2 pounds of solids per pound of gas at a temperature of about 1,400° F. to 1,600° F.
The process of the solids quench boiler 2E of FIGS. 2-5 is illustrated by the following example. Effluent from a TRC outlet 36E at about 1,500° F. is delivered to the quench riser tube 38E at a velocity of approximately 40 to 100 feet per second. The ratio of particulate solids to cracked effluent entering or leaving the tube 36E is approximately two pounds of solid per pound of gas at a temperature of about 1,500° F. At 70 to 100 feet per second the particulate solids entrained into the effluent stream by the eductor effect is between twenty five and fifty pounds solid per pound of gas. In 5 milliseconds the addition of the particulate solids from the bed 42E which is at a temperature of 1,000° F. reduces the temperature of the composite effluent and solids to 1,030° F. The gas-solids mixture is passed from the quench riser tube 38E to the quench exchanger 4E wherein the temperature is reduced from 1,030° F. to 1,000° F. by indirect heat exchange with the boiler feed water in the tubes 16E, 18E, and 20E. With 120,000 pounds of effluent per hour, 50 MMBTUs per hour of steam at 1,500 PSIG and 600° F. will be generated for system service. The pressure drop of the gas solid mixture passing through quench exchanger 4E is 1.5 PSI. The cooled gas-solids mixture is delivered through line 30E to the cyclone separator 8E wherein the bulk of the solids is removed from the quenched-cracked gas and returned through line 10E to the quench riser 6E.
The embodiment of FIG. 6 depicts a solids quench boiler 62E in which the inlet tube 10E terminates in an opening 11E in the effluent reactor outlet tube 36E. The indirect quench exchanger 4E is shown without the fluid bed quench riser, however it is comprised of the outer circle of tubes 16E terminating on the ends in an inlet torus 24E and a discharge torus 22E. The outlet hood 28E and downstream equipment such as elbow 30E and cyclone separator 8E are also shown. A regulatable valve 9E is shown in the line 10E.
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Apparatus for quenching and cooling the reactor effluent in a thermal regenerative cracking (TRC) system. The quench apparatus includes a section for introducing relatively cool particulate solids into a hot effluent stream to effect initial quenching and a section to further cool the composite of quenched effluent and solids.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to an automatic device for economizing compressed air.
2. Related Art
French Pat. No. 82 05 042 and its certificate of addition No. 83 03 513 cover a compressed air economizing device permitting the driving fluid pressure of a user-apparatus such as a cylinder actuator to be adjusted to a pressure lower than the pressure in the distribution network.
That device comprises a means of ensuring passage of the fluid under pressure during most of the stroke of the cylinder's moving element and blocks passage of the pressurized fluid before or at the end of the stroke of said moving element.
The certificate of addition, No. 83 03 513, describes such an economizing device constructed in the form of a single-unit fitting readily mountable on a cylinder, a pipe or a directional valve, which can be built very simply and cost-effectively.
OBJECTS AND SUMMARY OF THE INVENTION
The present invention is directed to an improved economizing device of the same type incorporated in a single-unit fitting designed to equip only one chamber of a double-acting cylinder.
The invention accordingly provides a device consisting of a fitting having a first circuit connecting a fluid supply pipe to a cylinder chamber. The first circuit is controlled by a valve which moves with a piston slidably driven by an elastic means within the fitting. The piston is actuated by the presence or absence of a pressure signal. The fitting has a second circuit short-circuiting the first circuit and connecting a fluid exhaust pipe to the cylinder chamber. The second circuit is controlled by a check valve and the top of the fitting is provided with a means for adjusting the tension of the elastic means and pursuant, the speed of the cylinder's moving element.
This device permits stopping the supplying of fluid to the cylinder before, or at, the end of the piston stroke and also permits adjusting the speed of the piston to suit the work required.
Control of the check valve is obtained either by the drop in pressure of the exhaust fluid or by a pressure signal generated by an end-of-travel detector in the cylinder.
BRIEF DESCRIPTION OF THE DRAWINGS
Other features and advantages of the invention will be more readily understood in reading the following description of several embodiments with reference to the appended drawings in which:
FIG. 1 is a cutaway view, taken longitudinally, of a single-unit economizing device of the pressure drop type, connected to one end of a cylinder actuator;
FIG. 2 is a cutaway view of an economizing device identical to that of FIG. 1 and comprising only one valve operating in both directions;
FIG. 3 is a cutaway view of an alternative embodiment of the device in FIG. 1;
FIG. 4 is a cutaway view of an economizing device with axially aligned pipes;
FIG. 5 is a cutaway view of an alternative embodiment of the device in FIG. 4;
FIG. 6 is a cutaway view of an economizing device fitted to an apparatus and specifically to a directional valve;
FIG. 7 is a cutaway view of an economizing device sandwiched between two apparatuses;
FIG. 8 is a cutaway view of an economizing device wherein the piston contains a passage for the exhaust fluid;
FIG. 9 is a cutaway view of an economizing device containing a normally-closed valve actuated by pressure drop;
FIG. 10 is a cutaway view of a variant of FIG. 9;
FIG. 11 is a cutaway view of an economizing device with a normally-closed valve actuated by a pressure signal;
FIG. 12 is a cutaway view of an economizing device with a normally-closed valve actuated by a pressure signal;
FIG. 13 is a cutaway view of a variant of the device shown in FIG. 12;
FIG. 14 is a cutaway view of an economizing device with a normally-open valve actuated sideways by a pressure signal;
FIG. 15 is a cutaway view of a variant of the device shown in FIG. 14, with axially aligned ports; and
FIG. 16 is a cutaway view of a variant of the device shown in FIG. 8, actuated by a pressure signal.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
FIG. 1 shows a cylinder actuator 1 in which is slidably mounted a piston 2 consisting of a rod 3 driving any suitable unit not shown in the drawing. A compressed air economizing device 4 is fitted between one of the chambers 1a of the cylinder and a directional valve 5 operable to alternatively connect chamber 1a to a compressed air source or to the atmosphere. The other chamber 1b of the cylinder is connected directly via a pipe 6 to the directional valve 5, although it would be possible to also equip the pipe 6 with an economizing device identical to economizing device 4.
The economizing device 4 consists of a tubular body 7, having a threaded bottom portion 8 for screwing into the tapped port of a supporting means and a cylindrical portion on which is fitted a collar 9 with a pipe connection 10 for fluid flow to pipe 11 and chamber 1a of the cylinder, said connection 10 extending at a right angle to the axis of body 7.
The body 7 of the device incorporates a valve 12 connected to a piston 13 via a stem 14 and operable to close off the passage between duct 15 and the opening of connection 10 when pushed against a valve seat 16 provided in the body 7. A tubular space above seat 16 communicates via openings 17 provided therein with a flow channel 18 in pipe connection 10 leading to pipe 11.
Flow channel 18 is provided with slots 19 which are closed off on the outside of said channel by a flexible sleeve 20 which is attached at one end and free to open at the other end to allow fluid to pass from pipes 11 and 18 in the direction of a tubular section 21 issuing into duct 15 to bypass the seat 16 of valve 12. This sleeve 20 forms a check valve enabling the fluid to pass only in the direction from chamber 1a to directional valve 5.
The top of body 7 has a threaded section mating with a plug 22, said plug having a center cavity 24 housing a spring 23 which pushes against the larger cross-sectional side of piston 13 such that the compression of spring 23 is adjusted in relation to the piston and the valve 12 to adjust the flow rate of the fluid and the speed of piston 2. Cavity 24 extends toward the top of plug 22 and opens, via openings 25, into a pipe connection 26 being part of a collar 27 fitted externally onto the top part of plug 22 and extending at a right angle to the axis of body 7.
Pipe connection 26 connects via pressure tap pipe 28 to the fluid outlet 6 of cylinder 1 chamber 1b.
When the cylinder piston 2 moves in the direction of arrow F in FIG. 1, the fluid escaping through pipe 6 transfers its pressure through pipe 28 to chamber 29 located above piston 13 such that the large face 13a of piston 13 is subjected to the combined pressure of the spring 23 and the exhaust fluid from cylinder chamber 1b. The small face 13b of piston 13 is subjected to the pressure action of the intake or driving fluid. Consequently, valve 12 moves to open position, allowing the driving fluid to pass through pipes 18 and 11 and into chamber 1a.
However, as soon as piston 2 reaches the end of its stroke, the exhaust fluid pressure disappears and no longer acts on the large face 13a of piston 13. Consequently, valve 12 closes due to the force of the driving fluid on the small face 13b of piston 13, said force being greater than that of the spring 23.
Lacking pressure in chamber 17, on the other hand, valve 12 returns to open position, pushed by spring 23.
When the cylinder piston 2 travels opposite the direction of arrow F and chamber 1a is in exhaust position, fluid flows out through pipe 11 to pipe 18 and pushes the small face 13b of piston 13 while the large face 13a of the piston is subjected to the action of the driving fluid and the spring which keep the valve 12 open.
Moreover, the fluid can escape into the annular space 21 and duct 15 toward the directional valve 5, by passing through the check valve 20, thus boosting the exhaust flow.
The speed of piston 2 can be varied by acting upon plug 22, screwing the plug in or out to change the tension on spring 23 and the fluid passage between seat 16 and valve 12.
FIG. 2 shows an economizing device identical to that of FIG. 1, except that in this embodiment, a valve is used which by itself ensures passage of the fluid on intake and exhaust.
To this end, valve 30 has a stem 31 adapted to slide in a blind hole 32 formed in the bottom of piston 13, said valve 30 being subjected to the action of a spring 33 acting in the direction of closure of valve 30.
Pipe connection 10 has only 1 channel 18 and the check valve 20 shown in FIG. 1 has been eliminated. When cylinder chamber 1a is supplied with driving fluid such that the exhaust fluid flows out of cylinder chamber 1b, the piston 13 is held in down by spring 23 in combination with the pressure of the exhaust fluid leaving pipe 28, so that valve 30 stays open and allows passage of the driving fluid into pipe 11.
As soon as the exhaust fluid pressure lets off on the large face 13a of piston 13, piston 13 moves up in response to the pressure acting on its small face 13b, thus allowing valve 30 to close against the seat 16 due to the pressure of spring 33.
Nevertheless, when the exhaust fluid flows the opposite way, through pipe 11 towards duct 15, valve 30 being independent of piston 13, this results in spring 33 being compressed by the fluid pressure and enabling valve 30 to open and the fluid to escape into duct 15.
Adjustment of the speed of piston 2 is done in the same way as above by acting on plug 22 and compressing spring 23 to a greater or lesser extent to allow a larger or smaller passage between the valve 30 and its seat 16.
FIG. 3 shows an economizing device analogous to that of FIG. 1, except that the plug 22 is fixed and cannot serve as a means of adjusting the tension of spring 23 as in FIG. 1 to control the fluid flow opening and the travel speed of piston 2 in the cylinder.
In the embodiment depicted in FIG. 4, the device comprises a main body 7 having a threaded part 34 at its base engaged into a tapped hole in a secondary body consisting of 2 pipe connections--fluid inlet 35 and outlet 36--which are axially aligned with one another at a right angle to the axis of the main body 7.
This provides a direct passage for the fluid due to the fact that the device can be fitted to a line 11, 11a connected on one side to the cylinder and on the other side to the directional valve.
The control means for valve 30 is identical to that which was the object of the embodiment of FIG. 2.
The economizing device illustrated in FIG. 5 is the same as the one of FIG. 3, except that, like the previous one, it includes a secondary body consisting of two pipe connections 35, 36 axially aligned with one another. The control means for valve 12 and the check valve 20 are the same as those featured in FIG. 3, which lack means for adjusting the tension of spring 23.
FIG. 6 shows an economizing device comprising a body 37 with a flat surface 38 through which it is attached to a corresponding surface of an apparatus, in particular a directional valve 30 having ports 40, 40a and 40b aligned with the intake and exhaust ports of the economizing device.
Valve 30 is controlled by a piston 13 in the same way as described above for the device in FIG. 2.
FIG. 7 shows a device identical to that of FIG. 6, except that it is sandwiched between two apparatuses 41 and 42. To this effect the body 37 of the device is given two flat surfaces 37a, 37b which apply to corresponding surfaces on the two apparatuses.
Ports 43a, b and c of the apparatuses are in direct communication with the ports of the economizing device body 37.
FIG. 8 shows an economizing device wherein the body 7 contains a piston 44 having a blind hole 32 in which is slidably mounted the stem 31 of valve 30.
The top of body 7 is closed off by a plug 45 against which presses one end of a spring 46 whose other end presses against a piston 44. A tapped hole is provided in plug 45 for receiving a screw 47 having an end pin 48 bearing on members 49 attached to piston 44.
This feature enables compression adjustment of spring 46 by adjusting the screw 47 and piston 44 in order to adjust the air output and, following, the speed of cylinder piston 2.
Above pipe connection 10, body 7 is fitted with a collar 27 and pipe connection 26 connected via pipe 28 to the exhaust of cylinder chamber 1b. Pipe connection 26 has a slanted duct 50 issuing into an annular space 51 communicating via an aperture 52 in body 7 and a center bore 53 in piston 44 with an chamber 54 located above piston 44.
The part of chamber 54 which is located under the piston is vented to the atmosphere via a duct 55 in body 7, an annular space 56 separated from annular space 51 by an O-ring 57, an an aperture 58 arranged in collar 27.
This device operates in the same way as the one described with reference to FIG. 2, except that the fluid from the exhausting chamber comes in above the piston after flowing through said piston's center bore 53.
FIG. 9 shows a device having a piston 59 connected to a valve 60 by means of a stem 61, said valve being held in its seat, in closed position, by a spring 62 housed in a compartment 63 provided in a plug 64 engaged in body 7 and having a threaded portion 65, said latter portion mating with a tapped hole in a collar 66 mounted rotatively but captively, due to a rib 67 engaged in a groove in body 7.
This feature makes it possible to axially move plug 64 by turning collar 66, so as to adjust the compression of spring 62 for purposes of adjusting fluid flow and the speed of the cylinder piston.
Collar 9 is provided with a ball check valve 68 making it possible to vent the space above valve 60.
When chamber 1a of the cylinder (FIG. 1) is supplied with fluid, valve 60 is in open position, piston 59 being pushed up against spring 62 by the pressure of the fluid exhausting from chamber 1b of the cylinder, which enters chamber 69 through pipe connection 26.
As soon as the pressure of the exhaust fluid disappears, as the piston 2 of the cylinder 1 reaches the end of its stroke, piston 59 returns to its initial position by the action of spring 62 and valve 60 closes.
Check valve 20 enables bypassing of valve 60 to allow fluid to pass in reverse when cylinder chamber 1a is in the exhausting phase.
The device illustrated in FIG. 10 is analogous to that of FIG. 9 except for the body 70 which comes in a single unit and has two pipe connections 71, 72 which are axially aligned with one another for insertion into a pipeline.
Moreover, connection with the fluid exhaust line is made via a pipe 73 issuing into chamber 69 of body 70.
FIG. 11 shows another embodiment of an economizing device whose valve is controlled to close by a pressure signal sent by an end-of-stroke detector on piston 2 of cylinder 1 or by any other suitable means providing a pressure signal.
This device includes a plug 22 with a threaded part 74 screwed into body 7, on which body is mounted at a right angle, by means of a collar 9, a pipe connection 10 containing a check valve 20. Plug 22 contains a cavity 75 in which is slidably mounted a piston 76 spring loaded by spring 77 and fitted with a closing member 78 on one of its ends forming the valve which closes against a seat 79 provided in the body between ducts 15 and 18.
The top of plug 22 is provided with a bore hole 80 connected to a pressure signal means,in particular to signal the end of the stroke of the cylinder piston.
When driving fluid is applied to the base of valve 78 said valve is pushed against the force of spring 77 and opens to allow the fluid to flow out through duct 18 and cylinder chamber 1a. If at a given time a pressure signal is sent via borehole 80 into cavity 75, the pressurized fluid, together with spring 77, act on piston 76, closing valve 78, which applies against the seat 79, thus cutting off the flow of driving fluid.
FIG. 12 shows an economizing device having a valve controlled by a pressure signal. A piston 81 and valve 82 unit is fitted in the body 7 such that the valve is kept open by a spring 83.
The top of body 7 is provided with a plug 84 having a threaded part 85 by which it engages in a tapped hole in an adjusting ring 86 having a circular rib 87 mating with a groove in body 7, said ring thus being rotatably maintained on body 7. This feature enables adjustment of valve 82 in relation to its seat when it is opened and, following, adjustment of the rate of fluid flow and of the speed of cylinder piston 2.
The top part of plug 84 has a center bore 88 enabling transmission of a pressure signal to piston 81 to close valve 82 against the action of spring 83 at a predetermined time, particularly when the cylinder is at the end of its stroke.
FIG. 13 shows a device like that of FIG. 12, except that it lacks a spring 83, due to the face that the chamber 89 is vented to the atmosphere via a duct 90.
FIG. 14 shows a device similar to that of FIG. 12 wherein the pressure signal however enters laterally.
To this effect, the device is provided with another pipe connection 91 above pipe connection 10, said connection 91 comprising a collar 92 fitted to body 7 and provided with seals 92a and 92b for the purpose of isolating an annular space between the body 7 and the collar 92, said annular space connecting pipe 93 via an aperture 94 to a chamber 95 located above piston 81.
The pressurized fluid corresponding to a signal can thus propagate from pipe 93 to chamber 95 wherein it acts upon the piston 81 and against the action of spring 83 and closes normally-open valve 82.
The device shown in FIG. 15 is the same as that of FIG. 14, except for the arrangement of body 96 which has two pipe connections 96a and 96b axially aligned with one another, said pipe connections ensuring the flow of fluid in one direction by valve 82 or in the other direction by means of check valve 20.
The device shown in FIG. 16 is the same as that of FIG. 8, except that it is used in the case of a piston operated by a pressure signal.
To this effect, collar 27 is flipped over so that the slanted duct 50 issues into annular space 56 and, via aperture 55, into chamber 54a under piston 44. Also, as space 51 is vented to the atmosphere via the aperture 58 in collar 27, it is possible to vent space 54 via center bore 53, which issues into annular space 51.
When a pressure signal is fed through pipe 28, duct 50, space 52 and aperture 55 to chamber 54a, piston 44 moves up against spring 46 such that valve 30 is pushed up by spring 33 to close off the passage between ducts 15 and 18.
The invention is not limited to the embodiments shown and a person ordinarily skilled in the art may make some modifications to it without departing from the scope of the invention.
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Automatic device for economizing compressed air comprises a means for ensuring the passage of driving fluid under pressure during most of the stroke of the moving element of a user apparatus. The device consists of a single-unit body having a first circuit connecting a fluid supply pipe to one chamber of the cylinder actuator. The first circuit is controlled by a valve moving with a piston subjected to the action of an elastic means and slidably mounted in the body. The piston is actuated by the presence or absence of a pressure signal, the body having a second circuit by-passing the first circuit and connecting a fluid exhaust pipe to the cylinder chamber.
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BACKGROUND OF THE INVENTION
The present invention relates to such a ground excavating apparatus as is suitable for excavating the heterogeneous ground consisting of hard and soft stratums including a rock bed and gravel.
The excavating apparatuses so far designed and manufactured for the purpose of conducting building of a tunnel or excavation of the ground are multifarious and diversiform, and are roughly classified into those of the bucket type proving suitable for excavating the soft ground and those of the impact crusher type proving suitable for excavating the comparatively hard ground.
The bucket type is such a type that generally conducts excavation of the soft ground by the operation of a bucket fitted in place on the top section of a bucket boom, hence unsuitable at all for the excavation of the hard ground. Meanwhile, the impact crusher type, on the part thereof, is what is applied to building of a tunnel in an extensive manner, and this category of ground excavating apparatus is what is employed for conducting excavation by cutting and crushing the face is a continuous manner without employing gunpowder, unlike the case of a blasting process.
The tunnel excavators presently employed are roughly classified into those of the total section cutting system and those of the partial section cutting system. The tunnel excavators of the partial section cutting system are those hitherto employed for excavating a coal mine and specifically remodeled for the purpose of conducting excavation for building a tunnel. The tunnel excavator of the total section cutting system are generally those employed for conducting excavation to a circular section. Multifarious models of tunnel excavators of the impact crusher type have been developed thus far, and have such common characteristics that generally cause the cutter thereof to be revolved, and to be given proper impellant force as well, for the purpose of conducting proper cutting or crushing of a rock.
However, for all the fact that the said bucket type and the said impact crusher type prove to be effective and efficient enough, in case the ground is well stabilized with a soft stratum and a hard rock bed, respectively, excavation by the employment of only either one of the said types is still impracticable or inefficient in the case of a general excavation work, since therein exist a variety of stratums in a mixed form as a reality.
SUMMARY OF THE INVENTION
In the case of the present invention, disclosed is such a ground excavator having the said two types properly combined therefor, wherein excavation of the soft ground is conducted by the employment of a bucket, while excavation of the hard ground, such as a rock bed or the like, is conducted by the employment of an impact crusher, thus proving well applicable for the excavation of the heterogeneous ground consisting of a soft stratum and a hard stratum.
To put it otherwise, one purpose of the present invention rests with providing such a ground excavating apparatus as is well applicable for excavating the heterogeneous ground consisting of both hard and soft stratums, another purpose of the present invention rests with providing such a ground excavating apparatus of a new system, wherein the bucket-applied excavation type and the impact crusher-applied excavation type are properly combined into a single set of ground excavating apparatus, and still other purpose of the present invention rests with providing such a ground excavating apparatus as is well capable of selecting at liberty any angle of excavation from within the range specified for the impact crusher for excavating a hard stratum, and is superb in workability as well.
Other purposes, features and advantages of the ground excavating apparatus introduced in the present invention will be made apparent enough readily through the following detailed description of certain perferred embodiments thereof given in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side view of one illustration of the present invention,
FIG. 2 is a front view of the illustration shown in FIG. 1,
FIG. 3 and FIG. 4 are explanatory drawings of the actuation thereof,
FIG. 5 is a front view of other illustration of the present invention,
FIG. 6 is a side view of still other illustration of the present invention,
FIG. 7 is a front view of the illustration shown in FIG. 6, and
FIG. 8 and FIG. 9 are explanatory drawings of the actuation thereof.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the drawings, 1 is a fixed member, and formed on the said fixed member 1 is a ring-shaped seat 2 for conducting proper fitting. The said ring-shaped seat 2 for conducting proper fitting has a swivel seat 4 properly set in place thereon through a pivoted bearing 3. The said swivel seat 4 has a bracket 5 properly fixed in place thereon. The said bracket 5 has a projecting section 6a of a housing 6 constituting a supporting member A properly fitted in place by means of a pin 7. The said swivel seat 4 has a bracket 8 properly fixed in place thereon, and the said bracket 8 has the base end section of a jack 9 for actuating a boom to face upward or downward properly fitted in place thereon. The said housing 6 has a bracket 11 properly set in place on the front upper section thereof, and the said bracket 11 has a rod 9a of the said jack 9 for actuating the boom to face upward or downward by the employment of a pin 12. The said housing 6 has an impact-crushing mechanism B fitted in place on the upper section thereof. The said impact-crushing mechanism B is provided with such a guide boom 23 as is properly fitted in place on the housing 6 in a manner of being capable of sliding in the forward and rearward directions, the said guide boom 23 has an impact-generating mechanism 24 properly fixed in place on the front end section thereof, and the said impact-generating mechanism 24 has a chisel 25 properly fitted in place on the movable side thereof.
The said guide boom 23 has an operating mechanism D, for instance, a sliding jack 26, properly set in place therein, and the base end section of the said sliding jack 26 is properly fitted in place on a jack support 36 by means of a pin 38. A rod 26a of the said sliding jack 26 is properly fitted in place on a bracket 24a fixed in place on the rear end section of the said impact-generating mechanism 24 by means of a pin 39. And, the said housing 6 has a bucket boom 13 properly set in place on the lower section thereof in a manner of being capable of traveling in the forward and rearward directions, the said bucket boom 13 has such a bracket 14a as is fixed in place on the back surface of a bucket 14 properly fitted in place on the front end section thereof, by means of a pin 15, the bucket boom 13 has a supporting bracket 13a properly fixed in place on the top end section thereof, the said supporting bracket 13a has such an inclination operation mechanism F as a bucket jack 16 properly fitted in place thereon by means of a pin 17, and a rod 16a of the said bucket jack 16 is properly fitted in place by means of a pin 18 on the said bracket 14a fixed in place on the back of the said bucket 14. The said bucket boom 13 has such an operating mechanism E as a sliding jack 20 properly set in place therein, the base end side of the said sliding jack 20 is properly fitted in place on a jack support 37 by means of a pin 40, and a rod 20a of the said sliding jack 20 is properly fitted in place on the said bucket boom 13 by means of a pin 41.
The said pivoted seat 4 is so designed as to be revolved by a revolution driving mechanism (not shown in the drawings).
Now, in the case of conducting excavation of a soft and weak stratum, the sliding jacks 20, 20 are actuated, the bucket boom 13 is thus caused to advance forward, the bucket 14 is caused to draw near to a proposed stratum, the bucket jack 16 is actuated in such a manner as to be subjected to rocking the bucket 14, and excavation of the stratum is conducted by means of such an excavating fluke 14b as is properly fitted in place on the said bucket 14.
Meanwhile, in the case of excavating a stratum consisting of a hard rock bed, the sliding jack 26 is extended for proper actuation, and the impact-generating mechanism 24 is caused to advance forward through the means of the said guide boom 23, thus causing the said chisel 25 to advance forward in a proper manner.
In this state, the said impact-generating mechanism 24 is put to proper actuation, and then impact-crushing of a proposed stratum is conducted by means of the said chisel.
The chips of the soft stratum thus excavated and/or the chips of the hard stratum thus crushed are raked together by means of the bucket 14. To put it otherwise, the said jack 9 for actuating the boom to face upward or downward is put in actuation in the state of having the bucket boom 13 properly extended, thus causing the bucket 14 to be transferred as far as to the position of the said excavated and/or crushed chips, the bucket jack 16 is actuated, the sliding jack 20 is extended and the bucket boom 13 is contracted in a concurrent manner, and the said jack 9 for actuating the boom to face upward or downward is also concurrently actuated, whereby raking the said excavated and/or crushed chips together by the employment of the said bucket 14 is thus properly conducted.
Next, shown in FIG. 5 is other illustration of the present invention, wherein a plurality of impact crushing mechanisms are properly fitted. To put it in concrete terms, this illustration is such that three sets of the impact crushing mechanism are fitted in place, unlike the case of the above-mentioned illustration, and this category of ground excavating apparatus proves more effective and efficient in the case of conducting crushing of a rock bed. The impact crushing mechanism on the right and the left is fitted in place on the said housing 6 in a proper manner by means of brackets 42, 43, respectively.
Shown in FIG. 6 through FIG. 9 is still other illustration of the present invention. In the drawings, 1 is a fixed member, and this fixed member has a ring-shaped seat 2 for fitting properly formed thereon. The said fitting seat 2 has a pivoted seat 4 properly set in place thereon through a pivoted bearing 3. The said swivel seat 4 has a bracket 5 properly fixed in place thereon. The said bracket 5 has a projection 6a of the housing 6 properly fitted in place thereon by means of a pin 7. The said swivel seat 4 has a bracket 8 properly fixed in place thereon, and this bracket 8 has the base end section of a jack 9 for actuating the boom to face upward or downward properly fitted in place thereon by means of a pin 10. The said housing 6 has a bracket 11 properly fitted in place on the front upper section thereof, and the said bracket 11 has a rod 9a of the jack 9 properly fitted thereon by means of a pin 12. The said housing 6 has jack supports 36, 37 properly fixed in place on the rear end section thereof, to thus constitute a supporting member A. The said supporting member A has the said guide boom 23 properly fitted in place on the upper section thereof in such a manner as to be capable of sliding, the said guide boom 23 has a bracket 50 for fitting properly fitted in place on the front end section thereof in a manner of being capable of inclining by the employment of a pin 50a, the said guide boom 23 further has a supporting bracket 51 properly fixed in place on the right and the left on the front end section thereof, and the said supporting bracket 51 has an inclination jack 52 properly fitted in place thereon in a manner of being capable of rocking. A rod 53 of the said inclination jack 52 is properly fitted in place on the upper section of the said bracket 50 for fitting by means of a pin 54. The said guide boom 23 has a notched hole 55 properly formed in the front upper section thereof. And, the said bracket 50 for fitting has an impact crushing mechanism B properly fitted in place thereon. This impact crushing mechanism B is provided with such an impact-generating mechanism 24 as is fixed in place on the said bracket 50 for fitting, and the said impact-generating mechanism 24 has a chisel 25 properly fitted in place on the movable side thereof.
The said guide boom 23 has a sliding jack 26 properly set in place therein, and the said sliding jack 26 has the jack support 36 properly fitted in place by means of a pin 38. A rod 26a of the said sliding jack 26 is properly fitted in place on the said guide boom 23 by means of a pin 39.
Furthermore, the said housing 6 has a bucket boom 13 properly set in place on the lower section thereof in a manner of being capable of sliding, the bucket boom 13 has such bracket as is set on the backside of a bucket 14 properly fitted in place on the front end section thereof by means of a pin 15, the said bucket boom 13 has a supporting bracket 13a properly fixed in place on the front end section thereof, the said supporting bracket 13a has a bucket jack 16 properly fitted in place thereon by means of a pin 17, and a rod 16a of the said bucket jack 16 is properly fitted in place on the said bracket 14a set on the back of the bucket 14, by means of a pin 18. The said bucket boom 13 has a sliding jack 20 properly set in place therein, the base end side of the said sliding jack 20 is properly fitted in place on a jack support 37 by means of a pin 40, and a rod 20a of the said sliding jack 20 is properly fitted in place on the said bucket boom 13 by means of a pin 41. The said swivel seat 4 is so designed as to be properly swiveled by means of a swivel driving mechanism (not shown in the drawings).
Now, in the case of conducting excavation of a soft and weak stratum, the sliding jacks 20, 20 are actuated, the bucket boom 13 is caused to advance forward, the bucket 14 is caused to draw near to a proposed stratum, the bucket jack 16 is actuated to thus subject the bucket 14 to the motion in the upward and downward directions, and excavation of the stratum is conducted in a proper manner by means of the excavating flukes 50 of the bucket 14.
Meanwhile, in the case of conducting excavation of a hard stratum consisting of a rock bed, the sliding jack 26 is extended for proper actuation, the impact-generating mechanism 24 is caused to advance forward by means of the said guide boom 23, and the chisel 25 is thus properly caused to advance forward.
It is in this state that the said impact-generating mechanism 24 is to be put to proper operation, thus conducting impact-crushing of the proposed stratum.
And, in case a portion of the stratum to be thus subjected to excavation is located underneath, the inclination jack 52 is actuated, the impact crushing mechanism B is inclined by a proper angle by means of the said bracket 50 for fitting, the angle for excavation is selected in a proper manner, and excavation of the proposed stratum can thus be conducted in an effective and efficient manner. (Reference is invited to FIG. 8 and FIG. 9.)
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Such a ground excavating apparatus that conducts excavation of a soft stratum by means of a bucket and employs an impact crusher for the excavation of such a hard stratum as a rock bed or the like is disclosed.
Introduced in the present application is a ground excavator of such a category that comprises a housing, a bucket boom properly set in place in the said housing in a manner of being capable of traveling forward and rearward, a bucket properly fitted in place on the front end section of the said bucket boom in a manner of being capable of inclining, and an impact crushing mechanism well capable of traveling forward and rearward by virtue of a hydraulic jack housed in the said bucket boom, and employs the said bucket and the said impact crushing mechanism in an alternate manner to best suit the nature of the ground to be excavated.
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This disclosure is based upon, and claims priority from French Patent Application No. 98/03484, filed Mar. 20, 1998, and International Application No. PCT/FR99/00602, filed Mar. 17, 1999, the contents of which are incorporated herein by reference.
BACKGROUND OF THE INVENTION
The invention relates to a telecommunication terminal provided with an integrated circuit card known as a smart card comprising one or more application programs.
The invention applies particularly to cellular telephone terminals of the mobile terminal type such as mobile telephones complying with the GSM or DCS standards.
It should be stated that the smart cards used in telephone terminals make it possible to identify the subscriber and contain a telephone application program. These cards are generally known as SIM (Subscriber Identity Module) cards.
New generations of telephone terminals are being provided, functioning with two smart cards, one smart card dedicated to telephony and another smart card dedicated to other applications, for example the electronic purse application.
For this purpose these terminals must be equipped with two interfaces for reading smart cards, one for communicating with the subscriber identification smart card and the other with the smart card dedicated to the other applications.
However, new developments are aimed at reducing the size of mobile telephones. One way of achieving this consists in using only one smart card, which is then of the multi-application type. Thus the mobile telephone no longer needs to have two reading interfaces.
Provision is therefore made, according to these new developments, for the same smart card to contain several application programs, one being for telephony and the other being able to be a banking application such as an electronic purse, another being able to be a loyalty application (loyalty points), a health application or a game application.
The telecommunication terminals are designed to be connected to a telecommunication network used by telephone subscribers to access other subscribers or services.
Amongst these networks are telephone networks, switched networks or integrated service networks and the cellular telephone network.
Up to the present time access to the smart card in a terminal or the smart cards in the said terminal was possible only through the terminal, from the said telecommunication network.
Provision is made, with the new developments, for this access to be open to any processing unit of the computer or microcomputer type (personal computer PC or network computer NC), referred to hereinafter as a microcomputer.
To this end the telecommunication terminal must be equipped with means of physical connection with the microcomputer. This is a case of a connector and a cable link. Some terminals are already equipped with an input/output port making it possible to connect them to a microcomputer for transferring data through the radio network.
It is therefore envisaged, according to these developments, to use the existing physical access means. However, the problem of access to the card by means other than the mobile telephone network is for all that unresolved.
SUMMARY OF THE INVENTION
The applicant has resolved this problem by providing in the terminal logical access means to the card from a microcomputer and means of managing the accesses from the telecommunication network and/or microcomputer.
The logical access means comprise means of interpreting commands sent from the microcomputer and/or sent from the network, executing these commands if it is a case of commands which can be executed by the terminal and transmitting to the card if it is a case of commands which can be executed by the card.
According to one characteristic of the invention, the management means are able:
according to a first embodiment:
to keep the two logical access means (by microcomputer and network) active, to then change to blocking mode to momentarily block one of the means of access to the card from the microcomputer or from the network, leaving the other access open, and to put on stand-by the commands arriving through the blocked access means;
according to a second operating mode:
to temporarily deactivate one of the access means, the terminal then functioning exclusively in smart card read mode (access through the microcomputer) or exclusively in telecommunication terminal mode (access through the network).
In fact, opening up access to the card through the terminal, other than through the telephone channel, also poses the problem of the management of the accesses in order to prevent any conflict and/or loss and/or unintentional modification of information on the card. This problem has therefore been resolved by the applicant.
Preferably the access management means keep the two access means active and put on standby the commands arriving through the network access means when the microcomputer requests access for an application different from the one which is able to be used by the network.
Preferably the access management means temporarily deactivate the network access means when the microcomputer requests access for the same application able to be used by the network.
The means of managing access to the card include means of blocking access to the card through the network and unblocking means, activated by the terminal after reception of a blocking command sent by the microcomputer to enable it to process two simultaneous accesses to the card, one access being requested by the network for one application and the other being requested by the microcomputer for a distinct application.
The means of managing access to the card also include reversible means of changing to exclusive card read mode, deactivating the telecommunication terminal operating mode, these means being activated by the terminal after reception of a read mode command.
This makes it possible to deal with the case where access is requested by the microcomputer for an application dedicated to access by the network. The terminal then functions as a smart card reader.
Advantageously the blocking means have a timeont, during which the terminal is able to receive one or more commands from the telephone network and to store this command or commands until unblocking.
Advantageously, the duration of the timeont corresponds to the maximum period required by the card for executing an application command.
BRIEF DESCRIPTION OF THE DRAWING
Reference can be made to the description below, which is given as an indication and in no way limitatively, with regard to the accompanying drawings, in which:
FIG. 1 illustrates schematically the functioning of the terminal in the case of two simultaneous accesses to two distinct applications,
FIG. 2 illustrates schematically the functioning of the terminal in the case of the smart card reader mode,
FIG. 3 illustrates the communication protocol according to the operating mode illustrated by FIG. 1
FIG. 4 illustrates the communication protocol according to the operating mode illustrated by FIG. 2 .
DETAILED DESCRIPTION
Currently, a SIM card, for example, inserted into a mobile terminal, receives commands in accordance with the standard for the mobile telephone network, for example the GSM standard.
The commands for the cards are strictly controlled by the mobile terminal. This means of access will be referred to as the GSM channel (it is a case of a logical rather than a physical channel).
Accessing the SIM card in a mobile terminal from a PC requires another means of access: this means will be referred to as the reading channel (it is case of a logical channel connected to the PC).
Simultaneous access to the SIM card by two different channels poses the problem of the sharing of a resource. For this purpose commands for blocking and unblocking access to the card are provided.
For the GSM channel to remain having priority, a timeout mechanism (or countdown) unblocks access for it.
Simultaneous access by two different applications in the same card through each of the channels is resolved by the multi-application operating system loaded in the terminal.
There are cases, and this will be detailed below, where it is advantageous to access, by means of the reading channel, the same application used by the GSM channel. As the card cannot resolve this problem, provision is made in accordance with the invention to change operating mode, the mobile terminal passing to smart card reader mode.
The terminal preferably gives priority to the GSM channel. The SIM commands of the network communication protocol (GSM) are executed within a reasonable time by the card. To do this, when the card is acted on through the reading channel, it cannot be acted on beyond a period predetermined by a timeout, possibly configurable. In practice this period corresponds to the period of execution of an application command (APDU: Application Protocol Data Unit) by the card.
In practice each application command (APDU format) sent to the card by the reading channel is framed by a Blocking Mode command and by a Unblocking Mode command.
In addition, in the cases of a multiple access, the type of command sent by the reading channel must be different from the type of command sent via the GSM channel, since the card has no means of distinguishing the origin of the commands, that is to say the commands via the reading channel or commands via the GSM channel. A sequence of commands of the same type creates a context in the card. Commands of the same type arriving by another channel could therefore modify this context unpredictably, causing a malfunction of the card, resolved solely by a reset of the card (power off/power on at the terminal).
Thus, in order to be able to execute commands arriving by the reading channel of the same type as those transmitted by the GSM channel, provision is made for changing the terminal to exclusive reading mode, as will be detailed below.
A description will now be given of the functioning of the terminal using the diagram in FIG. 1, which corresponds to the case of multiple accesses: access I by the PC and access II by the network in order to reach two different applications, appli.1 and appli.2 respectively.
The application installed on the PC sends the Blocking Mode command, to have access to the card of the mobile terminal.
When this command is successful, the PC application sends an application command (APDU format) to the card, via the mobile, recovers the result thereof in the PC and sends the Unblocking Mode command, relating to access to the card, to the terminal.
A description will now be given of the functioning of the terminal using the diagram in FIG. 2 in the case where the PC wishes to access appli.1 (telephony) normally used by the network.
The application installed on the PC sends the Reader Mode command, in order to have exclusive access to the card of the mobile terminal and consequently deactivate the telecommunication terminal function.
When this command is successful, the PC application sends one or more application commands (APDU format) to the card, via the mobile, retrieves the result in the PC on each occasion, and then, when it has finished, the PC application sends the End of Reader Mode command to the terminal, thus reopening access by the network.
A description will now be given of the communication protocol between PC, terminal and network according to FIG. 1; this protocol is illustrated in FIG. 3 .
When the application on the PC wishes to have the mobile terminal execute an APDU command (which may contain several TPDU commands), it requests of it access to the card by means of the Blocking Mode command. The terminal checks whether access is available. In this case, it places a lock limiting access only to the reading channel (that is to say it opens access to the microcomputer) and triggers a timeout at the end of which the lock will be removed automatically. The PC then sends the TPDU commands making up the APDU command, which the terminal makes the card execute. The terminal sends the responses from the card. At the end, the PC requests the terminal to release access by means of the Unblocking Mode command, and the terminal complies and ends the timeout.
If during this time the terminal has received, via the GSM channel, commands (SIM) to be executed by the card, it stores them.
When access II is once again available, the terminal blocks access only to the GSM channel, and causes the waiting commands to be executed by the card. At the end, it releases access II.
In normal mode, when the terminal receives a command via the GSM channel, it blocks access only to the GSM channel, makes the card execute the corresponding command, and then releases the access.
The maximum period of the timeout implemented by the terminal is directly related to the storage capacity for the commands received via the GSM channel. This timeout imposes a maximum period of execution of an APDU transmitted via the reading channel by the card.
The protocol corresponding to exclusive Reading Mode is described below and illustrated by FIG. 4 .
The advantage of this mode is to enable the user to have access to the card in order particularly to send commands (to customize the card) without risk of interfering with usage by the GSM network. It is no longer necessary to remove the card from the mobile terminal to insert it in to a conventional reader: the mobile terminal becomes a reader.
The PC requests the change to exclusive reader mode by means of the Reader Mode command. The terminal deactivates all the communications with the GSM network.
The PC then uses the terminal as a normal card reader, sending TPDU commands to it. The terminal transmits the responses of the card to these commands. At the end of the operation, the PC requests the reactivation of the communications with the GSM network by means of an End of Reader Mode command.
To keep consistency with multiple access mode, each APDU command sent to the terminal could be framed by Blocking Mode and Unblocking Mode commands. These commands in the exclusive reader mode should have no effect in the terminal: the timeout would not be triggered in the terminal since the commands succeed all the time.
When the terminal is restarted, following a failure during one communication or another, a default operating mode is provided; this will preferentially be the telecommunication terminal operating mode (access from the network).
The terminal can be used for example in the case of multi-application SIM cards for, for example:
control of access to distant computers, payment (electronic purse, credit, etc), etc,
point of sale terminals on GSM, ATM on GSM, etc.
customization by the subscriber of his multi-application SIM card.
Other ways of managing can be imagined such as, for example, priority GSM access, shared-time access, etc.
In the case of shared time access, provision can be made for prior storage in buffer memory respectively for each channel and authorisation of accesses, by alternate reading of each of the buffers.
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The invention concerns a telecommunication terminal ( 2 ) comprising means to be accessed by a telecommunication network and means to be accessed by a micro-computer type processing unit ( 1 ), said terminal comprising a chip card ( 3 ) for implementing at least one application and logic means (I) for the card to be accessed by the network, said terminal further comprising logic means (I) to access the card ( 3 ) from the microcomputer ( 1 ) and means for managing ( 20 ) accesses coming from the telecommunication network and/or the microcomputer.
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BACKGROUND OF THE INVENTION
The invention relates to α-amides of L-amino acids that are precursors of fragrances and which are useful in the formulation of deodorants, antiperspirants, body sprays, and other skin treatment compositions.
In humans, axillary malodors are produced by enzymatic cleavage of malodor precursors found in apocrine secretions. The enzymes that release the malodors are produced by axillary bacteria such as Staphylococcus sp. and Corynebacteria. Typical deodorants mask or decrease this malodor.
SUMMARY OF THE INVENTION
It has now been shown that various α-amides of L-amino acids can be cleaved by axillary bacterial enzymes, releasing pleasant fragrances and/or attenuating malodor. Such amino acid amides, therefore, are useful in skin treatment compositions such as deodorants, antiperspirants, and body sprays. Accordingly, the invention relates to α-amides of L-amino acids that are precursors of fragrances, or which can attenuate or mask malodor.
In one aspect, the invention features a skin treatment composition (e.g., a deodorant composition) for application to human skin; the skin treatment composition includes a dermatologically acceptable vehicle and an α-amide of an L-amino acid having the structure: ##STR1## wherein n is 1 or 2 and R 2 is selected so that cleavage of the α-amide of the L-amino acid leaves an R 2 -CO 2 H having a neutral or pleasant odor, or which is useful in attenuating or masking malodor. In general, these α-amides of L-amino acids are cleaved by bacterial enzymes by the reaction shown below. ##STR2##
The α-amide of the L-amino acid is present in an amount sufficient to produce fragrance or attenuate or mask malodor. Preferably, the α-amide of L-amino acid is present in the skin treatment composition at a concentration of 0.01 to 10.0% (preferably 0.1 to 5.0%) by weight. If desired, the skin treatment composition can include an antiperspirant active (e.g., aluminum chlorohydrate) or a deodorant active (e.g., an antimicrobial). In various preferred embodiments, the skin treatment composition is formulated as a lotion, cream, stick, gel, or aerosol.
The composition may be formulated as a skin moisturizer, shampoo, shave preparation, body spray, body wash, soap, and the like.
The invention offers several advantages. For example, when the α-amides of L-amino acids are formulated as skin treatment compositions, fragrance is released slowly over time. Consequently, the fragrance is long-lasting and fading of the scent over time is minimized. In many instances, the α-amide of L-amino acids competes with the malodor precursor and attenuates malodor production over a prolonged period.
Other features and advantages of the invention will be apparent from the following detailed description, and from the claims.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In preferred α-amides of L-amino acids, R 2 has 1 to 30 carbon atoms and is alkyl, alkenyl, alkynyl, cycloalkyl, cycloalkenyl, aryl or heterocyclic. These groups may be unsubstituted or substituted with one or more halo, hydroxyl, amino, nitro, amide, alkoxyl, carboxyl, cyano, thio, phosphoro, or other heteroatoms, phenyl, or heterocyclic groups. The amino, amide, alkoxyl, carboxyl, thio, phosphoro, or heterocyclic groups may be unsubstituted or substituted with one or more halo, hydroxyl, amino, nitro, alkyl, amide, alkoxyl, carboxyl, cyano, thio, or phosphoro groups.
R 2 can be, for example, methyl, ethyl, propyl, isopropyl, tert-butyl, sec-butyl, isobutyl, n-butyl, pentyl, hexyl, heptyl, octyl, 2-octyl, nonyl, 2-nonyl, decyl, 2-decyl, undecyl, 2-undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl, or octadecyl, or a mono or poly unsaturated form thereof, cyclopentyl, cyclohexyl, 2-cyclohexylethyl, 2,6-dimethylheptyl, geranyl, neryl, citronellyl, 9-decenyl, 2,6-dimethyl-5-heptenyl, 2,6-dimethyl-1,5-heptadienyl, 8,11-heptadecadienyl, 8-heptadecenyl, cyclopentenyl, cyclohexenyl, phenyl, p-methoxyphenyl, benzyl, 2-phenylethyl, 1-phenylethyl, 2-(p-methoxyophenyl)-ethenyl, 3-(p-methylphenyl)-2-propyl, 3-(p-isopropylphenyl)-2-propyl, 3-(p-tert-butylphenyl)-2-propyl,2,5,8-trioxanonyl, acetonyl, aminomethyl, hydroxymethyl, 1-hydroxyethyl, dimethylaminomethyl, 1-phenyl-1-aminoethyl, carboxymethyl, 2-carboxyethyl, 3-carboxypropyl, 4-carboxybutyl, 5-carboxypentyl, 6-carboxyhexyl, 7-carboxyheptyl, 8-carboxyoctyl, 9-carboxynonyl, 10-carboxy-2,5,8-trioxanonyl, 7-carboxamido-5-carboxy-4-aza-3-oxo-heptyl, 8-carboxamido-6-carboxy-5-aza-4-oxo-octyl, 9-carboxamido-7-carboxy-6-aza-5-oxo-nonyl, 10-carboxamido-8-carboxy-7-aza-6-oxo-decyl, 11-carboxamido-9-carboxy-8-aza-7-oxo-undecyl, 14-carboxamido-12-carboxy-11-aza-10-oxo-tetradecyl, 2-pentyl-cyclopropyl, menthyl, or terpineyl.
Preferred α-amides of L-amino acids for use in the invention include, without limitation, N-methylpentenylglutamine, N-methylpentenylasparagine, N-phenylacetylglutamine, N-phenylacetylasparagine, N-indolacetylglutamine, N-indolacetylasparagine, N-cyclohexylcarboxylglutamine, N-cyclohexylcarboxylasparagine, N-ethylbutyrylglutamine, N-ethylbutyrylasparagine, N-phenylpropionylglutamine, N-phenylpropionylasparagine, N-benzoylglutamine, N-benzoylasparagine, N-cyclohexylacetylglutamine, N-cyclohexylacetylasparagine, N-vanilloylglutamine, and N-vanilloylasparagine.
The preferred α-amides of L-amino acids generally can be prepared by coupling a carboxylic acid to a protected amino acid by known procedures. The carboxylic acids and protected amino acids generally are known in the art; they generally are either commercially available or can be made by known procedures.
Examples
Various α-amides of L-amino acids were synthesized and tested for cleavage by Staphylococcus haemolyticus, which is commonly found on human skin, especially in the axilla. In the following examples, amide analogs of the amino acid glutamine in which R 2 was phenylacetic acid (PAA) or methylpentenoic acid (MPA) were synthesized. Other known fragrant carboxylic acids (e.g., ethylbutyric acid, cyclohexylcarboxylic acid, or indole-3-acetic acid) can be substituted for PAA or MPA. The α-amides of the L-amino acids were synthesized as described below. The following working examples also provide general guidance for synthesis and testing of other α-amides of L-amino acids in accordance with the invention. These examples are meant to illustrate, not limit, the invention, the metes and bounds of which are defined by the claims.
Synthesis of α-Amides of L-Amino Acids
Coupling Carboxylic Acids to Protected Amino Acids
To couple the carboxylic acid to a protected amino acid. (e.g. L-glutamine t-butylester. HCl) the carboxylic acid (7.4 mmol), the protected amino acid (7.1 mmol), 4-dimethylaminopyridine (0.1 g), diisopropylethylamine (0.92 g, 7.1 mmol) and methylene chloride (40 mL) were stirred, under nitrogen in a 100 mL flask, until the amino acid was dissolved. The reaction was cooled in an ice-water bath and a solution of dicyclohexylcarbodiimide (DCC) (1.5 g, 7.3 mmol) dissolved in methylene chloride (20 mL) was added. Stirring was continued in the ice water bath for approximately 15 minutes, during which time a white precipitate of dicyclohexylurea (DCU) began to form. The reaction was then stirred overnight at room temperature under nitrogen. The following day, the DCU was suction-filtered off, and the filtrate was washed twice with 50 mL of 10% sodium bicarbonate, washed twice with 1M hydrochloric acid (50 ml) then washed once with 50 mL of saturated sodium chloride. The organic layer was dried over anhydrous magnesium sulfate for at least two hours, filtered, and rotary evaporated to dryness. The product can be analyzed with thin layer chromatography (TLC, using silica gel plates) in order to determine the optimal solvent for purification via flash chromatography (e.g., with the FLASH 40 system from Biotage). In general 30-40% ethyl acetate/hexane is suitable. Dissolution of the product prior to chromatography in the eluting solvent may leave additional DCU undissolved, which can be suction-filtered off.
Removal of the t-Butyl Ester Protecting Groups
The protected amino acid (approximately 10 mmol) was dissolved in trifluoroacetic acid (TFA; 25 mL), and the solution was stirred at room temperature for approximately 3 hours (until the reaction was completed, as determined by TLC using the solvents identified for chromatographic purification). The TFA was removed via rotary evaporation and vacuum-oven drying.
In an alternative method, the protected amino acid (10 mmol) was dissolved in ethyl acetate (25 mL), the solution was cooled in an ice-water bath, and hydrogen chloride gas was bubbled into the solution for approximately 15 minutes. The ice-water bath was removed, and the solution was stirred overnight. The solvent then was removed by rotary evaporation and vacuum-oven drying. The products from the reactions were analyzed by TLC on silica gel plates and by 1 H NMR with a Bruker AC-250 NMR Spectrometer.
Assay of the α-Amides Of L-Amino Acids for Cleavage by Bacteria
The synthesized α-amides of L-amino acids were tested for their ability to be cleaved by bacteria normally found in human axilla. For this example, a 100 mL culture of Staphylococcus haemolyticus was grown overnight at 37° C. in Trypticase Soy Broth medium. The cells were pelleted by centrifuging the culture at 5,000 rpm for 12 minutes, and the pelleted cells were resuspended in sterile saline. The cells were again pelleted and resuspended in sterile saline. After pelleting the cells once again, the cells were weighed and resuspended in sterile assay buffer (50 mM phosphate, pH 6.8, 1% glucose/dextran). The final concentration of cells was 0.05 g cells/mL (for the gas chromatography (GC) assay) or 0.1 g cells/mL (for the NMR assay). These cell suspensions can be stored at 4° C.
The α-amides of L-amino acids were prepared as stock solutions at a concentration of approximately 5 mg/mL in 50 mM potassium phosphate buffer (pH 6.8). If necessary, the pH can be adjusted to 6.8-7.0 with 1N NaOH. The amino acid stock solutions were sterilized by filtering them through 0.22 μm filters.
Gas Chromatography Assay
To demonstrate that the α-amides of L-amino acids can be cleaved by bacteria normally found in axilla, a 100 μL aliquot of the α-amides of L-amino acids stock was added to 100 μL of cells in sterile tubes. For a negative control, the cells were incubated with 100 μL sterile phosphate buffer. The samples were incubated for 16-18 hours at 37° C., and the reactions were quenched with 10 μL of 10 N HCl. The samples then were extracted with 100 μL chloroform and analyzed by gas chromatography.
NMR Assay
In addition to analyzing the cleavage reactions by gas chromatography, NMR analysis was used. A 500 μL aliquot of the α-amide of the L-amino acid stock solution was added to 500 μL of cells in sterile tubes. The cells and α-amides of L-amino acids were incubated for 16-18 hours at 37° C., with shaking, and the cleavage reactions were quenched with 50 μL of 10 N HCl. Each sample then was extracted with 600 μL of CDC 3 , and the extracts were filtered through a Na 2 SO 4 pipette filter to remove water from the samples. 1 H NMR spectra of the samples then were taken (64-128 scans generally is sufficient), zooming in on a region that would contain peaks from the cleavage product. The presence or absence of these peaks allowed for a qualitative determination of whether the α-amides of L-amino acids was cleaved. Each of the α-amides of L-amino acids (Phenylacetylglutamine and Methylpentenylglutamine) was cleaved by the Staphylococcus haemolyticus cells, as determined by gas chromatography or 1 H NMR. Thus, these α-amides of L-amino acids can be used as fragrance precursors in skin treatment compositions, for example.
Formulation of Skin Treatment Compositions
A variety of skin treatment (e.g., deodorant or antiperspirant) compositions are known in the art, and the α-amides of L-amino acids of the invention can be used in the formulation of such skin treatment compositions. A variety of skin treatment compositions can be made that include an effective amount of the α-amides of L-amino acids in a dermatologically acceptable vehicle. Such vehicles for use in deodorant or antiperspirant compositions and other ingredients that can be used in deodorant or antiperspirant compositions are known in the art. A preferred form is one containing a deodorant active (e.g. an antimicrobial). Another preferred form is one containing an antiperspirant active. The α-amides of L-amino acids of the invention are used in an amount sufficient to produce fragrance or attenuate or mask malodor when the skin treatment composition is applied topically to skin. Suitable formulations also are well known in the art. Generally, the α-amides of L-amino acids are used at a concentration of 0.01 to 10% by weight. A single α-amide of an L-amino acid can be used in a skin treatment composition, or multiple α-amides of L-amino acids can be used in combination.
Examples of suitable deodorant actives include, without limitation, triclosan, triclocarban, zinc phenolsulfonate, other zinc salts, lichen extract, and usnic acid. Examples of suitable antiperspirant actives include, without limitation, salts of aluminum chlorohydrate; aluminum sesquichlorohydrate, aluminum dichlorohydrate, aluminum chlorohydrex PG or PEG, aluminum sesquichlorohydrex PG or PEG, aluminum dichlorohydrex PG or PEG, aluminum zirconium trichlorohydrate, aluminum zirconium tetrachlorohydrate, aluminum zirconium tetrachlorohydrex PG or PEG, aluminum zirconium pentachlorohydrate, aluminum zirconium octachlorohydrate, aluminum zirconium trichlorohydrex-gly, aluminum zirconium tetrachlorohydrex-gly, aluminum zirconium pentachlorohydrex-gly, aluminum zirconium octachlorohydrex-gly, aluminum zirconium chloride, aluminum zirconium sulfate, potassium aluminum sulfate, sodium aluminum chlorohydroxylacetate, and aluminum bromohydrate. These deodorant or antiperspirant actives can be incorporated into the compositions in accordance with conventional methods for producing deodorants.
Methods for preparing various suitable skin treatment compositions are known in the art. Various deodorant, antiperspirant, and personal care compositions are within the invention; several examples are provided below.
______________________________________Ingredients % w/w______________________________________Deodorant StickPropylene glycol 70.300Water 20.500Sodium Stearate 7.000Triclosan 0.300Fragrance 1.400α-amide of L-amino acid 0.50Total 100.00Aerosol AntiperspirantCyclomethicone 10.0Dimethicone 2.0Cyclomethicone (and) Quaternium 18 2.0Hectorite (and) SDA 40SDA 40, Anydrous 0.5Aluminum Chlorohydrate 10.0α-amide of L-amino acid 1.0Propellant A-31 74.5Total 100.00Suspension Antiperspirant StickCyclomethicone 54.5Stearyl Alcohol 20.0PPG-14 Butyl Ether 2.0Hydrogenated Castor Oil 1.0Talc 2.0Aluminum Zirconium Tetrachlorohydrex- 20.0Glyα-amide of L-amino acid 0.5Total 100.00Anydrous Roll-On AntiperspirantCyclomethicone 69.0Dimethicone 5.0Cyclomethicone (and) Quaternium 18 3.0Hectorite (and) SDA 40SDA 40, Anhydrous 2.0Aluminum Zirconium Tetrachlorohydrex- 20.0Glyα-amide of L-amino acid 1.0Fragrance Oil q.s.Total 100.00Transparent Antiperspirant GelPhase ACyclomethicone (and) Dimethicone 10.0CopolyolCyclomethicone 7.0Phase BAluminum Chlorohydrate (and) Water 50.0Propylene Glycol 16.0Water 16.0α-amide of L-amino acid 1.0Total 100.00Nonionic O/W, Emollient CreamWater 73.000Stearic acid 7.200Glyceryl monostearate 4.500Lanolin 1.000Isopropyl myristate 4.300Polyethylene glycol 1000 monostearate 6.000α-amide of L-amino acid 1.00Preservative 0.300Perfume 0.200Total 100.00______________________________________
Other Embodiments
If desired, the α-amides of L-amino acids can be used in combination with other fragrance producing molecules or perfumes as indicators that the products are working, or to enhance the fragrance. In addition, the α-amides of L-amino acids can be used in personal care compositions to produce fragrance or attenuate or mask malodors.
It is to be understood that while the invention has been described in conjunction with the detailed description thereof, the foregoing description is intended to illustrate and not limit the scope of the invention, which is defined by the scope of the appended claims. Other aspects, advantages, and modifications are within the scope of the following claims.
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Disclosed are α-amides of L-amino acids that produce fragrance or attenuate or mask malodor. In particular, glutamine and asparagine amides can be used in the invention. Such α-amides of L-amino acids are useful for generating pleasant fragrances or attenuating or masking malodor upon cleavage of the α-amides of L-amino acids by bacteria in axillae. The α-amides of L-amino acids can be incorporated into skin treatment compositions and personal care products, such as deodorants, body sprays and antiperspirants, and used in methods for producing fragrance or attenuating or masking malodor.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
Embodiments of the present invention generally relate to introducing a gas into a micro cavity to enhance the lifetime of a micro-electromechanical system (MEMS) devices.
2. Description of the Related Art
A digital variable capacitor (DVC) utilizing MEMS technology operates by having a switching element of the MEMS device move between a state of high capacitance and a state of low capacitance. In a state of high capacitance, the switching element is in a position adjacent an RF electrode. In a state of low capacitance, the switching element is in a position adjacent to another electrode spaced from the RF electrode, or more specifically, away from an insulating layer that is disposed on the RF electrode. The switching element may also be moved to ground whereby the switching element is adjacent neither the RF electrode nor the other electrode.
During the lifetime of the MEMS device, the switching element cycles between the various states (i.e., high capacitance, low capacitance and ground). For a cycle, the switching element moves from the ground state to either the high or low capacitance state. After the cycle is completed, and before the next cycle, the switching element returns to the ground state. Then, a new cycle begins whereby the switching element moves to either a high or low capacitance state, or remains in the ground state. This corresponds to a physics movement of a plate which either touches the insulating layer overlying the RF electrode or touches the roof of the cavity in which it is housed.
There are only a finite number of times that the switching element can move before the MEMS device fails. With each movement of the switching element, the MEMS device accumulates a finite amount of damage which, given enough total cycles, results in failure. The magnitude of the finite damage to the MEMS device or the roof of the cavity or the insulating layer overlying the RF electrode is proportional to the impact speed of the fast moving switching element as the switching element is brought into contact therewith. In the above example the contact can cause material to be ejected from the exposed surfaces which then enter between the plates of the capacitor, reducing the closest distance that the ground MEMS plate can make to the insulating layer over the RF electrode. Thus, the maximum possible capacitance is reduced.
Therefore, there is a need in the art for increasing the lifetime of MEMS devices in DVCs by reducing the impact velocity of the switching element in a MEMS device as the switching element makes contact with various surfaces within the device cavity.
SUMMARY OF THE INVENTION
The present invention generally relates to methods for increasing the lifetime of MEMS devices by reducing the impact velocity of a switching element in the MEMS device. Rather than leaving the encapsulated MEMS device in a vacuum cavity, atoms are implanted into the cavity to introduce an inert gas into the cavity after the cavity has been sealed in the vacuum state. Introducing gas into the cavity causes gas damping and thin film damping which reduces the final impact speed.
In one embodiment, a method of MEMs fabrication comprises fabricating a MEMs device, the MEMs device having a cavity sealed by an encapsulating layer, implanting atoms into one of more of the encapsulating layer and another layer bordering the cavity and annealing the MEMs device to release the atoms into the cavity and pressurize the cavity.
In another embodiment, a MEMs device includes a first cavity having a switching element therein movable between a first position and a second position, a second cavity disposed adjacent the first cavity, a channel connecting the first cavity to the second cavity and atoms implanted into a portion of a boundary of the second cavity.
In another embodiment a MEMs device or set of MEMs devices are housed in a cavity under high vacuum. For example, the MEMs device may be a DVC consisting of a conducting beam that is electrically grounded and movable from a position close to a radio frequency (RF) electrode (i.e., a high capacitance state) that may be on the substrate and that is coated with a thin layer of insulator. The conductive beam is pulled into the high capacitance state by applying a voltage to the electrodes adjacent the RF electrode which is also coated with a thin insulator. The conductive beam can then be pulled to the roof of the cavity when a voltage is applied to an electrode (i.e., a pull-up electrode) above the conductive beam. An insulator under the pull-up electrode prevents the voltage on the pull-up electrode leading to current flow to the conductive beam (i.e., a low capacitance state). The low capacitance state moves the grounded conductive beam away from the RF electrode leading to the low capacitance state for the RF electrode. Typically voltages of between 10V and 30V are applied to move the conductive beam between the low and high capacitance states. These high voltages cause the conductive beam to accelerate across the cavity and land on the insulating material with velocities that can be greater than 1 m/s. These devices have to switch many hundreds of millions of times and if the impact velocity is too great, eventually material wears off the surfaces leading device failure. By introducing a gas into the cavity, the air under the conductive beam needs to move out the way as the beam makes contact with the insulating material. The gas has to flow laterally through an ever decreasing gap leading to an increased pressure in the narrow gap between the conductive beam and the surface it is approaching. This pressure causes a declaration force which slows down the conductive beam as the conductive beam lands reducing the impact damage.
Ion implantation of non reactive gases such as argon, nitrogen, or helium is available in semiconductor processing fab and is used to inject dopant into semiconductor substrates. A high voltage is used to accelerate ions to a very high velocity, these can be combined with a beam of electrons to then neutralize their charge before they enter the substrate. The high velocity ensures that most of the atoms come to rest some distance below the surface of the semiconductor. In this embodiment the ion acceleration would be adjusted to deposit most of the ions at a depth comparable to the thickness of the top layers of the cavity. There will be a distribution of depths where the atoms will come to a halt, and this will mean a large percentage of those atoms injected will come to rest either just above the cavity or just below. This may be an issue if there is a switching element in the cavity as the ions will then come to rest in the switching element itself, which may cause damage or a change in stress in the top surface leading to curvature of the switching element. To get around this issue a second cavity will be provided next to the MEMs cavity and joined by a pipe-like channel. An extra layer of masking material can be placed over the cavity containing the MEMs device and then be removed from over the empty cavity. The atom implanting process then implants atoms into the removable layer above the MEMs cavity (i.e., the masking material), but into the cavity and regions closely spaced just above and below the empty cavity. Subsequent annealing will then cause the gas to come out of the empty cavity walls and enter the empty cavity where pressure equalization will lead to gas diffusing into the cavity containing the switching element. The final stage of the process is to remove the masking material which has protected the MEMs cavity.
BRIEF DESCRIPTION OF THE DRAWINGS
So that the manner in which the above recited features of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to embodiments, some of which are illustrated in the appended drawings. It is to be noted, however, that the appended drawings illustrate only typical embodiments of this invention and are therefore not to be considered limiting of its scope, for the invention may admit to other equally effective embodiments.
FIG. 1A shows a MEMS device in a cavity connected to a neighboring empty cavity.
FIG. 1B shows the MEMS device and cavities of FIG. 1A after addition of the masking layer.
FIG. 1C shows the MEMS device and cavities of FIGS. 1A and 1B after the implantation process.
FIG. 1D shows the MEMS device and cavity of FIG. 1C after annealing and removal of the masking layer.
FIG. 2A shows the typical atom concentration versus depth in a solid substrate after high energy implantation.
FIG. 2B shows the typical atom concentration versus depth in the cast of a cavity.
FIG. 2C show the subsequent distribution of atoms shown in FIG. 2B after annealing.
To facilitate understanding, identical reference numerals have been used, where possible, to designate identical elements that are common to the figures. It is contemplated that elements disclosed in one embodiment may be beneficially utilized on other embodiments without specific recitation.
DETAILED DESCRIPTION
The present invention generally relates to methods for increasing the lifetime of MEMS devices by reducing the impact velocity of a switching element in the MEMS device. Rather than leaving the encapsulated MEMS device in a vacuum cavity, atoms are implanted into the cavity to introduce an inert gas into the cavity after the cavity has been sealed in the vacuum state. Introducing gas into the cavity causes gas damping and thin film damping which reduces the final impact speed.
FIG. 1A shows a MEMS device 100 in the ground state according to one embodiment. The MEMS device 100 includes a substrate 102 having a plurality of electrodes 104 A- 104 E formed therein. Two electrodes 104 B, 104 D are referred to as ‘pull-in’ electrodes because the electrodes 104 B, 104 D are used to pull the switching element 108 towards electrode 104 C. Electrode 104 C is an RF electrode. Electrodes 104 A, 104 E provide the ground connection to the switching element 108 through vias filled with electrically conductive material 110 . An electrically insulating layer 106 is formed over the electrodes 104 B- 104 D. In one embodiment, insulating layer 106 may comprise silicon dioxide, silicon nitride, or combinations thereof.
The switching element 108 may comprise an electrically conductive material such as titanium nitride or an alloy of aluminum titanium nitride. In one embodiment, the titanium nitride may be coated with a thin layer of electrically insulating material. The switching element 108 is shown to have a bottom layer 112 and a top layer 114 that are connected by one or more posts 116 . It is to be understood that the switching element 108 is contemplated to have other arrangements as well. Additionally, it is to be understood that both the top and bottom layer 112 , 114 of the switching element 108 are contemplated to comprise titanium nitride having a thin layer of electrically insulating material thereon, but other materials are contemplated as well. The switching element 108 is disposed within a cavity 118 and movable within the cavity 118 between the low capacitance, high capacitance and ground states.
Above the switching element 108 , another electrode 120 , sometimes referred to as a ‘pull-up’ or ‘pull-off’ electrode, is present. A thin layer 122 of electrically insulating material is disposed between the electrode 120 and the cavity 118 such that the layer 122 bounds the cavity 118 . The cavity 118 is sealed with a capping layer 124 that encapsulates the cavity 118 .
Next to the cavity 118 containing the switching element 108 is a separate cavity 130 . Cavity 130 is connected to cavity 118 containing the switching element 108 by the pipe or channel 131 . Cavity 130 can be used to introduce atoms into the cavity 118 , which would reduce the impact velocity of the switching element 108 in the cavity 118 . The atoms may be injected into the cavity 130 by an ion implantation process.
The MEMS device 100 may be formed as follows according to one embodiment. The substrate 102 is patterned by forming a mask thereover and etching the substrate 102 to form the trenches into which the electrically conductive material forming the electrodes 104 A- 104 E will be formed. Thereafter, the mask is removed and the electrically conductive material is deposited into the trenches to form the electrodes 104 A- 104 E. The electrically insulating layer 106 is then deposited thereover. Another mask is then formed over the electrically insulating layer 106 so that vias may be formed that will be filled with electrically conductive material 110 . The vias are etched into the insulating layer to expose the electrodes 104 A, 104 E, and then the mask is removed. The electrically conductive material 110 is then deposited in the vias.
A sacrificial material is then deposited over the electrically insulating layer 106 . The switching element 108 is then formed in the sacrificial material and additional sacrificial material is formed over the switching element 108 . The sacrificial material forms the boundary of the cavities 118 , 130 that are to be formed. An electrically insulating layer 122 is then formed over the topmost sacrificial layer followed by the electrode 120 . A hole is formed through the capping layer 124 , electrode 120 and insulating layer 122 to expose the sacrificial material. Etchant is introduced to the cavity 118 to remove the sacrificial material and thus form cavity 118 and cavity 130 . Within cavity 118 , the switching element 108 is free to move in response to electrical current applied to the electrode 120 or the pull-in electrodes 104 B, 104 D. An additional encapsulating layer may be deposited thereover to seal the cavities 118 , 130 . After the sealing, atoms may be implanted into cavity 130 through an ion implantation process.
In order to implant the atoms into the cavity 130 , a mask 140 is formed over the capping layer 124 . FIG. 1B shows the MEMS device 100 having cavity 118 and cavity 130 adjacent thereto. A mask 140 is formed over the capping layer 124 . The mask 140 has an opening 142 therethrough to expose the capping layer 124 over the cavity 130 . The masking material may comprise optical resist, polyimide or any other masking material that can absorb the accelerated atoms. The masking material is patterned using optical lithography and etching so as to be removed over the neighboring empty cavity 130 and thus form the mask 140 .
Once the mask 140 has been formed, atoms may be implanted through the mask 140 into the cavity 130 . FIG. 1C shows the MEMS device 100 in which atoms have been implanted into cavity 130 . The implanted atoms may include argon, helium, nitrogen, combinations thereof or any other material that forms a gas at ambient temperatures. In one embodiment, the implanted atoms comprise a gas that will not react with the materials in the cavity 118 . The implanted atoms are marked in regions 150 and 151 .
Following the implantation of the atoms, the MEMS device 100 can be annealed to diffuse the atoms into cavity 130 , channel 131 and cavity 118 . The annealing may occur at a temperature up to about 450 degrees Celsius. The mask 140 is also removed. The annealing may occur either before or after removal of the mask 140 . FIG. 1D shows the MEMS device 100 after annealing and after removal of the mask 140 . Due to the annealing, the gas molecules will have diffused into the cavity 118 . While not shown, it is contemplated that some sacrificial material may remain within the cavity 130 and have the atoms implanted therein during the implantation process.
FIG. 2A shows the typical atom concentration versus depth in a solid substrate after high energy implantation. The vertical axis shows the distance down into the substrate for a solid. The x horizontal axis shows the density of implanted atoms.
FIG. 2B shows the typical atom concentration versus depth in the cast of a cavity. The depth of the top of the cavity is marked as 1 and the depth of the bottom of the cavity is marked as 2 . Because the cavity provides hardly any opportunity for the injected atoms to lose energy, the atoms that make it through to the cavity traverse the cavity and are imbedded at the bottom of the cavity. Thus the distribution is broadened by almost the thickness of the cavity. Some atoms may be reflected by the bottom of the cavity and provide some pressure.
FIG. 2C show the subsequent distribution of atoms shown in FIG. 2B after annealing. The concentration gradient of implanted atoms leads to the diffusion of the atoms close to the cavity surface into the cavity providing a pressure of atoms that can reduce the impact velocity of the switching MEMs device.
In one embodiment, during the fabrication of the MEMs device 100 , some of the sacrificial material may remain in cavity 130 , so that the implanted atoms come to a halt in the cavity region. If this sacrificial material is porous or the atoms have a fast diffusion time, then they will be released into the joined cavities more quickly and more efficiently. The cavity 130 may also have material deposited in the cavity 130 during the fabrication stage that is not removed from the cavity during release, but will stop the implanted atoms easily, and allow them to diffuse out quickly on heating.
The invention has been described with respect to one capacitor in a cavity being part of many capacitors in a digital variable capacitor, but it is understood that the invention is applicable to cavities having multiple MEMS devices where the switching of the device causes impacts which limit the life of the device.
While the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
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The present invention generally relates to methods for increasing the lifetime of MEMS devices by reducing the landing velocity on switching by introducing gas into the cavity surrounding the switching element of the MEMS device. The gas is introduced using ion implantation into a cavity close to the cavity housing the switching element and connected to that cavity by a channel through which the gas can flow from one cavity to the other. The implantation energy is chosen to implant many of the atoms close to the inside roof and floor of the cavity so that on annealing those atoms diffuse into the cavity. The gas provides gas damping which reduces the kinetic energy of the switching MEMS device which then should have a longer lifetime.
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BACKGROUND OF THE INVENTION
Field of the Invention
[0001] The invention concerns a cleansing composition, in particular a make-up removing cosmetic composition of improved efficacy and rinse speed. In particular, it relates to a composition that removes makeup efficiently with excellent skin feel attributes.
Background of the Art
[0002] An important segment of the cosmetics market are makeup removal products (“MURs”) which are utilized for removing make-up by consumers. Removal of pigments of eye shadow, mascara, blush, lipstick and face powder is a daily problem for many women. The problem has been addressed through formulations which may include materials operating by solvent action or by emulsification. However, such cleansers often have disadvantages that they are slow rinsing and/or have negative skin feel attributes and may tend to phase separate over time i.e. they are not stable. Specifically high oil containing MURs have high make up removability but their slow rinsing speed and residual feeling are not preferred by many consumers. It is known that high oil make up removers must include high levels of low HLB nonionic surfactants to stabilize the high level of oil ingredients (typically 45%-80 wt. %) in the formulation for efficient make up removability. However it is also well known that high levels of low HLB nonionic surfactants leads to slow rinsing speed and often has a deleterious residual feeling on the skin.
[0003] U.S. Patent Publication No. 2005/0180942 published on Aug. 18, 2005 to Shimizu et al. describes a cleansing composition containing nonionic surfactants selected from various glycerol fatty acid esters in an oil base and having specific IOB values. The formulation is reported to resist phase separation.
[0004] U.S. Patent Publication No. 2004/0136943 published on Jul. 15, 2004 to Tomokuni describes a cleansing composition comprising (A) an oil component, (B) a hydrophilic nonionic surfactant, (C) a lipophilic amphiphile, (D) a water soluble solvent and (E) water. The composition reportedly has an isotropic liquid phase exhibiting a bicontinuous structure. The composition is described as exhibiting excellent detergency for the removal of both oil stains and water soluble stains and has high rinsability.
[0005] Various silicone oils have been used in the past to improve the sticky skin feeling from these products. Surprisingly the present inventive oil make up remover contains low levels of a high HLB nonionic surfactant and selected specific alkyl mono ester(s) and was seen to improve the rinsing speed and residual skin sensory feeling preferably without using silicone oils. Moreover it still was observed to stabilize high levels of hydrocarbon oil with excellent product transparency and stability.
[0006] Preferably the inventive product is used with a countertop mechanical pump that may be situated in a stable position so that the hand or forearm can be used to depress the pump and dispense the product. This arrangement results in a convenient and hygienic cleansing process.
BRIEF DESCRIPTION OF THE INVENTION
[0007] In one aspect of the invention is a cleansing composition including but not limited to:
a. about 10 to 25 wt. % of nonionic surfactant(s) collectively having a weight average HLB greater than 10.8. b. about 20 to 40 wt. % of linear and/or branched C5 to C 20 alkyl mono ester(s) where the molecular weight of the ester(s) is/are less than 320. c. about 25 to 40 wt. % of hydrocarbon oil(s); d. about 8 to 30 wt. % polyol(s); and e. about 1 to 10 wt. % of water.
Definitions
[0013] “Weight average HLB” is calculated referring to “The Atlas HLB Surfactant Selector”,
[0014] Griffin, W. C. (1949) J. Soc. Cosmet. Chem. 1:311-26
[0000] HLB average=Σ(Nonionic surfactant HLB×concentration)/total Nonionic surfactant concentration.
[0015] More specifically, as explained in Griffin, when two or more surfactants (emulsifiers) are combined (for our invention this relates specifically to combination of nonionic surfactants), the weight average HLB is the sum of the HLB value of each nonionic surfactant weighted by the concentration of each relative to overall concentration of nonionic surfactant. Thus, for example, if we were to blend three parts of a nonionic surfactant having HLB of 8 with one part of a nonionic surfactant having an HLB of 16, the weighted HLB average would be (¾) (8)+(¼) (16)=6+4=10.
[0016] Transparent means a turbidity of 0.05 optical density (OD) or less at 25 C measured at 500 nm using a 1 cm glass cell and a U-2810 spectrophotometer (Hitachi) or equivalent measured against distilled or deionized water as reference.
[0017] Stable means no phase separation after storage during 90 days at 45 C (in the dark).
[0018] Rinsing speed means either slow, moderate or fast rinsing of the product off the skin with water as judged by an expert panel using the test procedure described below.
BRIEF DESCRIPTION OF THE DRAWINGS
[0019] FIG. 1 is a photograph showing the comparative phase stability of inventive vs. comparative compositions.
[0020] FIG. 2 is a schematic diagram of a KES-SE friction tester manufactured by Kato Tech Co., Ltd. (Kyoto, Japan) that is useful to determine the MIU frictional value of selected compounds. MIU is defined as the average value of μ or frictional coefficient measured in a distance of 20 mm with the KES-SE friction tester using the procedure provided below.
[0021] FIG. 3 is graphical diagram demonstrating how the MIU frictional value is calculated using the KES-SE friction tester depicted in FIG. 2 .
DETAILED DESCRIPTION OF THE INVENTION
[0022] All publications and patent applications, patents, and other references mentioned herein are incorporated by reference in their entirety.
[0023] In one aspect of the invention is a cleansing composition including but not limited to:
a. about 10 to 25 wt. % of nonionic surfactant(s) collectively having a weight average HLB greater than 10.8, preferably greater than 11.0; preferably the concentration of nonionic surfactant(s) are in a maximum of about 23 wt. %, and a minimum of about 13 wt. %; b. about 20 to 40 wt. % of linear and/or branched C5 to C20 alkyl mono ester(s) where the molecular weight of the ester(s) is/are less than 320, preferably present at a minimum of about 23 and a maximum of about 33 wt. %; preferably where the maximum alkyl number is 18; c. about 25 to 40 wt. % of hydrocarbon oil(s) (preferably the hydrocarbon oil(s) comprise at least 50 wt. % Mineral oil based on the total oil content); preferably the hydrocarbon oil(s) have a maximum concentration of about 35 wt. %, and a minimum concentration of about 27 wt. %); d. about 8 to 30 wt. % polyol(s) (preferably a maximum concentration of about 20 wt. % and a minimum concentration of about 10 wt. %). e. about 1 to 10 wt. % of water (preferably a maximum concentration of about 8 wt. % and a minimum concentration of about 4 wt. %);
[0029] Advantageously the alkyl mono ester(s) have an average frictional coefficient upon application to the skin of less than 0.3 MIU as measured by the standard friction coefficient method described herein. Preferably the inventive composition further includes less than 1.0 wt. % of a silicone oil(s); preferably less than 0.5 wt. % and more preferably less than 0.1 or 0.01 or 0.001 wt. % of silicone oil(s).
[0030] Preferably at least 50 wt. % the total alkyl mono ester(s) is/are selected from Isodecyl Neopentanoate, Ethylhexyl Isononanoate, Isopropyl Myristate or blends thereof. More preferably at least 50 wt. % of the total polyol(s) are selected from propylene glycol, 1,3-Butylene Glycol, Dipropylene glycol or blends thereof.
[0031] Advantageously the inventive composition is transparent, preferably determined immediately after its preparation. Preferably the composition is stable. More preferably the composition has a viscosity in the range of 1 to 200 cps, preferably 10 to 150 cps at 25 C using the standard viscosity method. Most preferably the composition is a make-up remover composition.
[0032] Advantageously the invention is a packaged product for removing makeup from the skin comprising the above composition contained within a pump dispenser.
Nonionic Surfactants:
[0033] The inventive cleansing composition contains one or more nonionic surfactant(s) collectively having a weight average HLB greater than 10.8 (preferably greater than 11.0).
[0034] A variety of nonionic surfactants may be employed in the present invention as long as they collectively and preferably have the above weight average HLB value. Nonionic surfactants do not include linear and/or branched C5 to C 20 alkyl mono ester(s) with a molecular weight not exceeding 320. Particularly preferred nonionic surfactants are those with a C 10 -C 20 fatty alcohol or acid hydrophobe condensed with from about 2 to about 100 moles of ethylene oxide or propylene oxide per mole of hydrophobe; C 2 -C 10 alkyl phenols condensed with from 2 to 20 moles of alkylene oxide; mono- and di-fatty acid esters of ethylene glycol; fatty acid monoglyceride; sorbitan, mono- and di-C 8 -C 20 fatty acids; and polyoxyethylene sorbitan as well as combinations thereof. Alkyl polyglycosides are also suitable nonionic surfactants.
[0035] Useful materials also include POE-20 sorbitan monolaurate; POE-20 cetyl ether; POE-7 glyceryl cocoate; POE-15 stearyl ether; POE-10 stearyl ether; POE-15 palmityl ether; PEG-75 Stearate and combinations thereof. Other useful nonionic surfactants are alkyl polyglycosides such as lauryl polyglucoside available from the Henkel Corporation. Another class of nonionic surfactants are the long chain tertiary amine oxides.
Alkyl Mono Esters:
[0036] The inventive cleansing composition contains alkyl mono ester(s) comprising linear and/or branched alkyl mono ester(s) not exceeding an alkyl number of 20 where the molecular weight of the ester(s) is/are less than 320. Preferably the minimum alkyl chain length is 5. Examples of alkyl mono esters useful in the invention include, but are not limited to, one or more of the following: isodecyl neopentanoate, ethylhexyl isononanoate, isopropyl myristate, blends thereof and the like. Such alkyl mono esters may be obtained from the following suppliers:
Isodecyl Neopentanoate,
[0037] NEOLIGHT 100P, IPM-R, and ES108109 available from (Kokyu Alcohol Kogyo Co. Ltd, Narita, Chiba, Japan); DUB VCI-10 available from (Stearinerie Dubois, Boulogne-Billancourt, France)
Ethylhexyl Isononanoate,
[0038] ES108109 available from (Kokyu Alcohol Kogyo Co. Ltd, Narita, Chiba, Japan); EMALEX NIO-98 available from (Nihon Emulsion Co. Ltd, Tokyo, Japan)
Isopropyl Myristate
[0039] IPM-R available from (Kokyu Alcohol Kogyo Co. Ltd, Narita, Chiba, Japan);
[0040] IPM available from BASF SE, Ludwigshafen, Germany)
Hydrocarbon Oils:
[0041] The inventive cleansing composition contains hydrocarbon oil(s). Hydrocarbon oil(s) suitable for the present invention include mineral oil, isoparaffins and poly alpha-olefins (such as those available under the trademark Permethyl 99A or 101), and polyisobutenes.
[0042] Preferably these oils have a coefficient of kinematic viscosity not exceeding 300 (mm2/s) at 25° C. as determined using a Brookfield Model LVDV-II+ viscometer.
[0043] Examples of oils useful in the invention include one or more of the following: Mineral oil, Liquid paraffin, Squalene, blends thereof and the like. Useful oils include the following: Carnation and Blandol mineral oils available from Sonneborn LLC, Parsippany N.J., USA; Rajol WP 70 liquid paraffin available from Raj Petro Specialties P.LTD, Mumbai, India; and Parleam 4 Hydrogenated Polyisobutene (C13-16 Isoparaffin), EX and 6 Hydrogenated Polyisobutenes all available from NOF CORPORATION, Japan.
Polyols
[0044] Polyols are preferably present in compositions of this invention. These polyols may be monomeric or polymeric and are preferably liquid at 25 C. Monomeric polyols may have from 1 to 20 carbon atoms and from 2 to 10 hydroxyls. Illustrative monomeric polyols include glycerine, propylene glycol; glycerol; 1,4-butane diol; 1,3-butane diol; 1,2-butane diol; 1-6-hexanediol, 1,2-hexane diol; 3-methyl-1,3-butane diol; 2-methyl-1,3-propane diol, sorbitol and mixtures thereof. Particularly preferred are glycerin, propylene glycol, and 1,3-butane diol. Polymeric polyols are illustrated by polypropylene glycol, polyethylene glycol, dipropylene glycol, diglycerol, polyglycerol, trimethylene glycol, dipentaerythritol and combinations thereof.
Miscellaneous Agents
[0045] Thickening agents may optionally be included in compositions of the present invention. Particularly useful are the polysaccharides. Examples include starches, natural/synthetic gums and cellulosics. Representative of the starches are chemically modified starches such as sodium hydroxypropyl starch phosphate and aluminum starch octenylsuccinate. Tapioca starch is often preferred. Suitable gums include xanthan, sclerotium , pectin, karaya, arabic, agar, guar, carrageenan, alginate and combinations thereof. Suitable cellulosics include hydroxypropyl cellulose, hydroxypropyl methylcellulose, ethylcellulose and sodium carboxy methylcellulose. Synthetic polymers are yet another class of effective thickening agent. This category includes crosslinked polyacrylates such as the Carbomers, polyacrylamides such as Sepigel® 305 and taurate copolymers such as Simulgel EG® and Aristoflex® AVC, the copolymers being identified by respective INCI nomenclature as Sodium Acrylate/Sodium Acryloyldimethyl Taurate and Acryloyl Dimethyltaurate/Vinyl Pyrrolidone Copolymer. Another preferred synthetic polymer suitable for thickening is an acrylate-based polymer made commercially available by Seppic and sold under the name Simulgel INS100.
[0046] Amounts of the thickener, when used, may range from about 0.001 to about 5%, and preferably, from about 0.1 to about 3%, and most preferably, from about 0.2 to about 1.5% by weight of the composition including all ranges subsumed therein.
[0047] Fragrances, colorants, fixatives and abrasives may optionally be included in compositions of the present invention. Each of these substances may range from about 0.05 to about 5%, preferably between 0.1 and 3% by weight.
[0048] Turning to the actives suitable for use herein, the same can include opacifiers like TiO 2 and ZnO and colorants like iron oxide red, yellow and black. Such opacifiers and colorants typically have a particle size from 50 to 1200 nm, and preferably, from 50 to 350 nm.
[0049] To enhance skin moisturization, actives classified as cationic ammonium compounds may optionally be used in the compositions of this invention. Such compounds include salts of hydroxypropyltri (C 1 -C 3 alkyl) ammonium mono-substituted-saccharide, salts of hydroxypropyltri (C 1 -C 3 alkyl) ammonium mono-substituted polyols, dihydroxypropyltri (C 1 -C 3 alkyl) ammonium salts, dihydroxypropyldi (C 1 -C 3 alkyl) mono(hydroxyethyl) ammonium salts, guar hydroxypropyl trimonium salts, 2,3-dihydroxypropyl tri(C 1 -C 3 alkyl or hydroxalkyl) ammonium salts or mixtures thereof. In a most preferred embodiment and when desired, the cationic ammonium compound employed in this invention is the quaternary ammonium compound 1,2-dihydroxypropyltrimonium chloride. If used, such compounds typically make up from about 0.01 to about 30%, and preferably, from about 0.1 to about 15% by weight of the composition.
[0050] It is preferred that the composition comprises cationic compounds in combination with moisturizing agent. These moisturizing agents may include substituted ureas like hydroxymethyl urea, hydroxyethyl urea, hydroxypropyl urea; bis(hydroxymethyl) urea; bis(hydroxyethyl) urea; bis(hydroxypropyl) urea; N,N′-dihydroxymethyl urea; N,N′-di-hydroxyethyl urea; N,N′-di-hydroxypropyl urea; N,N,N′-tri-hydroxyethyl urea; tetra(hydroxymethyl) urea; tetra(hydroxyethyl) urea; tetra(hydroxypropyl) urea; N-methyl-N′-hydroxyethyl urea; N-ethyl-N,N—N′-hydroxyethyl urea; N-hydroxypropyl-N′-hydroxyethyl urea and N,N′-dimethyl-N-hydroxyethyl urea or mixtures thereof. Where the term hydroxypropyl appears, the meaning is generic for either 3-hydroxy-n-propyl, 2-hydroxy-n-propyl, 3-hydroxy-i-propyl or 2-hydroxy-i-propyl radicals. Most preferred is hydroxyethyl urea. The latter is available as a 50% aqueous liquid from the National Starch & Chemical Division of ICI under the trademark Hydrovance.
[0051] Amounts of substituted urea, when used, in the composition of this invention range from about 0.01 to about 20%, and preferably, from about 0.5 to about 15%, and most preferably, from about 2 to about 10% based on total weight of the composition and including all ranges subsumed therein.
[0052] It is highly preferred that in particular when cationic ammonium compound(s) and substituted urea(s) are used, at least from about 1 to about 15% glycerin is used, based on total weight of the composition and including all ranges subsumed therein.
[0053] Compositions of the present invention may include vitamins as the desired active. Illustrative vitamins are Vitamin A (retinol) as well as retinol esters like retinol palmitate and retinol propionate, Vitamin B 2 , Vitamin B 3 (niacinamide), Vitamin B 6 , Vitamin C, Vitamin E, Folic Acid and Biotin. Derivatives of the vitamins may also be employed. For instance, Vitamin C derivatives include ascorbyl tetraisopalmitate, magnesium ascorbyl phosphate and ascorbyl glycoside. Derivatives of Vitamin E include tocopheryl acetate, tocopheryl palmitate and tocopheryl linoleate. DL-panthenol and derivatives may also be employed. Total amount of vitamins when present in compositions according to the present invention may range from 0.001 to 10%, preferably from 0.01% to 1%, optimally from 0.1 to 0.5% by weight of the composition.
[0054] Azelaic acid, ubiquinone, dihydroxyacetone (DHA) and mixtures thereof may also be used as actives in the composition of this invention. Such compounds, when used, typically make up from about 0.2 to 4.5%, and preferably, from about 0.5 to 3% by weight of the composition, including all ranges subsumed therein.
[0055] Other optional actives suitable for use in this invention include resveratrol, resorcinols like 4-ethyl resorcinol, 4-hexyl resorcinol, 4-phenylethyl resorcinol, dimethoxytoluyl propyl resorcinol, 4-cyclopentyl resorcinol, 4-cyclohexylresorcinol, alpha-an/or beta-hydroxyacids, phenylethyl resorcinol (Symwhite 377 from Symrise), undecylenol phenylalanine (Seppi White from Seppic) mixtures thereof or the like. Such actives, when used, collectively make up from about 0.001 to about 12% by weight of the composition.
[0056] Desquamation promoters may be present. Illustrative are the alpha-hydroxycarboxylic acids, beta-hydroxycarboxylic acids. The term “acid” is meant to include not only the free acid but also salts and C 1 -C 30 alkyl or aryl esters thereof and lactones generated from removal of water to form cyclic or linear lactone structures. Representative acids are glycolic and its derivatives, lactic and malic acids. Salicylic acid is representative of the beta-hydroxycarboxylic acids. Amounts of these materials when present may range from about 0.01 to about 15% by weight of the composition.
[0057] A variety of herbal extracts may optionally be included as actives in compositions of this invention. The extracts may either be water soluble or water-insoluble carried in a solvent which respectively is hydrophilic or hydrophobic. Water and ethanol are the preferred extract solvents. Illustrative extracts include those from green tea, yarrow, chamomile, licorice, aloe vera, grape seed, citrus unshui, willow bark, sage, thyme and rosemary. Soy extracts may be used and especially when it is desirable to include retinol.
[0058] Also optionally suitable for use include materials like chelators (e.g., EDTA), C 8-22 fatty acid substituted saccharides, lipoic acid, retinoxytrimethylsilane (available from Clariant Corp. under the Silcare 1M-75 trademark), dehydroepiandrosterone (DHEA) and combinations thereof. Ceramides (including Ceramide 1, Ceramide 3, Ceramide 3B and Ceramide 6) as well as pseudoceramides may also be useful. Occlusives like Oilwax LC are often desired. Amounts of these materials may range from about 0.000001 to about 10%, preferably from about 0.0001 to about 1% by weight of the composition.
[0059] Sunscreen actives may also be included in compositions of the present invention as described herein. Particularly preferred are such materials as phenylbenzimidazole sulfonic acid (Ensulizole), ethylhexyl p-methoxycinnamate, available as Parsol MCX®, Avobenzene, available as Parsol 1789® and benzophenone-3, also known as Oxybenzone. Inorganic sunscreen actives may be employed such as microfine titanium dioxide, zinc oxide, polyethylene and various other polymers. Also suitable for use is octocrylene. Amounts of the sunscreen agents when present may generally range from 0.1 to 30%, preferably from 0.5 to 20%, optimally from 0.75 to 10% by weight.
[0060] Conventional buffers/pH modifiers may be used. These include commonly employed additives like sodium hydroxide, potassium hydroxide, hydrochloric acid, citric acid and citrate/citric acid buffers. In an especially preferred embodiment, the pH of the composition of this invention is from about 4 to about 8, and preferably, from about 4.25 to about 7.75, and most preferably, from about 6 to about 7.5, including all ranges subsumed therein. The Brookfield viscosity of the inventive composition is preferably in the range of 1 to 200 cps, more preferably in the range of 10 to 150 cps as preferably measured by a Brookfield viscometer, preferably Model LVDV-II+, and with a Spindle No. 1, 50 rpm, at 25° C., preferably measured after 30 sec.
[0061] The invention will now be described in greater detail by way of the following non-limiting examples. The examples are for illustrative purposes only and not intended to limit the invention in any way. Physical test methods are described below:
[0062] Except in the operating and comparative examples, or where otherwise explicitly indicated, all numbers in this description indicating amounts or ratios of materials or conditions of reaction, physical properties of materials and/or use are to be understood as modified by the word “about”.
[0063] Where used in the specification, the term “comprising” is intended to include the presence of stated features, integers, steps, components, but not to preclude the presence or addition of one or more features, integers, steps, components or groups thereof.
[0064] All percentages in the specification and examples are intended to be by weight unless stated otherwise.
Example 1
[0065] A series of inventive and comparative examples were made according to Tables 1 and 2 respectively using the procedure described below in order to evaluate clarity, stability and skin feel.
[0000]
TABLE 1
Inventive examples:
D
E
F
G
Stability
Stable
Stable
Stable
Stable
Rinsing
Fast
Fast
Fast
Fast
HLB(AVE)
11.29
11.29
11.29
11.29
chemical name
HLB
MIU
MW
WT. %
WT. %
WT. %
WT. %
oil
Mineral Oil
0.37
—
34.05
30.05
30.05
30.05
Fatty esters
ISODECYL NEOPENTANOATE
0.15
242.4
5
30
ETHYLHEXYL ISONONANOATE
0.15
270.4
30
ISOPROPYL MYRISTATE
0.21
270.4
21
30
TRIETHYLHEXANOIN
0.3
470.6
DIETHYLHEXYL SUCCINATE
0.31
342.5
BIS-ETHOXYDIGLYCOL SUCCINATE
0.41
350.4
Nonionic surfactant
PEG-75 STEARATE
19
0.5
0.5
0.5
0.5
POLYSORBATE 80
15
3
3
3
3
SORBETH-30 TETRAISOSTEARATE
11.1
PEG-20 Glyceryl Triisostearate
11
11.1
11.1
11.1
11.1
Sorbitan Isostearate
9
PEG-20 Hydrogenated Castor Oil
8
3.6
3.6
3.6
3.6
Isostearate
Polyol
Propylene glycol
14.5
14.5
14.5
14.5
C12-C20 n-alkyl Fatty acid(s)
0.3
0.3
0.3
0.3
Water
6
6
6
6
Additives
perfume, colors, preservatives, pH
0.95
0.95
0.95
0.95
adjusters etc.
Total
100
100
100
100
[0000]
TABLE 2
Comparative examples.
A
B
C
H
J
J
K
Stability
Stable
Stable
Stable
un-stable
un-stable
un-stable
un-stable
Rinsing
Slow
Slow
Slow
N/A
N/A
N/A
N/A
HLB(AVE)
10.63
10.63
10.63
11.29
11.29
11.29
11.29
chemical name
HLB
MIU
MW
WT. %
WT. %
WT. %
WT. %
WT. %
WT. %
WT. %
oil
Mineral Oil
0.37
—
29.25
33.25
29.25
30.05
30.05
30.05
60.05
Fatty esters
ISODECYL
0.15
242.4
30
5
NEOPENTANOATE
ETHYLHEXYL
0.15
270.4
ISONONANOATE
ISOPROPYL MYRISTATE
0.21
270.4
21
30
TRIETHYLHEXANOIN
0.3
470.6
30
DIETHYLHEXYL
0.31
342.5
30
SUCCINATE
BIS-ETHOXYDIGLYCOL
0.41
350.4
30
SUCCINATE
Nonionic surfactant
PEG-75 STEARATE
19
0.5
0.5
0.5
0.5
POLYSORBATE 80
15
3
3
3
3
SORBETH-30
11.1
5
5
5
TETRAISOSTEARATE
PEG-20 Glyceryl
11
11
11
11
11.1
11.1
11.1
11.1
Triisostearate
Sorbitan
9
1.5
1.5
1.5
Isostearate
PEG-20
8
1.5
1.5
1.5
3.6
3.6
3.6
3.6
Hydrogenated
Castor Oil
Isostearate
Polyol
Propylene glycol
14.5
14.5
14.5
14.5
14.5
14.5
14.5
C12-C20 n-alkyl
0.3
0.3
0.3
0.3
0.3
0.3
0.3
Fatty acid(s)
Water
6
6
6
6
6
6
6
Additives
perfume, colors,
0.95
0.95
0.95
0.95
0.95
0.95
0.95
preservatives, pH
adjusters etc.
Total
100
100
100
100
100
100
100
[0066] Based on the results reported in Tables 1 and 2, it is evident that clarity, stability and skin feel sensory results was generally better for the inventive samples when compared to the comparative samples.
Example 2
[0067] Selected comparative and inventive compositions described in Tables 1 and 2 were tested by an expert test panel for perception of skin feel after rinsing according to the procedure described below and the results are shown in Table 3.
[0000]
TABLE 3
Rinsing test results
A
B
C
D
E
G
Results
Slow
Slow
Slow
Fast
Fast
Fast
Slow
Slow
Slow
Fast
Fast
Fast
Moderate
Moderate
Slow
Fast
Fast
Fast
Moderate
Moderate
Moderate
Fast
Fast
Fast
Expert panel who can assess rinsing speed accurately has been screened by Pre-test from 10 experts.
Assessed 4 replicates by expert panel.
Whole face, Home in use. Blind, 1 day usage/1 product
Evaluated speed of rinsing by 3 point scale
(1: slow, 2: moderate and 3: fast)
a. Preparation of the examples illustrated in Tables 1-2:
1. Weigh all raw materials except for perfume in a beaker as appropriate.
2. Heat beaker contents to 85 C in a hot water bath to 90 C and hold for 10 min.
3. Blend gently via stirring for 5 min with a stirring rod.
4. Cool the beaker contents to 45 C.
5. Add Perfume and gently resume stirring for 5 min.
b. MIU frictional coefficient measurement method
[0078] Measurement Method of Friction in the Present Invention
1) A drop of the compound to be tested (0.1 mL) is applied on artificial leather*. 2) Measurement is started according to the following conditions.
[0081] Measurement Conditions
Apparatus: Friction Tester KES-SE (Kato Tech Co., Ltd.) Temperature: 25+/−3° C. Humidity: 65+/−3% RH (Relative humidity) Load: 25 g Detector: Silicone sensor Artificial Leather: Tricot whose surface is treated with polyurethane and coated with collagen. Supplier: Idemitsu Technofine Co., Ltd. (Japan)/Ideatex Japan Co Ltd. This is available under the tradename Sapulale.
3. MIU is calculated via the graphical method illustrated in FIG. 3 . The friction μ measured over a distance x, equals
[0000]
1
X
∫
0
x
μ
dx
[0088] The number of “MIU” is automatically provided by the KES-SE friction tester. The number of X is the actual distance of continuous measurement which affect to measurement accuracy. This equation exemplifies that the average of the friction coefficient equals MIU, derived from a continuous friction coefficient measurement. As known in the art, by dividing the integrated value by the monitoring width X, the mean coefficient of friction MIU is obtained.
[0089] The foregoing description and examples illustrate selected embodiments of the present invention. In light thereof variations and modifications will be suggested to one skilled in the art, all of which are within the scope and spirit of this invention.
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A cleansing composition is provided for removing waxy makeup, and for cleansing the skin with excellent rinse speed and after-feel. The inventive composition is also transparent and stable to phase separation and includes specific amounts of high average HLB nonionic surfactants, specific alkyl mono esters, hydrocarbon oils and polyol(s) and in a preferred embodiment contains very low levels of or no silicone oils.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] The present application is a US National Stage of International Application No. PCT/CN2009/000668, filed 18 Jun. 2009, designating the United States, and claiming priority to Chinese Patent Application No. 200810115310.2 filed 20 Jun. 2008.
FIELD OF THE INVENTION
[0002] The present invention relates to the field of communications and particularly to a distributed antenna system and a data transmission method thereof and a central controller.
BACKGROUND OF THE INVENTION
[0003] The International Telecommunication Union (ITU) is very demanding for the performance of the next generation mobile communication system of International Mobile
[0004] Telecommunications-Advanced (IMT-Advanced), for example, regarding the maximum system transmission bandwidth up to 100 MHz and peak rates of uplink and downlink data transmission up to 500 Mbps/Hz and 1 Gbps/Hz, and also very demanding for an average spectrum efficiency and an edge spectrum efficiency of the system.
[0005] In order to accommodate the IMT-Advanced system, the 3 rd Generation Partner Project (3GPP) has proposed in its next generation mobile cellular communication system of Long Term Evolution (LET)-Advanced the use of a technology of distributed antennas to improve the performance of the system. The technology of distributed antennas refers to that antennas are distributed uniformly in a geographical area and all of the antennas are connected with a central controller through transmission lines, e.g., optical fibers, etc., so that the distance between each pair of distributed antennas is generally far above ten times the wavelength of a carrier. The central controller controls an antenna transmitting a signal to a user equipment at a time and receives a signal originated from a user equipment. FIG. 1 illustrates a scenario of downlink transmitting data at a moment of time T. At the moment of time T, the central controller selects three distributed antennas for transmission of data from a base station to a user equipment
[0006] The technology of distributed antennas is considered in the 3GPP LTE-Advanced as a rather promising multiple antenna technology to improve the throughout and spectrum utilization factor of a dense cell system and has become a hot area of research in the LTE-Advanced. Distributed antennas can improve the capacity and cell edge transmission efficiency of a system, avoid inter-cell interference and improve the overall performance of the system. In an existing communication system, however, there has been a lack of an established specific solution to a design of distributed antennas.
SUMMARY OF THE INVENTION
[0007] An embodiment of the invention provides a data transmission method for a distributed antenna system to enforce a solution of distributed antennas in a communication system and improve the performance of the communication system. The system includes a central controller and a plurality of radio transceiver units, the data transmission method includes:
[0008] measuring, by the radio transceiver units, power information of a received user equipment pilot reference signal; and transmitting, by the radio transceiver, the power information to the central controller;
[0009] selecting, by the central controller, a set of radio transceiver units for transmission of data to a user equipment according to the power information of the user equipment pilot reference signal transmitted from the radio transceiver units;
[0010] processing, by the central controller, the data according to the set of radio transceiver units;
[0011] distributing, by the central controller, the processed data to the radio transceiver units in the set of radio transceiver units; and
[0012] performing, by the radio transceiver units in the set of radio transceiver units, downlink transmission of the data.
[0013] An embodiment of the invention further provides a central controller for a distributed antenna system to enforce a solution of distributed antennas in a communication system and improve the performance of the communication system, the central controller includes:
[0014] a reception module, configured to receive power information of a user equipment pilot reference signal transmitted from a plurality of radio transceiver units;
[0015] a selection module, configured to select a set of radio transceiver units for transmission of data to a user equipment according to the received power information of the user equipment pilot reference signal transmitted from the radio transceiver units;
[0016] a data processing module, configured to process the data according to the set of radio transceiver units; and
[0017] a transmission module, configured to distribute the processed data to the radio transceiver units in the set of radio transceiver units.
[0018] An embodiment of the invention further provides a distributed antenna system to enforce a solution of distributed antennas in a communication system and improve the performance of the communication system, the system includes:
[0019] a plurality of radio transceiver units, configured to measure power information of a received user equipment pilot reference signal, to transmit the power information and to perform downlink transmission of data; and
[0020] a central controller, configured to select a set of radio transceiver units for transmission of the data to a user equipment according to the power information of the user equipment pilot reference signal transmitted from the radio transceiver units, to process the data according to the set of radio transceiver units and to distribute the processed data to the radio transceiver units in the set of radio transceiver units.
[0021] In embodiments of the invention, radio transceiver units measure power information of a received user equipment pilot reference signal, and transmit the power information to a central controller, the central controller selects a set of radio transceiver units for transmission of data to a user equipment according to the power information of the user equipment pilot reference signal transmitted from the radio transceiver units, processes the data according to the set of radio transceiver units and distributes the processed data to the radio transceiver units in the set of radio transceiver units, and the radio transceiver units in the set of radio transceiver units perform downlink transmission of the data, thereby enforcing a solution of distributed antennas in a communication system and improve the performance of the communication system.
BRIEF DESCRIPTION OF THE DRAWINGS
[0022] FIG. 1 illustrates a schematic diagram of implementing distributed antennas in the prior art;
[0023] FIG. 2 illustrates a flow chart of a data transmission process for distributed antennas according to an embodiment of the invention;
[0024] FIG. 3 illustrates a schematic diagram of implementing distributed antennas according to an embodiment of the invention;
[0025] FIG. 4 illustrates a schematic structural diagram of a central controller of a distributed antenna system according to an embodiment of the invention;
[0026] FIG. 5 illustrates a schematic structural diagram of a data processing module according to an embodiment of the invention;
[0027] FIG. 6 illustrates a schematic structural diagram of a processing unit according to an embodiment of the invention;
[0028] FIG. 7 illustrates a schematic structural diagram of a distributed antenna system according to an embodiment of the invention.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0029] Embodiments of the invention are detailed hereinafter with reference to the drawings.
[0030] A distributed antenna system according to an embodiment of the invention includes a central controller and a plurality of radio transceiver units. FIG. 2 illustrates a flow chart of a data transmission process for the distributed antenna system, particularly, the data transmission process comprising the following operations 201 - 205 .
[0031] Operation 201 . The radio transceiver units measure power information of a received user equipment pilot reference signal, and transmit the power information to the central controller.
[0032] Operation 202 . The central controller selects a set of radio transceiver units for transmission of data to a user equipment according to the power information of the user equipment pilot reference signal transmitted from the radio transceiver units.
[0033] Operation 203 . The central controller processes the data according to the set of radio transceiver units.
[0034] Operation 204 . The central controller distributes the processed data to the radio transceiver units in the set of radio transceiver units.
[0035] Operation 205 . The radio transceiver units in the set of radio transceiver units perform downlink transmission of the data.
[0036] Each of the radio transceiver units may include at least one antenna and may transmit or receive one or more data streams, and in an implementation, each of the radio transceiver units is configured to measure power information of a received user equipment pilot reference signal. A user equipment may transmit a pilot reference signal at a prescribed moment of time and in a prescribed frequency band dependent upon a configuration of a network, and the pilot reference signal may be referred to as a Sounding Reference Symbol or simply SRS. There may be multiple SRSs represented as SRS={SRS 1 ,SRS 2 , . . . ,SRS i , . . . ,SRS m } indicating a total number, m, of different SRSs, each of which is consisted of pilot reference signals transmitted over one or more antennas. As illustrated in FIG. 3 , the user equipment transmits two different SRSs represented as SRS={SRS 1 ,SRS 2 }, where a solid line represents the pilot reference signal SRS 1 and a dashed line represents the SRS 2 .
[0037] A user equipment may report power information of a pilot reference signal transmitted therefrom to an antenna in various ways, for example, report the absolute value of the power, the power headroom report, etc. In an implementation, the power of the user equipment pilot reference signal may alternatively be calculated from data transmission power reported from the user equipment arid the difference between the data transmission power and the power of the pilot reference signal.
[0038] A central controller may select a set of radio transceiver units for transmission of data to a user equipment according to the power information of the user equipment pilot reference signal transmitted from the radio transceiver units. As illustrated in FIG. 3 , the central controller selects a set of radio transceiver units represented as S={A 2 ,A 3 ,A 5 } for downlink transmission of the data to the user equipment, where S represents a subset of all the distributed antennas in an area covered by a base station on the network side.
[0039] In an embodiment, the central controller may determine, from the power information of the user equipment pilot reference signal transmitted from the radio transceiver units, channel status information in downlink transmission of the data from the radio transceiver units in the set of radio transceiver units and process the data according to the channel status information. In an implementation, the central controller may determine channel status information of uplink channels from the power information of user equipment pilot reference signal transmitted from the radio transceiver units and determine, from the channel status information of the uplink channels, channel status information of downlink channels in downlink transmission of the data from the radio transceiver units in the set of radio transceiver units, and further process the data according to the channel status information of the downlink channels.
[0040] The distributed antenna system according to an embodiment of the invention is applicable to a Time Division Duplex (TDD) system or a Frequency Division Duplex (FDD) system. Taking an application in the TDD system as an example, the central controller may determine the channel status information of the downlink channels from the channel status information of the uplink channels in view of the symmetry of the uplink and downlink channels. The channel status information of the downlink channels refers to status information of channels between each of downlink transmission antennas and a corresponding reception antenna of the user equipment, and includes information on the amplitude, phase, etc., of a signal. Due to the symmetry of the TDD uplink and downlink channels, the information on the phase of a signal transmitted from each uplink transmission antenna of the user equipment to a reception antenna of the base station is the same as that of a signal transmitted from the antenna of the base station to a reception antenna of the user equipment, thus the channel status information of the downlink channels can be determined from the channel status information of the uplink channels in view of the symmetry.
[0041] The channel status information may be a matrix of channel impulse responses. The central controller may determine a matrix of channel impulse responses of the downlink channels from a matrix of channel impulse responses of the uplink channels, i.e., a matrix of channel impulse responses of pilot reference signals transmitted from the user equipment up to the set of radio transceiver units S (a matrix H hereinafter). For example, the central controller may transpose the matrix H to convert channel phase status information of a reception matrix into channel phase status information of a transmission matrix.
[0042] In an embodiment, the central controller may further determine from the channel status information the number of data streams for transmission to the user equipment and subsequently process the data according to the number of data streams and the channel status information.
[0043] The central controller may determine from the matrix H the number, N, of data streams for transmission to the user equipment (equal to the number of parallel multiplexed data streams transmitted from the user equipment). Also as illustrated in FIG. 3 , channel impulse responses of pilot reference signals transmitted from the user equipment to the network side are represented as H={h 2 ,h 3 ,h 5 }, where h i represents a channel impulse response of a pilot reference signal up to a radio transceiver unit A i . In the case the user equipment transmits SRS 1 and SRS 2 to the network side, then h i =[h i,1 ,h i,2 ], where, h i,1 and h i,2 represent channel impulse responses of SRS 1 and SRS 2 up to the radio transceiver unit A i respectively. The central controller may determine from the matrix H the use of two parallel data streams for transmission of the data to the user equipment, and in a specific implementation, determine the number of data streams for transmission to the user equipment from eigen-values resulting from decomposition of the matrix H.
[0044] In an embodiment, processing, by the central controller, the data according to the channel status information may comprises: decomposing the matrix of channel impulse responses to derive vectors of shaping weights for each radio transceiver units in the set of radio transceiver units and subsequently performing a shaping weight process on the data for transmission from each radio transceiver units in the set of radio transceiver units according to the derived vectors of shaping weights.
[0045] Specifically, the matrix H is decomposed through for example the Singular Value Decomposition (SVD) or the Eigen-Value Decomposition (EVD), to derive vectors of shaping weights, i.e., W i ={W i,1 , W i,2 , . . . ,W i,j , . . . ,W i,N } for each radio transceiver units in the set of radio transceiver units S transmitting a number, N, of data streams to the user equipment, where w i,j represents a shaping weight of the j th data stream of the i th radio transceiver unit.
[0046] The data streams for transmission may be preprocessed according to the vectors of shaping weights by multiplying the data streams for transmission with the vectors of shaping weights, so that the data streams for transmission can be better configured to the status of the channel and therefore the power of the downlink data can be more concentrated with less interference and a higher signal noise ratio, thus improving the capacity of the system.
[0047] In an implementation, the central controller may weight one or more streams of data respectively according to the weights for each stream of each radio transceiver unit and transmit the weighted data to the radio transceiver units in the set of radio transceiver units among which the data is shaped jointly. The same stream of data is processed according to different shaping weights for one or more units A i and then transmitted.
[0048] The central controller may further distinguish data transmitted from different units A i , where different data may be transmitted from different units A i and one or more streams may be transmitted from one unit A i . The central controller transmits data streams for transmission from different units A i to the corresponding radio transceiver units, and the radio transceiver units transmit different data respectively.
[0049] In an embodiment, control signaling may be further carried in the data for downlink transmission from the radio transceiver units in the set of radio transceiver units at the network side according to a Channel Quality Indicator (CQI) reported from the user equipment and a transmission channel condition, to indicate an OFDM resource in the time and frequency domains to be occupied for the data streams for transmission, and subsequently the user equipment may receive the downlink data over the OFDM resource in the time and frequency domains indicated in the controlling signaling. The control signaling may further indicate the number of data streams for transmission, and the user equipment may receive the data streams of this number.
[0050] In an embodiment, the control signaling may further include a modulation scheme and an encoding rate of the downlink data, and subsequently the user equipment may demodulate the received downlink data in the modulation scheme of the downlink data in the control signaling and decode the demodulated downlink data at the encoding rate of the downlink data in the control signaling.
[0051] In an embodiment, when the shaping weighted data streams are transmitted to the user equipment through the set of radio transceiver units S, dedicated pilots for the user equipment to decode the data may further be included in the OFDM resource block in the time and frequency domains occupied for the transmission of the data. The number of dedicated pilots is equal to the number of transmitted downlink data streams, and the dedicated pilots are processed prior to transmission according to the set of radio transceiver units. Specifically, the dedicated pilots may be processed according to the channel status information of the downlink channels, for example, according to the same shaping weights for the downlink data transmitted over the OFDM resource in the time and frequency domains. For example, a dedicated pilot D i corresponds to the shaping weight of the data stream i over the corresponding resource in the time and frequency domains. Subsequently, the user equipment may demodulate the received downlink data according to the received dedicated pilots.
[0052] Based upon a similar inventive concept, an embodiment of the invention further provides a central controller for a distributed antenna system. The central controller is structured as illustrated in FIG. 4 and includes:
[0053] a reception module 401 , configured to receive power information of a user equipment pilot reference signal transmitted from a plurality of radio transceiver units each of which includes at least one antenna;
[0054] a selection module 402 , configured to select a set of radio transceiver units for transmission of data to a user equipment according to the received power information of the user equipment pilot reference signal transmitted from the radio transceiver units;
[0055] a data processing module 403 , configured to process the data according to the set of radio transceiver units; and
[0056] a transmission module 404 , configured to distribute the processed data to the radio transceiver units in the set of radio transceiver units.
[0057] As illustrated in FIG. 5 , the data processing module 403 in an embodiment may include:
[0058] a determination unit 4031 , configured to determine, from the power information of the user equipment pilot reference signal transmitted from the a plurality of radio transceiver units, channel status information in downlink transmission of the data from the radio transceiver units in the set of radio transceiver units; and
[0059] a processing unit 4032 , configured to process the data according to the channel status information.
[0060] In an embodiment, the channel status information includes a matrix of channel impulse responses, and as illustrated in FIG. 6 , the processing unit 4032 may include:
[0061] a decomposition sub-unit 601 , configured to decompose the matrix of channel impulse responses to derive vectors of shaping weights for each of the radio transceiver units in the set of radio transceiver units; and
[0062] a shaping weight sub-unit 602 , configured to perform a shaping weight process on the data for transmission from each of the radio transceiver units in the set of radio transceiver units according to the derived vectors of shaping weights.
[0063] In an embodiment, the determination unit 4031 may further be configured to determine the number of data streams for transmission to the user equipment from the channel status information, and then the processing unit 4032 may further be configured to process the data according to the number of data streams and the channel status information.
[0064] Based upon a similar inventive concept, an embodiment of the invention further provides a distributed antenna system. The system is structured as illustrated in FIG. 7 and includes:
[0065] a user equipment 701 , configured to transmit and receive data;
[0066] multiple antenna transceiver units 702 , configured to measure power information of a received user equipment pilot reference signal, to transmit the power information and to perform downlink transmission of data; and
[0067] a central controller 703 , configured to select a set of radio transceiver units for transmission of data to the user equipment according to the power information of the user equipment pilot reference signal transmitted from the radio transceiver units, to process the data according to the set of radio transceiver units and to distribute the processed data to the radio transceiver units in the set of radio transceiver units.
[0068] In an embodiment of the invention, radio transceiver units measure power information of a received user equipment pilot reference signal and transmit the power information to a central controller, the central controller selects a set of radio transceiver units for transmission of data to a user equipment according to the power information of the user equipment pilot reference signal transmitted from the radio transceiver units, processes the data according to the set of radio transceiver units and distributes the processed data to the radio transceiver units in the set of radio transceiver units, and the radio transceiver units in the set of radio transceiver units perform downlink transmission of the data, thereby enforcing a solution of distributed antennas in a communication system and improve the performance of the communication system.
[0069] Embodiments of the invention are applicable to a TDD system or an FDD system, and particularly for the TDD system, an applicable solution for processing of the data by the central controller according to the set of radio transceiver units is further proposed.
[0070] Evidently, those skilled in the art can make various modifications and variations to the invention without departing from the scope of the invention. Accordingly, the invention is also intended to encompass these modifications and variations thereto provided these modifications and variations come into the scope of the appended claims and their equivalences.
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A data transmission method and central controller for a distributed antenna system and a distributed antenna system. The system includes a central controller and multiple wireless transceiver units. The method includes that wireless transceiver units measure the power of the pilot reference signals received from user terminals and forward this power rate to a central controller; the central controller selects a set of wireless transceiver units for transmitting data to the terminal according to the pilot reference signal power rates of the terminals forwarded by the multiple wireless transceiver units; the central controller performs data processing according to said set of wireless transceiver units; the central controller distributes the processed data to the wireless transceiver units in said set of wireless transceiver units, and the wireless transceiver units in said set perform the downlink data transmission.
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[0001] This application claims the priority benefit under 35 U.S.C. §119 to Japanese Patent Application No. JP2013-139561 filed on Jul. 3, 2013, which disclosure is hereby incorporated in its entirety by reference.
BACKGROUND
[0002] 1. Field
[0003] The presently disclosed subject matter relates to a light guide plate and a side-edge type surface-emission optical apparatus including the light guide plate used in a liquid crystal display (LCD) unit.
[0004] 2. Description of the Related Art
[0005] Side-edge type surface-emission optical apparatuses used for LCD units are advantageous in terms of their thin and light structures.
[0006] FIG. 15A is a plan view illustrating a prior art side-edge type surface-emission optical apparatus, and FIGS. 15B and 15C are cross sectional views of the side-edge type surface-emission optical apparatus of FIG. 15A taken along the lines B-B and C-C, respectively, in FIG. 15A (see: FIGS. 1( a ) and 9 of JP2009-81094A & US2009/0086509A1).
[0007] In FIGS. 15A , 15 B and 15 C, the side-edge type surface-emission optical apparatus is constructed by a light guide plate 1 made of transparent material such as acryl resin or polycarbonate resin with a light incident surface S in , a light distributing control surface S cont perpendicular to the light incident surface S in and a light emitting surface S out opposing the light distributing control surface S cont . A light source 2 formed by a plurality of light emitting diodes (LEDs) is disposed on the light incident surface S in . Also, a prism sheet 3 , which is illustrated only in FIG. 15C , is disposed on the light emitting surface S out of the light guide plate 1 , and a Liquid crystal display (LCD) panel (not shown) is disposed outside of the prism sheet 3 . The prism sheet 3 is a single-face-deformed triangular prism sheet; however, the prism sheet 3 may have a cross section such as a curved cross section other than a triangular cross section. Further, a flexible reflective sheet 4 , which is illustrated only in FIGS. 15B and 15C , is disposed on the light distributing control surface S cont . The flexible reflective sheet 4 is operated to return light leaked from the light distributing control surface S cont thereto, thus enhancing the luminous intensity. In FIGS. 15B and 15C , note that the flexible reflective sheet 4 is apart from the light guide plate 1 ; however, the flexible reflective sheet 4 is actually in close proximity to the light distributing control surface S cont of the light guide plate 1 .
[0008] As illustrated in FIG. 15A , a plurality of flat mirror-finish portions 11 are provided on the light distributing control surface S cont of the light guide plate 1 and extend from the light incident surface S in . The flat mirror-finish portions 11 serve as means for spreading light to the inner part of the light guide plate 1 . In this case, the farther from the light incident surface S in a location of the flat mirror-finish portions 11 , the smaller the width of the flat mirror-finish portions 11 at that location. A plurality of triangular prism sequences 12 are provided on areas of the light distributing control surface S cont of the light guide plate 1 where the flat mirror-finish portions 11 are not provided. The triangular prism sequences 12 are protruded with respect to the flat mirror-finish portions 11 . Each of the triangular prism sequences 12 includes a plurality of equidistantly-arranged triangular prisms for bending the path of light. In this case, the farther from the light incident surface S in a location of the triangular prism sequences 12 , the larger the width of the triangular prism sequences 12 at that location. Thus, much more light is totally reflected by the triangular prism sequences 12 , to realize a uniform surface emission.
[0009] In FIG. 16 , which is a partly-enlarged cross sectional view of the light guide plate 1 of FIG. 15A , 15 B and 15 C, each prism 12 P of the triangular prism sequences 12 per pitch P 0 has an asymmetrical structure formed by a straight-type rising sloped surface 12 a whose slope angle is defined by α0, and a straight-type falling sloped surface 12 b whose slope angle is defined by α1 (≠α0). Particularly, the falling sloped surface 12 b carries out a light distributing control to bend the path of light. In order to enhance the luminous intensity of a surface-emission along the normal direction to the prism sheet 3 , the slope angle α1 of the falling sloped surface 12 b with respect to the flat mirror-finish portions 11 is preferably as small as possible, for example.
[0000] 4°≦α1≦5°
[0000] As a result, spatial light distribution characteristics of the light guide plate 1 with a narrow full-width at half maximum as shown in FIG. 17 can be realized. In FIG. 17 , note that the full-width at half maximum is 25° with a range from 55° to 80°. Also, the slope angle α0 of the rising sloped surface 12 a with respect to the flat mirror-finish portions 11 is 12 a with respect to the flat mirror-finish portions 11 is
[0000] 15°≦α0≦90°
[0010] Thus, light distribution characteristics of the prism sheet 3 as shown in FIG. 18 with a high emission along the normal direction to the prism sheet 3 can be realized.
[0011] In the side-edge type surface-emission optical apparatus of FIGS. 15A , 15 B and 15 C, in order to further enhance the luminous intensity along the normal direction to the prism sheet 3 , the slope angle α1 of the falling sloped surface 12 b with respect to the flat mirror-finish portions 11 is preferably smaller than 4″. As a result, the falling sloped surface 12 b on the side of the light source 2 is approximately in parallel with the flat mirror-finish portions 11 . Therefore, as illustrated in FIG. 19 , the flexible reflective sheet 4 is in broad contact with the falling sloped surface 12 b so that a region R with no air gap may be generated between the falling sloped surface 12 b and the flexible reflective sheet 4 . In the region R, the flexible reflective sheet 4 partly spreads light reflected at the falling sloped surface 12 b , so that a so-called wet-out phenomenon inviting irregular patterns as illustrated in FIG. 20 may occur in the light emitting surface S out of the light guide plate 1 , which would degrade the light distribution characteristics of the prism sheet 3 of FIG. 18 .
SUMMARY
[0012] The presently disclosed subject matter seeks to solve one or more of the above-described problems.
[0013] According to the presently disclosed subject matter, in a light guide plate having a light incident surface, a light distributing control surface perpendicular to the light incident surface and a light emitting surface opposing the light distributing control surface, a flat mirror finishing portion is provided on a first area of the light distributing control surface, and a prism sequence is provided on a second area of the light distributing control surface where the flat mirror finishing portion is not provided. The prism sequence is protruded with respect to the flat mirror finishing portion. Each prism of the prism sequence has a rising sloped surface opposing the light incident surface, a first falling sloped surface connected to the rising sloped surface, and a second falling sloped surface connected to the first falling sloped surface. A slope of the first falling sloped surface is larger than a slope of the second falling sloped surface.
[0014] According to the presently disclosed subject matter, while the second falling sloped surface is not so sloped to improve the light distributing control efficiency, the first falling sloped surface is rapidly sloped, so that the angle between the first falling sloped surface and the rising sloped surface is reduced to form a sharper edge. As a result, when the light guide plate according to the presently disclosed subject matter is applied to a side-edge type surface-emission optical apparatus, the contact area between the light guide plate and the reflective sheet can be decreased to suppress the wet-out phenomenon.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] The above and other advantages and features of the presently disclosed subject matter will be more apparent from the following description of certain embodiments, taken in conjunction with the accompanying drawings, as compared with the prior art, wherein:
[0016] FIG. 1 is a cross-sectional view illustrating a side-edge type surface-emission optical apparatus including a first embodiment of the light guide plate according to the presently disclosed subject matter;
[0017] FIG. 2 is a partly enlarged cross-sectional view of the light guide plate of FIG. 1 ;
[0018] FIG. 3 is a cross-sectional view illustrating a contact state between the sloped surface of the light guide plate and the flexible reflective sheet of FIG. 1 ;
[0019] FIG. 4 is a graph illustrating proper states of the spatial light distribution characteristics of the light guide plate of FIG. 1 ;
[0020] FIG. 5 is a graph illustrating proper states of the light distribution characteristics of the prism sheet of FIG. 1 ;
[0021] FIG. 6 is a graph illustrating improper states of the spatial light distribution characteristics of the light guide plate of FIG. 1 ;
[0022] FIG. 7 is a graph illustrating improper states of the light distribution characteristics of the prism sheet of FIG. 1 ;
[0023] FIG. 8 is a cross-sectional view illustrating a side-edge type surface-emission optical apparatus including a second embodiment of the light guide plate according to the presently disclosed subject matter;
[0024] FIG. 9 is a partly-enlarged cross-sectional view of the light guide plate of FIG. 8 ;
[0025] FIG. 10 is a cross-sectional view illustrating a contact state between the sloped surfaces of the light guide plate and the flexible reflective sheet of FIG. 8 ;
[0026] FIG. 11 is a cross-sectional view illustrating a side-edge type surface-emission optical apparatus including a third embodiment of the light guide plate according to the presently disclosed subject matter;
[0027] FIG. 12 is a partly-enlarged cross-sectional view of the light guide plate of FIG. 11 ;
[0028] FIG. 13 is a cross-sectional view illustrating a contact state between the sloped surfaces of the light guide plate and the flexible reflective sheet of FIG. 11 ;
[0029] FIG. 14 is a cross-sectional view illustrating a modification of the side-edge type surface-emission optical apparatus of FIG. 12 ;
[0030] FIG. 15A is a plan view illustrating a prior art side-edge type surface-emission optical apparatus;
[0031] FIGS. 15B and 15C are cross-sectional views of the side-edge type surface-emission optical apparatus of FIG. 15A taken along the lines B-B and C-C, respectively, in FIG. 15A ;
[0032] FIG. 16 is a partly-enlarged cross-sectional view of the light guide plate of FIGS. 15A , 15 B and 15 C;
[0033] FIG. 17 is a graph illustrating spatial light distribution characteristics of the light guide plate of FIGS. 15A , 15 B and 15 C;
[0034] FIG. 18 is a graph illustrating light distribution characteristics of the prism sheet of FIGS. 15A , 15 B and 15 C;
[0035] FIG. 19 is a cross-sectional view illustrating a contact state between the sloped surfaces of the light guide plate and the flexible reflective sheet of FIGS. 15A , 158 and 15 C; and
[0036] FIG. 20 is a perspective view for explaining the wet-out phenomenon in FIGS. 15A , 15 B and 15 C.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
[0037] In FIG. 1 , which is a cross-sectional view illustrating a side-edge type surface-emission optical apparatus including a first embodiment of the light guide plate according to the presently disclosed subject matter, the light guide plate 1 of FIGS. 15A , 15 B and 15 C is replaced by a light guide plate 1 A whose triangular prism sequences 12 A are different from the triangular prism sequences 12 of FIGS. 15A , 15 B and 15 C.
[0038] In FIG. 2 , which is a partly-enlarged cross-sectional view of the light guide plate 1 A of FIG. 1 , each prism 12 PA of the triangular prism sequences 12 A per pitch P has an asymmetrical structure formed by a rising sloped surface 12 c whose slope angle is defined by β0, and two straight-type falling sloped surfaces 12 d and 12 e whose slope angles are defined by β1 and β2, respectively. The falling sloped surfaces 12 d and 12 e are straightly-sloped. In this case, the rising sloped surface 12 c can be either straightly-sloped or concavedly-sloped (curvedly-sloped). The slope angle β1 of the falling sloped surface 12 d with respect to the flat mirror-finish portions 11 and the slope angle β2 of the falling sloped surface 12 e with respect to the flat mirror-finish portions 11 satisfy the following:
[0000] β1>β2
[0039] That is, the falling sloped surface 12 d is more sloped than the falling sloped surface 12 e. Thus, a sharper edge is formed by the rising sloped surface 12 c and the falling sloped surface 12 d. On the other hand, the slope angle β0 of the rising sloped surface 12 c with respect to the flat mirror finish portions 11 is the same as the slope angle α0 of FIG. 16 , i.e.,
[0000] 15°≦β0≦90°
[0040] In FIG. 2 , in order to suppress the wet-out phenomenon, the slope angle β1 of the falling sloped surface 12 d satisfies the following formula (1):
[0000] 3°<β1<8° (1)
[0041] On the other hand, in order to enhance the light distributing control efficiency, the slope angle β2 of the falling sloped surface 12 e satisfies the following formula (2):
[0000] 0.5°<β2<3° (2)
[0042] Further, the following formula (3) is satisfied:
[0000] 2 ·S 12d ≦S 12e ≦6 ·S 12d (3)
[0043] where S 124 is the area of the falling sloped surface 12 d ; and
[0044] S 12e is the area of the falling sloped surface 12 e.
[0045] If S 12e /2·S 12d , the falling sloped surface 12 d would adversely affect the light distributing control efficiency, to increase the full-width at half maximum of the spatial light distributing characteristics. On the other hand, if S 12e >6·S 12d , the falling sloped surface 12 d is increased to reduce the suppressing effect of the wet-out phenomenon.
[0046] Also, the pitch P of the prisms 12 PA is
[0000] 15 μm≦P≦250 μm
[0047] The minimum height of the falling sloped surface 12 d is about 1 μm in order to sufficiently exhibit the suppressing effect of the wet-out phenomenon. In this case, the minimum value of the pitch P is about 15 μm. On the other hand, if the pitch P is larger than the maximum value 250 μm, each prism 12 PA can be recognized as dots in the LCD unit.
[0048] According to the first embodiment, as illustrated in FIG. 3 , due to a sharper edge formed by the rising sloped surface 12 c and the falling sloped surface 12 d, the contact area between the flexible reflective sheet 4 and the rising sloped surface 12 c as well as the contact area between the flexible reflective sheet 4 and the falling sloped surface 12 d is reduced to suppress the wet-out phenomenon.
[0049] In FIG. 4 , which is a graph illustrating proper states of the spatial light distribution characteristics of the light guide plate 1 A, a state I to satisfy the formulae (1), (2) and (3) is defined by
[0000] β1=7°
[0000] β2=1°
[0000] S 12e =5 ·S 12d
[0050] Also, a state II to satisfy the formulae (1), (2) and (3) is defined by
[0000] β1=4°
[0000] β2=2°
[0000] S 12e =2 ·S 12d
[0051] In the state I, the full-width at half maximum of the spatial light distribution characteristics of the light guide plate 1 A as illustrated in FIG. 4 is reduced to 14° with a range from 68° to 82° as compared with the prior art where the full-width at half maximum is 25° with a range from 55° to 80°. As a result, as illustrated in FIG. 5 , the luminous intensity of a surface-emission along the normal direction to the prism sheet 3 can be increased as compared with the prior art.
[0052] Also, in the state II, the full-width at half maximum of the spatial light distribution characteristics of the light guide plate IA as illustrated in FIG. 4 is reduced to 18° with a range from 63° to 81° as compared with the prior art where the full-width at half maximum is 25° with a range from 55° to 80°. As a result, as illustrated in FIG. 5 , the luminous intensity of a surface-emission along the normal direction to the prism sheet 3 can be increased as compared with the prior art.
[0053] In FIG. 6 , which is a graph illustrating improper states of the spatial light distribution characteristics of the light guide plate 1 A, a state III to satisfy the formulae (1) and (2) and not satisfy the formula (3) is defined by
[0000] β1=6°
[0000] β2=2°
[0000] S 12e =3 ·S 12d
[0054] Also, a state IV to satisfy the formulae (2) and (3) and not satisfy the formula (1) is defined by
[0000] β1=8°
[0000] β2=1°
[0000] S 12e =3 ·S 12d
[0055] In the state III, the full-width at half maximum of the spatial light distribution characteristics of the light guide plate 1 A as illustrated in FIG. 6 is 24° with a range from 56° to 80° which is almost the same as that of the prior art where the full-width at half maximum is 25° with a range from 55° to 80°. As a result, as illustrated in FIG. 7 , the luminous intensity of a surface-emission along the normal direction to the prism sheet 3 is almost the same as that of the prior art.
[0056] Also, in the state IV, the full-width at half maximum of the spatial light distribution characteristics of the light guide plate 1 A as illustrated in FIG. 6 is 23° with a range from 57° to 80° which is almost the same as that of the prior art where the full-width at half maximum is 25° with a range from 55° to 80°. As a result, as illustrated in FIG. 7 , the luminous intensity of a surface-emission along the normal direction to the prism sheet 3 is almost the same as that of the prior art.
[0057] In FIG. 8 , which is a cross-sectional view illustrating a side-edge type surface-emission optical apparatus including a second embodiment of the light guide plate according to the presently disclosed subject matter, the light guide plate 1 A of FIG. 1 is replaced by a light guide plate 1 B whose triangular prism sequences 12 B are different from the triangular prism sequences 12 A of FIG. 1 .
[0058] In FIG. 9 , which is a partly-enlarged cross-sectional view of the light guide plate 1 B of FIG. 8 , the straight-type falling sloped surface 12 d of FIG. 2 is replaced by a concave-type falling sloped surface 12 d′ . The concave-type falling sloped surface 12 d′ is tangentially-curved and extended from the straight-type falling sloped surface 12 e; however, the concave-type falling sloped surface 12 d ′ is not always tangentially-curved. Also, the concave-type falling sloped surface 12 d ′ is curvedly-sloped with one radius of curvature. In any case, the concave-type falling sloped surface 12 d ′ is more sloped than the straight-type falling sloped surface 12 e. Thus, a sharper edge is formed by the rising sloped surface 12 c and the concaved-type falling sloped surface 12 d′.
[0059] In FIG. 9 , in order to suppress the wet-out phenomenon, the slope angle β1′ of a line segment between the ends of the concave-type falling sloped surface 12 d ′ satisfies the following formula (1′) in the same way as the formula (1):
[0000] 3°<β1′<8° (1′)
[0060] On the other hand, in order to enhance the light distributing control efficiency, the slope angle β2 of the straight-type falling sloped surface 12 e satisfies the following formula (2′) in the same way as the formula (2):
[0000] 0.5°<β2<3° (2′)
[0061] Further, the following formula (3′) in the same way as the formula (3) is satisfied:
[0000] 2 ·S 12d ′≦S 12e ≦6· S 12d ′ (3′)
[0062] where S 12d ′ is the area of the concave-type falling sloped surface 12 d′; and
[0063] S 12e is the area of the straight-type falling sloped surface 12 e.
[0064] The formula (3′) can be modified to the following formula:
[0000] 2· L 12d ≦L 12e ≦6 ·L 12d
[0065] where L 12d is the length of the circular segment of a cross section of the concave-type falling sloped surface 12 d′ ; and
[0066] L 12e is the length of the line segment of a cross section of the straight-type falling sloped surface 12 e.
[0067] Also, since the minimum height of the concave-type falling sloped surface 12 d ′ is about 1 μm to exhibit the suppressing effect of the wet-out phenomenon, the pitch P of the prisms 12 PB is
[0000] 15 μm≦P≦250 μm
[0068] In the above-described second embodiment, since the straight-type falling sloped surface 12 e is the same as that of the first embodiment, the light distributing control effect is the same as that of the first embodiment. However, since the slope angle β1′ of the concave-type falling sloped surface 12 d ′ is smaller than the slope angle β1 of the straight-type falling sloped surface 12 d of the first embodiment to form a sharper edge by the rising sloped surface 12 c and the falling sloped surface 12 d ′, the contact area between the concave-type falling sloped surface 12 d ′ and the flexible reflective sheet 4 is further decreased as illustrated in FIG. 10 to further improve the suppressing effect of the wet-out phenomenon.
[0069] In FIG. 11 , which is a cross-sectional view illustrating a side-edge type surface-emission optical apparatus including a third embodiment of the light guide plate according to the presently disclosed subject matter, the light guide plate 1 A of FIG. 1 is replaced by a light guide plate IC whose triangular prism sequences 12 C are different from the triangular prism sequences I 2 A of FIG. 1 .
[0070] In FIG. 12 , which is a partly-enlarged cross-sectional view of the light guide plate IC of FIG. 11 , the straight-type falling sloped surface 12 d of FIG. 2 is replaced by a concave-type falling sloped surface 12 d ″. Also, the straight-type falling sloped surface 12 d of FIG. 2 is replaced by a concave-type falling sloped surface 12 e ″. Cross sections of the concave-type falling sloped surfaces 12 d ″ and 12 e ″ are curved. In this case, the radius of curvature of the concave-type falling sloped surface 12 d ″ is smaller than that of the concave-type falling sloped surface 12 e ″, so that the concave-type falling sloped surface 12 d ″ is more sloped than the concave-type falling sloped surface 12 e ″. Thus, a sharper edge is formed by the rising sloped surface 12 c and the concave-type falling sloped surface 12 d″.
[0071] In FIG. 12 , in order to suppress the wet-out phenomenon, the slope angle β1″ of a line segment between the ends of the concave-type falling sloped surface 12 d ″ satisfies the following formula (1″) in the same way as the formula (1):
[0000] 3°<β1″<8° (1″)
[0072] On the other hand, in order to enhance the light distributing control efficiency, the slope angle β2 of a line segment between the ends of the concave-type falling sloped surface 12 e ″ satisfies the following formula (2″) in the same way as the formula (2):
[0000] 0.5°<β2<3° (2′)
[0073] Further, the following formula (3″) in the same way as the formula (3) is satisfied:
[0000] 2 ·S 12d ″≦S 12e ″≦6 ·S 12 ″ (3′)
[0074] where S 12d ″ is the area of the concave-type falling sloped surface 12 d ″; and
[0075] S 12e ″ is the area of the concave-type falling sloped surface 12 e″.
[0076] The formula (3″) can be modified to the following formula:
[0000] 2 ·L 12d ″≦L 12e ″≦6 ·L 12 ″
[0077] where L 12d ″ is the length of the circular segment between the ends of the concave-type falling sloped surface 12 d ″; and
[0078] L 12e ″ is the length of the circular segment between the ends of the concave-type falling sloped surface 12 e″.
[0079] Further, a distance D between a center of the concave-type falling sloped surface 12 d ″ and a center of the line segment of the concave-type falling sloped surface 12 d ″ satisfies the following:
[0000] 3/1000· L 12d ″≦D≦ 2/100 ·L 12d ″
[0080] Still further, since the minimum height of the concave-type falling sloped surface 12 d ″ is about 1 μm to exhibit the suppressing effect of the wet-out phenomenon, the pitch P of the prisms PC is
[0000] 15 μm≦P≦250 μm
[0081] In the above-described third embodiment, since the concave-type falling sloped surface 12 e is the same as that of the first embodiment, the light distributing control effect is the same as that of the first embodiment. However, since the angle between the rising sloped surface 12 c and the concave-type falling sloped surface 12 d ″ becomes smaller, the contact area between the concave-type falling sloped surface 12 d ″ and the flexible reflective sheet 4 is further decreased as illustrated in FIG. 13 to further improve the suppressing effect of the wet-out phenomenon.
[0082] In FIG. 14 , which illustrates a modification of the light guide plate 1 C of FIG. 12 , the concave-type falling sloped surfaces 12 d ″ and 12 e ″ are formed by a single concave-type falling sloped surface 12 de whose concaved cross section has one radius of curvature. In this case, the farther from the light source 2 a location of the concave-type falling sloped surface 12 de , the larger of the slope of the concave-type falling sloped surface 12 de . As a result, the contact area between the concave-type falling sloped surface 12 de and the flexible reflective sheet 4 is decreased to further improve the suppressing effect of the wet-out phenomenon while maintaining the light distributing control effect due to the small slope of a part of the concave-type falling sloped surface Sde.
[0083] It will be apparent to those skilled in the art that various modifications and variations can be made in the presently disclosed subject matter without departing from the spirit or scope of the presently disclosed subject matter. Thus, it is intended that the presently disclosed subject matter covers the modifications and variations of the presently disclosed subject matter provided they come within the scope of the appended claims and their equivalents. All related or prior art references described above and in the Background portion of the present specification are hereby incorporated in their entirety by reference.
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In a light guide plate having a light incident surface, a light distributing control surface perpendicular to the light incident surface and a light emitting surface opposing the light distributing control surface, a flat mirror-finish portion is provided on a first area of the light distributing control surface, and a prism sequence is provided on a second area of the light distributing control surface where the flat mirror-finish portion is not provided. The prism sequence is protruded with respect to the flat mirror-finish portion. Each prism of the prism sequence has a rising sloped surface opposing the light incident surface, a first falling sloped surface connected to the rising sloped surface, and a second falling sloped surface connected to the first falling sloped surface, A slope of the first falling sloped surface is larger than a slope of the second falling sloped surface.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a National Phase Application of PCT International Application No. PCT/CN2011/079393, International Filing Date Sep. 6, 2011, claiming priority of Chinese Patent Application No. 201010535957.8, filed Nov. 8, 2010, which is hereby incorporated by reference.
FIELD OF THE INVENTION
The disclosure relates to the field of wireless communication technology, and in particular relates to a method and device for configuring cell parameters of a Relay Node (abbreviated as RN).
BACKGROUND OF THE INVENTION
In order to satisfy the increasing requirements of the large bandwidth high-speed mobile access, the Third Generation Partnership Projects (abbreviated as 3GPP) put forward a Long-Term Evolution advance (abbreviated as LTE-Advanced) standard. The LTE-Advanced reserves a core of a Long-Term Evolution (abbreviated as LTE) for the evolution of the LTE, and adopts a series of techniques to expand the frequency domain and the space domain based on the above, so as to realize the purpose of improving the utilization ratio of the spectrum, and increasing the system capacity and the like.
The Wireless Relay technique, namely, one of the LTE-Advanced techniques, aims at expanding the cell coverage area, reducing the blind angle (or dead angle) area in communication, balancing the load, transferring the service in the hotspot area, and saving the transmitting power of the User Equipment (abbreviated as UE). As shown in FIG. 1 , the RN provides the functions and services similar with a normal eNB for the UE which is accessed to a cell of the RN, and then accesses an eNB which serves for the RN through a wireless interface in the similar mode of a normal UE; the eNB which serves for the RN is called as a Donor eNB (abbreviated as DeNB).
According to whether the RN has its own independent cells, or is taken as a part of a cell under the DeNB, a Type1 Relay and a Type2 Relay are respectively defined. The Type1 Relay refers that the RN can establish its own independent cells which have their own Physical Cell ID (abbreviated as PCI). The RN works as an eNB in its own cells, for example, transmitting reference signals, scheduling the UE, and the like. The Type2 Relay does not have its own independent cells and PCI, and is only used for assisting the DeNB to transmit data. Besides the Type1 Relay, a “Type1a” Relay and a “Type1 b” Relay are also defined in the standard, and are similar with the Type1 Relay in a cell establishment aspect; both the “Type1 a” Relay and the “Type1b Relay” have their own independent cells, and can independently receive and transmit control signals and perform the scheduling.
In view of the structure, the RN and the DeNB establish a unique S 1 connection on the control plane, and the DeNB is taken as a unique Mobility Management Entity (abbreviated as MME), all the S 1 signaling related to the UE will be transmitted to the DeNB through the S 1 connection, the DeNB transmits the S 1 signaling to a real MME destination on the S 1 connection established by the DeNB and the MME. Similarly, the RN also only establishes a unique X 2 connection with the DeNB, the X 2 signaling between the RN and other eNBs must be forwarded through the DeNB.
It should be noted that, an Operation and Maintenance (abbreviated as OAM) of the RN cannot communicate with the OAM of the DeNB (for example, the two belong to different operators), thus, the cell parameters allocated by the OAM of the RN, such as an Evolved Universal Terrestrial Radio Access Network (E-UTRAN) Cell Global Identifier (abbreviated as ECGI), may conflict with the ECGI of the cell managed by the DeNB, namely, the uniqueness of the ECGI is lost. So, the cell parameters of the cell managed by the RN are allocated by the DeNB, but not by the OAM of the RN. Thereby, the DeNB needs to know the number of the cells managed by the RN before allocating the cell parameters for the RN.
SUMMARY OF THE INVENTION
For that reason, one main purpose of the disclosure is to provide a method and device for configuring cell parameters of a RN, for solving the technical problem that the DeNB cannot reasonably configure the cell parameters since the DeNB does not know the cell amount of the RN.
In order to achieve the purpose, the technical solution of the disclosure is realized below.
a method for configuring cell parameters of an RN, comprising:sending, by a RN, a control signaling which carries a cell amount of one or more serving cells of the RN to a Donor eNB, DeNB; configuring, by the DeNB, cell parameters of the one or more serving cells for the RN according to the cell amount contained in the control signaling.
Preferably, the cell parameters of the one or more serving cells configured for the RN by the DeNB comprise an ECGI and a PCI.
Preferably, the control signaling comprises at least one of the following: a RRC signaling, an S 1 signaling and an X 2 signalling.
The RRC signaling comprises at least one of the following: a RRC Connection Setup Request message, a RRC Connection Setup Complete message, a RRC Connection Reestablishment Request message, a RRC Connection Reestablishment Complete message and a RRC Connection Reconfiguration Complete message; the S 1 signaling includes comprises at least one of the following: an S 1 Setup Request message and an eNB Configuration Update message; the X 2 signalling is an eNB Configuration Update message.
Preferably, sending, by the RN, the control signaling which carries the cell amount of the one or more serving cells of the RN to the DeNB comprises: before the RN establishes a RRC connection, or re-establishes a RRC connection, or performs a RRC connection reconfiguration, or establishes an S 1 connection with the DeNB, sending by the RN the control signaling which carries the cell amount of the one or more serving cells of the RN to the DeNB; and when the RN has a RRC connection, or an S 1 connection, or an X 2 connection with the DeNB, and the cell amount of the one or more serving cells of the RN is increased, sending, by the RN, the control signaling which carries the cell amount of the one or more serving cells of the RN to the DeNB.
According to the method of the disclosure, the disclosure also provides a device for configuring cell parameters of a RN, comprising a RN and a DeNB, wherein, the RN is further configured to send a control signaling which carries a cell amount of one or more serving cells of the RN to the DeNB;the DeNB is further configured to configure cell parameters of the one or more serving cells for the RN according to the cell amount contained in the control signaling.
Preferably, before the RN establishes a RRC connection, or re-establishes a RRC connection, or performs a RRC connection reconfiguration, or establishes an S 1 connection with the DeNB, the RN is configured to send the control signaling which carries the cell amount of the one or more serving cells of the RN to the DeNB; and when the RN has a RRC connection, or an S 1 connection, or an X 2 connection with the DeNB, and the cell amount of the one or more serving cells of the RN is increased, the RN is further configured to send the control signaling which carries the cell amount of the one or more serving cells of the RN to the DeNB.
In the disclosure, the RN sends the cell amount of the cell which are managed by the RN to the DeNB through the control signaling, so as to make the DeNB more reasonably configure the cell parameters of the RN. The disclosure solves the problem that the DeNB cannot reasonably distribute resources according to the cell number of the RN, and avoids resources conflicts, wherein the resources contain the ECGI, PCI and the like.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows a diagram of a network structure using a Wireless Relay technique;
FIG. 2 shows a flow chart of a preferred embodiment 1 according to the disclosure;
FIG. 3 shows a flow chart of a preferred embodiment 2 according to the disclosure;
FIG. 4 shows a flow chart of a preferred embodiment 3 according to the disclosure;
FIG. 5 shows a flow chart of a preferred embodiment 4 according to the disclosure;
FIG. 6 shows a flow chart of a preferred embodiment 5 according to the disclosure; and
FIG. 7 shows a flow chart of a preferred embodiment 6 according to the disclosure.
DETAILED DESCRIPTION OF THE EMBODIMENTS
In order to make the purpose, the technical proposal and the advantage of the disclosure more clear, the disclosure is further described in details with reference to the embodiments and drawings below.
Before a DeNB distributes cell parameters of a serving cell of a RN for the RN, the RN needs to send a control signaling which carries a cell amount of one or more serving cell(s) of the RN to the DeNB; the DeNB configures the cell parameters of the RN according to the cell amount contained in the signaling.
The control signaling includes at least one of the following: a RRC signaling, an S 1 signaling and an X 2 signaling.
The RRC signaling includes at least one of the following: a RRC Connection Setup Request message (RRCConnectionRequest), a RRC Connection Setup Complete message (RRCConnectionSetupComplete), a RRC Connection Reestablishment Request message (RRCConnectionReestablishmentRequest), a RRC Connection Reestablishment Complete message (RRCConnectionReestablishmentComplete) and a RRC Connection Reconfiguration Complete message (RRCConnectionReconfigurationComplete).
The S 1 signaling includes at least one of the following: an S 1 Setup Request message (S 1 SETUP REQUEST) and an eNB Configuration Update message (eNB CONFIGURATION UPDATE).
The X 2 signaling includes the eNB Configuration Update message.
The step of configuring the cell parameters of the RN by the DeNB includes at least one of the following: configuring or reconfiguring the cell parameters, such as ECGI and PCI, of the servicing cell(s) of the RN for the RN by the DeNB.
The disclosure is further described in details with reference to the embodiments and drawings below.
Embodiment 1
If the RN has acquired the cell amount of the serving cell(s) of the RN (the cell amount can be preconfigured, or can be allocated by the OAM of the RN) before the RN establishes or re-establishes the RRC connection with the DeNB, the RN can send a RRC message which contains the cell amount of the serving cell(s) of the RN to the DeNB during the process of establishing or re-establishing the RRC connection, and thus the cell amount of one or more cell(s) managed by the RN is reported to the DeNB, so as to make the DeNB more reasonably configure the cell parameters of the RN.
The steps are as shown in FIG. 2 :
Step 201 : during the process of establishing or re-establishing the RRC connection between the RN and the DeNB, the RN reports the cell amount of the cell(s) managed by the RN by sending a RRC message which contains the cell amount of the serving cell(s) of the RN to the DeNB.
The RRC message can be the RRCConnectionRequest message, the RRCConnectionSetupComplete message, the RRCConnectionReestablishmentRequest message, and the RRCConnectionReestablishmentComplete message.
Step 202 : after the DeNB successfully receives the RRC message which carries the cell amount, the DeNB reasonably configures the ECGI and the PCI for the serving cell(s) of the RN according to the cell amount. If current environment and the available resources owned by the DeNB allow the RN to establish cells as many as the RN can support, the DeNB allocates cell parameters, which correspond to the cell amount, for the RN; otherwise, the allocated cell parameters may be smaller than the cell amount.
The message replied to the RN from the DeNB can be a RRC Connection Setup (RRCConnectionSetup) message, a RRC Connection Reestablishment (RRCConnectionReestablishment) message, or a RRC Connection RN Reconfiguration (RRCConnectionRNReconfiguration) message.
Embodiment 2
If the RN has acquired the cell amount of the serving cell(s) of the RN (the cell amount can be preconfigured, or can be allocated by the OAM of the RN) before the RN performs the RRC connection reconfiguration with the DeNB, the RN also can send an RRC message which contains the cell amount of the serving cell of the RN to the DeNB during the process of the RRC connection reconfiguration, and thus the cell amount of the cell(s) managed by the RN is reported to the DeNB, so as to make the DeNB more reasonably configure the cell parameters of the RN.
The steps are as shown in FIG. 3 :
Step 301 : during the process of the RRC connection reconfiguration between the RN and the DeNB, the RN reports the cell amount of the cell(s) managed by the RN by sending a RRC message which contains the cell amount of the serving cell(s) of the RN to the DeNB.
The RRC message can be the RRCConnectionReconfigurationComplete message.
Step 302 : after the DeNB successfully receives the RRC message which carries the cell amount, the DeNB reasonably configures the ECGI and the PCI for the serving cell(s) of the RN according to the cell amount. If current environment and available resources owned by the DeNB allows the RN to establish cells as many as the RN can support, the DeNB allocates the cell parameters, which correspond to the cell amount, for the RN; otherwise, the allocated cell parameters may be smaller than the cell amount. The message replied to the RN from the DeNB can be a RRC Connection RN Reconfiguration (RRCConnectionRNReconfiguration) message.
Embodiment 3
If an RRC connection has existed between the RN and the DeNB, and the cell amount of the serving cell(s) is increased, then the RN can send a RRC message which carries the cell amount of the serving cell(s) to the DeNB, and thus the cell amount of the cell(s) managed by the RN is reported to the DeNB, so as to make the DeNB more reasonably configure the cell parameters of the RN.
The steps are as shown in FIG. 4 :
Step 401 : after the cell amount of the serving cell(s) of the RN is changed, the RN can send a RRC message which carries the cell amount of the serving cell(s) of the RN to the DeNB to report the cell amount of the cell(s) currently managed by the RN, wherein this amount can be the number of added cell(s), and also can be updated complete number.
Step 402 : after the DeNB successfully receives the RRC message which carries the cell amount, the DeNB reasonably configures the ECGI and the PCI for the serving cell(s) of the RN according to the cell amount. If current environment and available resources owned by the DeNB allows the RN to establish cells as many as the RN can support, the DeNB allocates the cell parameters, which correspond to the cell number, for the RN; otherwise, the allocated cell parameters may be smaller than the cell amount. The message replied to the RN from the DeNB can be a RRC Connection RN Reconfiguration (RRCConnectionRNReconfiguration) message.
Embodiment 4
If the RN has acquired the cell amount of the serving cell(s) of the RN (the cell amount can be preconfigured, or can be allocated by the OAM of the RN) before the RN establishes an S 1 connection with the DeNB, the RN can send an S 1 message which contains the cell amount of the serving cell(s) of the RN to the DeNB during the process of establishing the S 1 connection, and thus the cell amount of the cell(s) managed by the RN is reported to the DeNB, so as to make the DeNB more reasonably configure the cell parameters of the RN.
The steps are as shown in FIG. 5 :
Step 501 : during the process of establishing the S 1 connection between the RN and the DeNB, the RN reports the cell amount of the cell(s) managed by the RN by sending an S 1 message which contains the cell amount of the serving cell(s) of the RN to the DeNB.
The S 1 message can be an S 1 Setup Request (S 1 SetupRequest) message.
Step 502 : after the DeNB successfully receives the S 1 message which carries the cell amount, the DeNB reasonably configures the ECGI and the PCI for the serving cell(s) of the RN according to the cell amount. If current environment and available resources owned by the DeNB allows the RN to establish cells as many as the RN can support, the DeNB allocates the cell parameters, which correspond to the cell amount, for the RN; otherwise, the allocated cell parameters may be smaller than the cell amount. The message replied to the RN from the DeNB can be an S 1 Setup Response (S 1 SetupResponse) message or a RRC Connection RN Reconfiguration (RRCConnectionRNReconfiguration) message.
Embodiment 5
If an S 1 connection has existed between the RN and the DeNB, and the cell amount of the serving cell(s) of the RN is increased, then the RN can send an S 1 message which carries the cell amount of the serving cell(s) to the DeNB, and thus the cell amount of the cell(s) managed by the RN is reported to the DeNB, so as to make the DeNB more reasonably configure the cell parameters of the RN.
The steps are as shown in FIG. 6 :
Step 601 : after the cell amount of the service cell(s) of the RN is changed, the RN can send an S 1 message which carries the cell amount of the serving cell(s) of the RN to the DeNB to report the cell amount of the cell(s) currently managed by the RN, wherein this amount can be the number of added cell(s), and also can be a updated complete number.
The S 1 message can be an eNB Configuration Update (eNB CONFIGURATION UPDATE) message.
Step 602 : after the DeNB successfully receives the S 1 message which carries the cell amount, the DeNB reasonably configures the ECGI and the PCI for the serving cell(s) of the RN according to the cell amount. If current environment and available resources owned by the DeNB allows the RN to establish cells as many as the RN can support, the DeNB allocates the cell parameters, which correspond to the cell amount, for the RN; otherwise, the allocated cell parameters may be smaller than the cell amount.
The message replied to the RN from the DeNB can be an eNB Configuration Update Acknowledge (eNB CONFIGURATION UPDATE ACKNOWLEDGE) message or a RRC Connection RN Reconfiguration (RRCConnectionRNReconfiguration) message.
Embodiment 6
If an X 2 connection has existed between the RN and the DeNB, and the cell amount of the serving cell(s) is increased, then the RN can send an X 2 message which carries the cell amount of the serving cell(s) to the DeNB, and thus the cell amount of the cells managed by the RN is reported to the DeNB, so as to make the DeNB more reasonably configure the cell parameters of the RN.
The steps are as shown in FIG. 7 :
Step 701 : after the cell amount of the service cell(s) of the RN is changed, the RN can send an X 2 message which carries the cell amount of the serving cell(s) of the RN to the DeNB to report the cell amount of the cell(s) currently managed by the RN, wherein this amount can be the number of added cell(s), and also can be updated complete number.
The X 2 message can be an eNB Configuration Update (eNB CONFIGURATION UPDATE) message.
Step 702 : after the DeNB successfully receives the X 2 message which carries the cell amount, the DeNB reasonably configures the ECGI and the PCI for the serving cell(s) of the RN according to the cell number. If current environment and available resources owned by the DeNB allows the RN to establish cells as many as the RN can support, the DeNB allocates the cell parameters, which correspond to the cell amount, for the RN; otherwise, the allocated cell parameters may be smaller than the cell amount.
The message replied to the RN from the DeNB can be an eNB Configuration Update Acknowledge (eNB CONFIGURATION UPDATE ACKNOWLEDGE) message or a RRC Connection RN Reconfiguration (RRCConnectionRNReconfiguration) message.
Certainly, the disclosure may have various other embodiments; in the case of obeying the spirits and nature of the disclosure, those skilled in the art can make various corresponding changes and deformations according to the disclosure; and all the corresponding changes and deformations shall fall within the protection range of the attached claims of the disclosure.
The above is only the preferred embodiment of the disclosure and not intended to limit the disclosure.
INDUSTRIAL APPLICABILITY
In the disclosure, the RN sends the cell amount of the cell which are managed by the RN to the DeNB through the control signaling, so as to make the DeNB more reasonably configure the cell parameters of the RN cells. The disclosure solves the problem that the DeNB cannot reasonably allocate resources according to the cell number of the RN, and avoids resources such as ECGI, PCI conflicts.
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The disclosure claims a method and a device for configuring cell parameters of a Relay Node (RN), which can solve the technical problem that the cell parameters cannot be reasonably configured as a Donor eNB (DeNB) does not know the cell amount of the RN. In the disclosure, the RN sends the cell amount of cells which are managed by the RN to the DeNB via a control signaling, so as to make the DeNB more reasonably configure the cell parameters of the RN. The disclosure solves the problem that the DeNB cannot reasonably allocate resources according to the cell amount of the RN, and avoids resources conflicts, wherein the resources contain an Evolved Universal Terrestrial Radio Access Network (E-UTRAN) Cell Global Identifier (ECGI), a Physical Cell ID (PCI) and the like.
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BACKGROUND
[0001] An auditory prosthesis can be placed on the skull of a recipient to deliver a stimulus in the form of a vibration to the skull. These types of auditory prosthesis are generally referred to as bone conduction devices. The auditory prosthesis receives sound via a microphone located on a head-mounted processor. The head-mounted processor is secured to the head with a magnet that interacts with a magnet implanted in the head of the recipient. Processed sound signals are delivered as a vibration stimulus from the external portion to a bone anchor via the implanted magnet. The bone anchor vibrates the skull of the recipient at the appropriate frequency to generate a hearing percept. The magnets form a mass that can make tuning of the auditory prosthesis difficult, due to the dampening of vibrations by the mass.
SUMMARY
[0002] Reducing the amount of mass subject to vibrations in an auditory prosthesis has a positive effect on tuning of the device. One way of reducing such mass is to resiliently mount magnets, electronics, and other components within the auditory prosthesis housing. Such resilient mounting reduces the dampening effect that these massive components have on vibrations generated by the prosthesis. When electronic components are suspended, feedback to said components is also reduced, resulting improved performance.
[0003] 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 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.
BRIEF DESCRIPTION OF THE DRAWINGS
[0004] FIG. 1A depicts a partial perspective view of a percutaneous bone conduction device worn on a recipient.
[0005] FIG. 1B is a schematic diagram of a percutaneous bone conduction device.
[0006] FIG. 2 depicts a cross-sectional schematic view of a transcutaneous bone conduction device worn on a recipient.
[0007] FIGS. 3A-3C depict partial cross-sectional schematic views of external portions of transcutaneous bone conduction devices.
[0008] FIG. 4 depicts a partial perspective view of a plate/mass subsystem for use in an external portion of a transcutaneous bone conduction device.
[0009] FIG. 5 depicts a partial cross-sectional schematic view of an external portion of a transcutaneous bone conduction device.
[0010] FIGS. 6A and 6B depict partial cross-sectional schematic views of alternative embodiments of plate/mass subsystems for use in an external portion of transcutaneous bone conduction devices.
[0011] FIG. 7 depicts spring deformation curves for springs utilized in an external portion of a transcutaneous bone conduction device.
DETAILED DESCRIPTION
[0012] The technologies described herein can typically be utilized with transcutaneous bone conduction devices. Such devices utilize one or more magnets disposed in an external portion and/or implanted portion of the bone conduction device. The magnetic field of an external magnet interacts with a magnetic field of a magnet disposed in an implanted portion of the bone conduction device. The technologies described herein are also applicable to percutaneous bone conduction prostheses that utilize an anchor that penetrates the skin of the head. An external portion of the auditory prosthesis is secured to the anchor with, e.g., a snap connection. By utilizing the technologies described herein, the anchor can be manufactured in whole or in part of a magnetic material, and a mating magnetic material can be disposed in the external portion to mate with the anchor, either alone, or also in conjunction with a snap connection. Additionally, the technologies described herein contemplate a single bone conduction device that can be utilized in both percutaneous and transcutaneous applications. Such devices can include a housing containing sound processing components, microphones, and a vibration element. When used in a percutaneous application, the vibration element can be directly connected to the anchor that penetrates the skin. When used in a transcutaneous application, a module can be attached to the vibration element and then held on the skin via, e.g., the magnetic components described above.
[0013] FIG. 1A depicts a partial perspective view of a percutaneous bone conduction device 100 positioned behind outer ear 101 of the recipient and comprises a sound input element 126 to receive sound signals 107 . The sound input element 126 can be a microphone, telecoil or similar. In the present example, sound input element 126 can be located, for example, on or in bone conduction device 100 , or on a cable extending from bone conduction device 100 . Also, bone conduction device 100 comprises a digital sound processor (not shown), a vibrating electromagnetic actuator and/or various other operational components.
[0014] More particularly, sound input device 126 converts received sound signals into electrical signals. These electrical signals are processed by the sound processor. The sound processor generates control signals that cause the actuator to vibrate. In other words, the actuator converts the electrical signals into mechanical force to impart vibrations to skull bone 136 of the recipient.
[0015] Bone conduction device 100 further includes coupling apparatus 140 to attach bone conduction device 100 to the recipient. In the example of FIG. 1A , coupling apparatus 140 is attached to an anchor system (not shown) implanted in the recipient. An exemplary anchor system (also referred to as a fixation system) can include a percutaneous abutment fixed to the recipient's skull bone 136 . The abutment extends from skull bone 136 through muscle 134 , fat 128 and skin 132 so that coupling apparatus 140 can be attached thereto. Such a percutaneous abutment provides an attachment location for coupling apparatus 140 that facilitates efficient transmission of mechanical force.
[0016] It is noted that sound input element 126 can comprise devices other than a microphone, such as, for example, a telecoil, etc. In an exemplary embodiment, sound input element 126 can be located remote from the BTE device 100 and can take the form of a microphone or the like located on a cable or can take the form of a tube extending from the BTE device 100 , etc. Alternatively, sound input element 126 can be subcutaneously implanted in the recipient, or positioned in the recipient's ear canal or positioned within the pinna. Sound input element 126 can also be a component that receives an electronic signal indicative of sound, such as, from an external audio device. For example, sound input element 126 can receive a sound signal in the form of an electrical signal from an MP3 player or a smartphone electronically connected to sound input element 126 .
[0017] The sound processing unit of the BTE device 100 processes the output of the sound input element 126 , which is typically in the form of an electrical signal. The processing unit generates control signals that cause an associated actuator to vibrate. In other words, the actuator converts the electrical signals into mechanical vibrations for delivery to the recipient's skull. These mechanical vibrations are delivered by an external portion of the auditory prosthesis 100 , as described below.
[0018] FIG. 1B is a schematic diagram of a percutaneous bone conduction device 100 . Sound 107 is received by sound input element 152 . In some arrangements, sound input element 152 is a microphone configured to receive sound 107 , and to convert sound 107 into electrical signal 154 . Alternatively, sound 107 is received by sound input element 152 as an electrical signal. As shown in FIG. 1B , electrical signal 154 is output by sound input element 152 to electronics module 156 . Electronics module 156 is configured to convert electrical signal 154 into adjusted electrical signal 158 . As described below in more detail, electronics module 156 can include a sound processor, control electronics, transducer drive components, and a variety of other elements.
[0019] As shown in FIG. 1B , transducer or vibration element 160 receives adjusted electrical signal 158 and generates a mechanical output force in the form of vibrations that is delivered to the skull of the recipient via a coupling apparatus 140 , as described above. The coupling apparatus 140 connects to the anchor system 162 , so as to couple the anchor system 162 to bone conduction device 100 . Delivery of this output force causes motion or vibration of the recipient's skull, thereby activating the hair cells in the recipient's cochlea (not shown) via cochlea fluid motion.
[0020] FIG. 1B also illustrates power module 170 . Power module 170 provides electrical power to one or more components of bone conduction device 100 . For ease of illustration, power module 170 has been shown connected only to user interface module 168 and electronics module 156 . However, it should be appreciated that power module 170 can be used to supply power to any electrically powered circuits/components of bone conduction device 100 .
[0021] User interface module 168 , which is included in bone conduction device 100 , allows the recipient to interact with bone conduction device 100 . For example, user interface module 168 can allow the recipient to adjust the volume, alter the speech processing strategies, power on/off the device, etc. In the example of FIG. 1B , user interface module 168 communicates with electronics module 156 via signal line 164 .
[0022] Bone conduction device 100 can further include external interface module that can be used to connect electronics module 156 to an external device, such as a fitting system. Using external interface module 166 , the external device, can obtain information from the bone conduction device 100 (e.g., the current parameters, data, alarms, etc.) and/or modify the parameters of the bone conduction device 100 used in processing received sounds and/or performing other functions.
[0023] In the example of FIG. 1B , sound input element 152 , electronics module 156 , vibration element 160 , power module 170 , user interface module 168 , and external interface module have been shown as integrated in a single housing, referred to as housing 150 . However, it should be appreciated that in certain examples, one or more of the illustrated components can be housed in separate or different housings. Similarly, it should also be appreciated that in such embodiments, direct connections between the various modules and devices are not necessary and that the components can communicate, for example, via wireless connections.
[0024] FIG. 2 depicts an exemplary embodiment of a transcutaneous bone conduction device 200 that includes an external portion 204 and an implantable portion 206 . The transcutaneous bone conduction device 200 of FIG. 2 is a passive transcutaneous bone conduction device in that a transducer or vibration element 208 is located in the external portion 204 . In general, the external portion 204 can include the control and sound processing components depicted above in FIG. 1B . For clarity however, these components are generally not depicted; instead, structural elements particular to a transcutaneous bone conduction device 200 are shown. Vibration element 208 is located in housing 210 of the external component, and is coupled via a coupling apparatus 211 to the plate 212 , which can be discrete from the housing 210 as depicted, or disposed within the housing 210 . Plate 212 can be in the form of a permanent magnet and/or in another form that generates and/or is reactive to a magnetic field, or otherwise permits the establishment of magnetic attraction between the external portion 204 and the implantable portion 206 sufficient to hold the external portion 204 against the skin of the recipient. In other embodiments, magnets or magnetic materials can be discrete from plate 212 . Magnetic attraction can be further enhanced by utilization of a magnetic implantable plate 216 . In alternative embodiments, multiple magnets in both the external portion 204 and implantable portion 206 can be utilized.
[0025] In an exemplary embodiment, the vibration element 208 is a device that delivers vibration stimulus to the skull of a recipient. In operation, sound input element 126 converts sound into electrical signals. Specifically, the transcutaneous bone conduction device 200 provides these electrical signals to vibration element 208 , or to a sound processor (not shown) that processes the electrical signals, and then provides those processed signals to vibration element 208 . The vibration element 208 converts the electrical signals (processed or unprocessed) into vibrations. Because vibration element 208 is mechanically coupled to plate 212 , the vibrations are transferred from the vibration element 208 to plate 212 via coupling apparatus 211 . Implantable plate assembly 214 is part of the implantable portion 206 , and can be made of a ferromagnetic material that can be in the form of a permanent magnet, that generates and/or is reactive to a magnetic field, or otherwise permits the establishment of a magnetic attraction between the external portion 204 and the implantable portion 206 sufficient to hold the external portion 204 against the skin 132 of the recipient. Accordingly, vibrations produced by the vibration element 208 of the external portion 204 are transferred from plate 212 across the skin 132 to implantable plate 216 of implantable plate assembly 214 . This can be accomplished as a result of mechanical conduction of the vibrations through the skin 132 , resulting from the external portion 204 being in direct contact with the skin 132 and/or from the magnetic field between the two plates 212 , 216 . These vibrations are transferred without a component penetrating the skin 132 , fat 128 , or muscular 134 layers on the head.
[0026] As can be seen, the implantable plate assembly 214 is substantially rigidly attached to bone fixture 220 in this embodiment. Implantable plate assembly 214 includes through hole 220 that is contoured to the outer contours of the bone fixture 218 , in this case, a bone screw that is secured to the bone 136 of the skull. This through hole 220 thus forms a bone fixture interface section that is contoured to the exposed section of the bone fixture 218 . In an exemplary embodiment, the sections are sized and dimensioned such that at least a slip fit or an interference fit exists with respect to the sections. Plate screw 222 is used to secure implantable plate assembly 214 to bone fixture 218 . As can be seen in FIG. 2 , the head of the plate screw 222 is larger than the hole through the implantable plate assembly 214 , and thus the plate screw 222 positively retains the implantable plate assembly 214 to the bone fixture 218 . In certain embodiments, a silicon layer 224 is located between the implantable plate 216 and bone 136 of the skull.
[0027] Notably, the external portion of a bone conduction auditory prosthesis can be utilized in both the percutaneous application of FIGS. 1A and 1B , and the transcutaneous application of FIG. 2 . For example, a bone conduction auditory prosthesis can include a housing containing, e.g., the various modules and elements depicted in FIG. 1B . Those elements include vibration element 160 ( FIG. 1B ), which is equivalent to vibration element 208 ( FIG. 2 ). The vibration element can be connected to a coupling apparatus 140 ( FIG. 1B ) or 211 ( FIG. 2 ). Such a coupling apparatus can be connected to an anchor system 162 ( FIG. 1B ) in a percutaneous bone conduction application. Alternatively, the coupling apparatus can be connected to a plate or other transmission element 212 (FIG. 2 ) to be utilized in a transcutaneous application. This increases manufacturing efficiencies by allowing the same bone conduction device to be used in either configuration.
[0028] FIGS. 3A-3C depict partial cross-sectional schematic views of external portions 300 a - c of transcutaneous bone conduction devices. These depicted embodiments are described generally together followed by a description of each specific embodiment. Each of the depicted embodiments includes a housing 304 a - c that includes a vibration element, sound processing electronics, batteries, and other elements disposed therein. These elements are not depicted in the FIGS. A coupling apparatus 306 a - c extending from the housing 304 a - c is connected to the vibration element. The coupling apparatus 306 a - c can be connected to a bone anchor system (in the case of a percutaneous bone conduction device) or to a transmission element 308 a - c (in the case of a transcutaneous bone conduction device). An underside 318 a - c of the transmission element 308 a - c is adapted to contact the skin of a recipient. A magnet housing 302 a - c contains one or more masses 310 a - c . Either or both of the housing 302 a - c and the masses 310 a - c are connected to the transmission element 308 a - c with one or more resilient elements 312 a - c . Different types of resilient elements 312 a - c , such as coil springs, leaf springs, torsion springs, shape-memory elements, wave springs, and elastomeric elements, can be utilized in the external portions described herein.
[0029] The masses 310 a - c can be any type of material that can be utilized to help secure the external portion 300 a - c to the skin of a patient, proximate an implanted portion of a bone conduction device. As described above, the external portion 300 a - c is held against the skin of a recipient due to magnetic force between elements of the external portion 300 a - c and the implanted portion. Thus, the masses 310 a - c can be a magnetic component, such as a permanent magnet, a soft magnetic material, or other materials capable of transmitting magnetic flux, e.g., iron, nickel, cobalt, and compositions thereof. In general, utilizing permanent magnets on both an external portion 300 a - c and an implanted portion can exhibit the strongest retention forces. However, in other embodiments, the masses 310 a - c can be permanent magnets while a soft magnetic material can be utilized in the implanted portion. In yet another embodiment, the masses 310 a - c can be a soft magnetic material and permanent magnets can be disposed in the implanted portion. Regardless of the type of magnetic component used, the presence of the masses 310 a - c can display undesirable effects on the auditory performance of the auditory prosthesis. In one example, the added weight of the masses 310 a - c can reduce the level of force transmitted through the skin by the transmission element 308 a - c at higher frequencies. Indeed, the heavier the masses 310 a - c , the greater the force reduction. In another example, the masses 310 a - c cause increased feedback. This feedback can be at least partially be caused by the pumping of air by the masses 310 a - c . To remedy this and other problems, resilient elements 312 a - c flexibly connect the housing 302 a - c and/or the masses 310 a - c to the transmission element 308 a - c . By utilizing resilient elements 312 a - c , vibration of the masses 310 a - c is reduced or eliminated while the transmission element delivers vibrational stimulus to the skull of a recipient. In other embodiments, the masses 310 a - c can be incorporated into the vibration element 304 a - c . The external portions 300 a - c are utilized in conjunction with transcutaneous bone conduction devices and are individually described in more detail below.
[0030] Referring to the external portion 300 a of FIG. 3A , specifically, the transmission element 308 a includes a rigid connection element 314 a that connects to the coupling apparatus 306 a . The rigid connection element 314 a passes through an opening 324 a in the magnet housing 302 a , which has a substantially annular shape. The connection can be made with a screw, bolt, press-fit connection, threaded connection, adhesive, and/or other mechanical or chemical connections. In certain embodiments, the coupling apparatus 306 a can be eliminated such that the rigid connection element 314 a can be directly connected to the vibration element 304 a . The rigid connection element 314 a is connected to, or integral with, a plate 316 a that has an external surface 318 a that is adapted to contact a skin surface of a recipient when worn. In embodiments, the masses 310 a are disposed within a magnet housing 302 a and are proximate an internal surface 320 a of the plate. One or more resilient elements 312 a connect the plate 316 a to the magnet housing 302 a . An odd or even number of resilient elements 312 a can be disposed so as to evenly balance the weight of the masses 310 a about an axis A defined by the rigid connection element 314 a.
[0031] FIG. 3B depicts an external portion 300 b having a generally similar configuration to that depicted in FIG. 3A , thus, many of the components are not described further. In this embodiment, the magnet housing 302 b and the masses 310 b contained therein are disposed proximate an internal surface 320 b of a plate 316 b . In this case, however, the magnet housing 302 b is flexibly connected to the rigid connection element 314 b of the transmission plate 316 b with one or more resilient elements 312 b . An odd or even number of resilient elements 312 b can be disposed so as to evenly balance the weight of the masses 310 b about axis A. FIG. 3C depicts another embodiment of an external portion 300 c with components generally similar to that depicted in FIG. 3A , thus, many of the components are not described further. In this embodiment, the transmission element 308 c is the rigid connection element 314 c , which has sufficient surface area so as to deliver a vibration stimulus to the skull of a recipient via the external surface 318 c . Here, as in FIG. 3B , the magnet housing 302 c is flexibly connected to the rigid connection element 314 c with one or more resilient elements 312 a . An odd or even number of resilient elements 312 c can be disposed so as to evenly balance the weight of the masses 310 c about the axis A.
[0032] FIG. 4 depicts a partial perspective view of a plate/mass subsystem 400 for use in an external portion of a transcutaneous bone conduction device such as described herein. As described above, an external portion of a bone conduction device can be utilized for both percutaneous and transcutaneous applications. The plate/mass subsystem 400 depicted in FIG. 4 can be connected to the coupling apparatus of the external portion so as to enable the external portion to be utilized in a transcutaneous application. The plate/mass subsystem 400 includes a mass 402 that, in the depicted embodiment, includes a magnet housing 404 having one or more magnets 406 disposed therein. Other materials, such as those described above, can be used in place of the magnets 406 . Although two magnets 406 are depicted, other numbers of magnets can be utilized, although it is advantageous to position the magnets about the magnet housing 404 so as to balance the forces attendant therewith.
[0033] The mass 402 is connected to a transmission element 408 via a number of resilient members 410 , such that a bottom surface 412 of the mass 402 is spaced apart from a top surface 414 of the transmission element 408 , which in this embodiment is a plate. A rigid connection element 416 such as a shaft is connected to or integral with a central portion of the transmission element 408 . The rigid connection element 416 penetrates a central opening or through-hole 418 defined by both a top surface and a bottom surface of the mass 402 , so as to not contact the mass 402 . Since the mass 402 is connected to the transmission element 408 with resilient members 410 , contact between the connection element 408 and the mass 402 would cause vibrations to be transmitted to the mass 402 , thus defeating one of the purposes of the proposed configuration. The rigid connection element 416 includes an interface 420 for releasably securing the rigid connection element 416 to a coupling apparatus of a vibration element, as described above. The interface 420 can be a shaft, a threaded rod, a screw, a bolt, or other connection structure that allows the plate/mass subsystem 400 to be connected to the vibration element of an external portion of an auditory prosthesis. Once secured, the complete external portion can be placed on the head and used as a transcutaneous bone conduction auditory prosthesis. The magnets 406 magnetically couple with one or more implanted magnets proximate the skull of a recipient.
[0034] FIG. 5 depicts a partial cross-sectional schematic view of another embodiment of an external portion 500 of a transcutaneous bone conduction device. The external portion 500 includes a housing 502 in which is disposed a vibration element 504 . The vibration element 504 is connected directly to a transmission element 508 without, e.g., a coupling apparatus such as described above. Thus, the external portion 500 of FIG. 5 is utilized in a dedicated transcutaneous bone conduction application, unlike certain of the previous embodiments that can be interchanged between transcutaneous and percutaneous applications. In the depicted embodiment, the transmission element 508 includes a shaft 514 connected to or integral with a plate 516 . As in the previous embodiments, the plate 516 has a lower surface 518 adapted to contact the skin of a recipient, as well as an upper surface 520 . Resilient members 512 flexibly connect the upper surface 520 to one or more masses 510 . The external portion 500 also includes a number of additional components 524 required for the functionality of the external portion 500 . These are described generally above and can include a battery, electronics, wireless communication devices, sound input elements such as microphones, and so on. To further reduce feedback, the components 524 can be connected to the masses 510 at interface 526 . In such an embodiment, the housing 502 can be connected to the transmission element 508 such that vibrations generated by the vibration element 504 are dissipated into the housing 502 , while the components 524 are isolated from vibration via the resilient elements 512 . In another embodiment, the components 524 can be connected to the housing 502 at interface 528 . In such an embodiment, the vibration element 504 and/or transmission element 508 can be connected to the housing via a flexible or resilient connection, not shown.
[0035] FIGS. 6A and 6B depict partial cross-sectional schematic views of alternative embodiments of plate/mass subsystems 600 for use in an external portion of transcutaneous bone conduction devices. The plate/mass subsystems 600 of both FIGS. 6A and 6B are described together. Each plate/mass subsystem 600 includes a transmission element 608 having a form factor in the shape of a plate, although other configurations are contemplated. A rigid connection element 616 extends from the transmission element 608 and includes an interface 620 can be a shaft, a threaded rod, a screw, a bolt, or other connection structure that allows the plate/mass subsystem 600 to be connected to the vibration element of an external portion of an auditory prosthesis. Masses 606 can be magnetic components such as described above. In FIG. 6A , the masses 606 include one or more arms 630 that can extend from the mass 606 . The arm 630 provides a point of connection for a resilient element 610 that connects the mass 606 to the transmission element 608 . Similarly the masses 606 of FIG. 6B can define bores 632 therein. One or more resilient elements 610 can be disposed in the bores 632 to resiliently connect the masses 606 to the transmission element 608 . Contrasted with the embodiments described above where the resilient elements are connected to a lower surface of a mass, the configurations depicted in FIGS. 6A and 6B connect the resilient elements 610 proximate an upper portion of the masses 606 . This can also allow for use of smaller masses 606 than might otherwise be utilized in the embodiments where resilient elements are connected to the underside of the mass (for example, as depicted in FIG. 3A ).
[0036] FIG. 7 depicts spring deformation curves for springs utilized in an external portion of a transcutaneous bone conduction device. Again, different types of resilient elements, such as coil springs, leaf springs, torsion springs, shape-memory elements, wave springs, and elastomeric elements, can be utilized in the external portions described herein. FIG. 7 depicts curves for springs with linear characteristics, degressive characteristics, and progressive characteristics, each of which can be utilized in conjunction with the embodiments described herein. The label W depicts work performed in the spring. In certain embodiments, a degressive spring can be desirable, as it will minimize the required length of compression from the static magnetic attraction force (e.g., the force generated by attraction to an implanted portion of an auditory prosthesis and an associated magnet). Such a degressive spring is non-linear with respect to force and length and still allows for a low spring constant (e.g., a weak spring) in the working range, which allows for a low decoupling frequency.
[0037] This disclosure described some embodiments of the present technology with reference to the accompanying drawings, in which only some of the possible embodiments were shown. Other aspects, however, can be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments were provided so that this disclosure was thorough and complete and fully conveyed the scope of the possible embodiments to those skilled in the art.
[0038] Although specific embodiments were described herein, the scope of the technology is not limited to those specific embodiments. One skilled in the art will recognize other embodiments or improvements that are within the scope of the present technology. Therefore, the specific structure, acts, or media are disclosed only as illustrative embodiments. The scope of the technology is defined by the following claims and any equivalents therein.
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An external portion of an auditory prosthesis includes magnets, electronics, and other components. In bone conduction auditory prostheses, reducing the amount of mass subject to vibrations in an auditory prosthesis has a positive effect on tuning of the device. One way of reducing such mass is to resiliently more massive components within the auditory prosthesis housing. Such resilient mounting reduces the dampening effect that these massive components have on vibrations generated by the prosthesis. When electronic components are suspended, feedback to said components is also reduced, resulting improved performance.
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BACKGROUND OF THE INVENTION
The present invention pertains to compounds having at least one olefinic unsaturated group and at least one glycidyl ether group.
Unsaturated epoxy compounds such as glycidyl methacrylate have been employed in halogenated polymers as acid scavengers however, because of the ester groups, they are hydrolytically unstable.
It has now been discovered that compounds having a terminal acetylenic group react with an epihalohydrin by addition to the acetylenic group to form an ethylenic halohydrin ether which can be dehydrohalogenated by conventional means to form an ethylenically unsaturated glycidyl ether. Glycidyl ethers are much more hydrolytically stable.
SUMMARY OF THE INVENTION
One aspect of the present invention pertains to compounds represented by the formula ##STR1## wherein each R is independently hydrogen, a hydrocarbyl group having from about 1 to about 12, preferably from 1 to about 6 carbon atoms, a glycidyl ether group or a glycidyl ether substituted hydrocarbyl group having from 4 to about 8, preferably from 4 to about 6 carbon atoms or two of such R groups can be combined to form a cyclic structure and wherein R' is hydrogen or an alkyl group having from 1 to about 3 carbon atoms.
The present invention also pertains to cured compositions of the aforementioned compounds having two or more glycidyl ether groups.
DETAILED DESCRIPTION OF THE INVENTION
Suitable materials having at least one terminal acetylenic group which can be employed herein include, for example, those represented by the formula ##STR2## wherein each R is independently hydrogen, a hydrocarbyl group having from 1 to about 12, preferably from about 1 to about 6 carbon atoms, a hydroxyl substituted hydrocarbyl group having from about 1 to about 12, preferably from about 1 to about 6 carbon atoms or two of such R groups can be combined to form a cyclic structure.
Particularly suitable such acetylenic compounds include, for example, 3,5-dimethyl-1-hexyne-3-ol, methyl acetylene, butylene acetylene, acetylene, mixtures thereof and the like.
Suitable epihalohydrins which can be employed herein include, for example, those represented by the formula ##STR3## wherein R' is hydrogen or an alkyl group having from 1 to about 3 carbon atoms and X is a halogen.
Particularly suitable epihalohydrins include, for example, epichlorohydrin, epibromohydrin, epiiodohydrin, methylepichlorohydrin, methylepibromohydrin, methylepiiodohydrin, mixtures thereof and the like.
The reaction between the acetylenic compound and the epihalohydrin is usually conducted in the presence of a phase transfer catalyst such as, for example, quaternary ammonium compounds, quaternary phosphonium compounds, sulfonium compounds, crown ethers, mixtures thereof and the like.
Particularly suitable quaternary ammonium compounds include, for example, benzyl trimethyl ammonium chloride, benzyl trimethyl ammonium bromide, tetrabutyl ammonium chloride, mixtures thereof and the like.
Suitable quaternary phosphonium compounds include those disclosed in U.S. Pat. No. 3,948,855 and U.S. Pat. No. 3,477,990 which are incorporated herein by reference.
Particularly suitable quaternary phosphonium compounds include, for example, methyl tributyl phosphonium dimethyl phosphate, benzyl triphenyl phosphonium chloride, methyl tri-n-butyl phosphonium bicarbonate, mixtures thereof and the like.
Suitable sulfonium compounds include, for example, tributyl sulfonium iodide, dimethyl isobutyl sulfonium chloride, n-amyl dimethyl sulfonium hydroxide, mixtures thereof and the like.
Suitable crown ethers include, for example, 18-Crown-6, 12-Crown-4, 15-Crown-5, mixtures thereof and the like.
These ethylenically unsaturated compounds can be polymerized with themselves or copolymerized with one or more materials containing at least one polymerizable ethylenically unsaturated group.
Suitable such materials containing at least one polymerizable unsaturated group include, for example, styrene, vinyl toluene, ortho-, meta- and parahalostyrenes, vinyl naphthalene, the various alpha-substituted styrenes, as well as the various di-, tri- and tetrahalo styrenes and acrylic, methacrylic and crotonic acid esters which include both the saturated alcohol esters and the hydroxyalkyl esters, mixtures thereof and the like.
The polymerization is conducted in the presence of free radical catalysts such as organic peroxides such as, for example, benzoyl peroxide, azobisisobutyronitrile, cumene hydroperoxide, mixtures thereof and the like.
Also, it may be desirable to include accelerators such as, for example, cobalt naphthenate, mixtures thereof and the like.
The usual epoxy resin curing agents can be employed to prepare cured compositions such as, for example, dicarboxylic acids, and anhydrides thereof, primary, secondary and tertiary amines, mixtures thereof and the like.
The epoxy resins can be employed in the preparation of structural or electrical laminates or composites, coatings, castings, potting, encapsulation, mixtures thereof and the like.
The following examples are illustrative of the present invention, but are not to be construed as to limiting the scope thereof.
EXAMPLE
Preparation of the diglycidyl ether of 3,5-dimethyl-1-hexyne-3-ol
63 g (0.5 mole) of 3,5-dimethyl-1-hexyne-3-ol was dissolved in 1000 ml epichlorohydrin. Tetrabutylammonium chloride (20 ml of 50% aqueous solution) was added. The mixture was stirred at 550 rpm and heated to 55° C., 200 ml of 50% aqueous sodium hydroxide (3.8 moles) was added and the reaction temperature maintained at 60° C. for 20 minutes (1200 s). The reaction mixture was then cooled to 35° C., ice water (200 ml) was then added with gentle mixing. After settling, the bottom aqueous layer was removed through the bottom takeoff valve. A second charge of caustic (200 ml) was then added and the mixture heated and stirred for 15 minutes (900 s) at 60° C. The workup procedure above was repeated and followed with a third and final caustic treatment. After the final caustic treatment, the 50% caustic was diluted with an equal volume of ice water and the mixture stirred for one hour (3600 s) at 30° C. to complete epoxidation of residual chlorohydrins. After the epoxidation step the aqueous layer was removed by the bottom valve and the organic layer washed with a solution of 5% NaH 2 PO 4 to neutralize residual caustic. This was followed by a final wash with an equal volume of deionized water. The epichlorohydrin and volatile by-products were removed by vacuum evaporation in a rotary vacuum evaporator. The product was a mobile liquid. IR analysis indicated the absence of acetylenic triple bonds and the presence of C═C. NMR analysis showed the product to be a compound represented by the structure ##STR4##
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Olefinic epoxy compounds are prepared by reacting a material containing at least one terminal --C═CH group with an epihalohydrin followed by dehydrohalogenation. The materials are useful as halogen scavengers in the preparation of coatings, castings, laminates, composites, and the like.
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FIELD OF THE INVENTION
The invention relates to a radial antifriction bearing according to the features of patent claim 1 which form the preamble, and it can be realized particularly advantageously on single-row grooved antifriction bearings or angular contact antifriction bearings.
BACKGROUND OF THE INVENTION
It is generally known to a person skilled in the art of antifriction bearing technology that single-row grooved ball bearings represent a classic form of rigid radial antifriction bearings which cannot be dismantled, have deep grooves configured with a radius a little larger than the ball radius and are distinguished above all by the fact that their radial and axial loadbearing capability is equally high and that they have the highest speed limits of all bearing types on account of their low friction. In contrast, single-row angular contact ball bearings are a further form of radial antifriction bearings which can or cannot be dismantled, since their raceways are arranged in such a way that the forces which occur are transmitted from one raceway to the other at a defined contact angle obliquely with respect to the radial plane. However, on account of their contact angle, angular contact ball bearings are better suited to absorbing higher axial forces than grooved ball bearings, it being possible for radial forces to be transmitted by single-row angular contact ball bearings only if they are loaded axially at the same time. These single-row grooved ball bearings and angular contact ball bearings have been known for a long time and comprise substantially an outer bearing ring and inner bearing ring and a multiplicity of balls as rolling bodies which are arranged between the bearing rings. Ball raceways which are delimited by one or two shoulders, each of which are machined into the inner side of the outer bearing ring and into the outer side of the inner bearing ring, in which ball raceways the balls roll by way of their running faces and are guided at uniform spacings from one another by a bearing cage.
In grooved ball bearings or angular contact ball bearings of this type, the necessarily different configuration of the raceway radii in comparison with the ball radii has proven disadvantageous, however, to the extent that the bearing balls are only in punctiform contact with their raceway in the inner bearing ring as a result and therefore cause a high surface pressure on the raceway in the region of the contact angle axis, which high surface pressure is responsible for increased wear of said raceway. In addition, high edge stresses occur in the region of the shoulder edge/edges of the raceway as a result of the bearing balls which overlap said shoulder edge/edges in the case of normal osculation but bear against the shoulder edge/edges after the osculation has been used up, as a result of which high edge stresses the wear of the raceway for the bearing balls is increased still further and the service life of grooved ball bearings or angular contact ball bearings of this type is reduced considerably.
One possibility of avoiding the high surface pressure on the raceway of the inner bearing ring in the region of the contact angle axis of the rolling bodies has been disclosed in DE 43 34 195 A1. In the radial antifriction bearings which are disclosed in said document and are configured per se as single-row grooved ball bearing or angular contact ball bearing, however, the rolling bodies are not formed by balls but rather either partially or completely by what are known as spherical disks which are configured with two side faces which are flattened symmetrically from a basic spherical shape and are arranged parallel to one another. The width of these spherical disks between their side faces is configured to be smaller than the spacing between the inner side of the outer bearing ring and the outer side of the inner bearing ring, with the result that, when the bearing is filled, the spherical disks can be inserted into the bearing axially with respect to the bearing through the spacing between the inner ring and the outer ring and can be rotated into the raceway. Since the spherical disks have a constant rotational axis in contrast to conventional bearing balls, the running faces of the spherical disks are configured with the same radius as their raceways in the bearing rings, with the result that the spherical disks are in linear contact with the raceways. As a result of this linear contact, instead of the disadvantageous punctiform contact which occurs in single-row grooved ball bearings or angular contact ball bearings, a situation is achieved where a uniform surface pressure with a low stress level occurs between the spherical disks and the raceways.
However, it has been shown in operation and under load that, in grooved antifriction bearings or angular contact antifriction bearings of this type with spherical disks as rolling bodies, as a result of the fact that the raceways in the bearing rings are of wider configuration than the spherical disks, the spherical disks cause high edge stresses at the outer edge regions of the raceway in the inner bearing ring by way of their edge parts which adjoin their straight side faces, which high edge stresses are still responsible for increased wear of this raceway and therefore reduce the service life of grooved antifriction bearings or angular contact antifriction bearings of this type.
OBJECT OF THE INVENTION
Proceeding from the cited disadvantages of the solutions of the known prior art, the invention is therefore based on the object of designing a radial antifriction bearing, particularly a single-row grooved antifriction bearing or angular contact antifriction bearing with spherical disks as rolling bodies, with which both high surface pressure on the raceway which occurs in the region of the contact angle axis and a high edge stress which occurs at the outer edge regions of the raceway in the inner bearing ring are avoided effectively and the service life of the grooved antifriction bearing or angular contact antifriction bearing is therefore increased.
DESCRIPTION OF THE INVENTION
According to the invention, this object is achieved in a radial antifriction bearing in such a way that at least the raceway in the inner bearing ring, in each case at its outer edge regions, and/or the running faces of the spherical disks, in each case at their edge parts which adjoin the side faces, merges/merge into a logarithmically falling profile.
The invention is therefore based on the realization that, as a result of a logarithmically falling profile in the regions of the edge stresses which have occurred up to then, it is possible to effectively avoid edge stresses of this type and at the same time to retain the linear contact of the spherical disks with their raceways which is advantageous for a uniformly low surface stress. At the same time it can be advantageous to optionally arrange the logarithmic profile either at the outer edge regions of the raceway in the inner bearing ring or at those edge parts of the running faces of the spherical disks which adjoin the side faces or both at the edge regions of the raceway and at the running faces of the spherical disks.
Preferred embodiments and advantageous developments of the single-row radial antifriction bearing which is configured according to the invention are described in the subclaims.
Accordingly, there is provision that in the radial antifriction bearing, which is configured according to the invention, for the surface area portion of those outer edge regions of the raceway of the inner bearing ring which are configured with a logarithmically falling profile and/or of the edge parts of the running faces of the spherical disks to be each from approximately 10% to 40% of the surface area of the raceway of the inner bearing ring or of the running face of a spherical disk. As a result, the portion which is configured with the same radius of the running faces of the spherical disks and of the raceway face of the inner bearing ring is between 60% and 90%, as a result of which 100% osculation and linear contact is ensured between the spherical disks and the raceways.
Finally, as a further embodiment of the radial antifriction bearing, which is configured according to the invention, it is also proposed that the radius of the logarithmic profile at the outer edge regions of the raceway of the inner bearing ring is preferably greater than the radius of the running faces of the spherical disks, and that the radius of the logarithmic profile at the edge parts of the running faces of the spherical disks is preferably smaller than the radius of the running faces of the spherical disks. The center points of all the radii are arranged above one another, preferably on the contact angle axis of the radial antifriction bearing, with the result that uniform large wedge-shaped annular gaps are produced on both sides between the edge parts of the running faces of the spherical disks and the edge regions of the raceway of the inner bearing ring. However, it is also possible to arrange the center points of the radii for the logarithmic profile at the spherical disks and/or at their raceway in the inner bearing ring on both sides next to the contact angle axis of the radial nonfriction bearing, with the particular advantage that the radii merge tangentially into one another as a result.
In comparison with the radial antifriction bearings which are known from the prior art, the radial antifriction bearing which is configured according to the invention therefore has the advantage that, as a result of the arrangement of logarithmically falling profiles in the regions of the edge stresses which have occurred up to then, it has neither a high surface pressure on the raceway which occurs in the region of the contact angle axis nor a high edge stress which occurs at the outer edge regions of the raceway in the inner bearing ring, and is therefore distinguished by a high service life.
BRIEF DESCRIPTION OF THE DRAWINGS
One preferred embodiment of the radial antifriction bearing which is configured according to the invention will be explained in greater detail in the following text with reference to the appended drawings, in which:
FIG. 1 shows a cross section through a radial antifriction bearing which is configured according to the invention in the form of a grooved antifriction bearing;
FIG. 2 shows an enlarged illustration of the detail X of the radial antifriction bearing which is configured according to the invention in accordance with FIG. 1 ; and
FIG. 3 shows an enlarged illustration of the contact region between the rolling bodies and the raceway of the inner bearing ring of the radial antifriction bearing which is configured according to the invention.
DETAILED DESCRIPTION OF THE DRAWINGS
A radial antifriction bearing 1 which is configured as a grooved antifriction bearing is clearly apparent from FIG. 1 , which, in a similar manner to known grooved ball bearings, comprises substantially an outer bearing ring 2 and an inner bearing ring 3 and a multiplicity of rolling bodies 4 which are arranged between the bearing rings 2 , 3 and are kept at uniform spacings from one another in the circumferential direction by a bearing cage 5 . The detail X according to FIG. 1 which is shown enlarged in FIG. 2 shows that the rolling bodies 4 are configured as spherical disks 11 having two side faces 12 , 13 each which are flattened symmetrically from a basic spherical shape and are arranged parallel to one another and roll by way of their running faces 6 in two raceways 7 , 8 which are delimited in each case by two shoulders and are machined into the inner side 9 of the outer bearing ring 2 and into the outer side 10 of the inner bearing ring 3 .
Furthermore, it becomes clear from FIG. 3 that, in order to avoid a high edge stress which occurs at the outer edge regions 14 , 15 of the raceway 8 in the inner bearing ring 3 , both the raceway 8 in the inner bearing ring 3 , at its outer edge regions 14 , 15 , and the running faces 6 of the spherical disks 11 , at their edge parts 16 , 17 which adjoin the side faces 12 , 13 , merge into a logarithmically falling profile P log . The surface area portion of those outer edge regions 14 , 15 of the raceway 8 of the inner bearing ring 3 which are configured with a logarithmically falling profile P log and of the edge parts 16 , 17 of the running faces 6 of the spherical disks 11 is, as is apparent from FIG. 3 at least in outlines, in each case approximately 30% of the surface area of the raceway 8 of the inner bearing ring 3 or of the running face 6 of a spherical disk 11 , with the result that the portion, which is configured with the same radius, of the running faces 6 of the spherical disks 11 and of the surface area of the raceway 8 in the inner bearing ring 3 is approximately 70%.
It can likewise be seen from FIG. 3 that the radius R 1 of the logarithmic profile P log at the outer edge regions 14 , 15 of the raceway 8 of the inner bearing ring 3 is greater than the radius R 2 of the running faces 6 of the spherical disks 11 , and that the radius R 3 of the logarithmic profile P log at the edge parts 16 , 17 of the running faces 6 of the spherical disks 11 is smaller than the radius R 2 of the running faces 6 of the spherical disks 11 . The center points M 1 , M 2 , M 3 of all the radii R 1 , R 2 , R 3 are arranged above one another in a clearly visible manner on the contact angle axis A D of the radial antifriction bearing 1 , with the result that uniform large wedge-shaped annular gaps are produced on both sides between the edge parts 16 , 17 of the running faces 6 of the spherical disks 11 and the edge regions 14 , 15 of the raceway 8 of the inner bearing ring 3 .
LIST OF DESIGNATIONS
1 Radial antifriction bearing
2 Outer bearing ring
3 Inner bearing ring
4 Rolling body
5 Bearing cage
6 Running face of 4
7 Raceway in 2
8 Raceway in 3
9 Inner side of 2
10 Outer side of 3
11 Spherical disks
12 Side face of 11
13 Side face of 11
14 Edge region of 8
15 Edge region of 8
16 Edge part of 6
17 Edge part of 6
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The radial antifriction bearing has an outer bearing ring, an inner bearing ring and roller bodies, which are arranged between the bearing rings, are held at uniform distances from one another in the peripheral direction by a bearing cage. The roller bodies are discs that each have two parallelly arranged lateral surfaces which are symmetrically flattened from a spherical basic shape. In order to prevent edge stresses between the discs and the raceways, at least the raceway in the inner bearing ring, on its outer edge areas, transition into a logarithmically decreasing profile.
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BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention pertains to sonic transmission systems and more particularly to systems for transmitting low frequency sonic signals with long range characteristics. Most particularly, this invention pertains to a parametrically pumped sonic weapon system.
2. Statement of the Prior Art
In order to destroy a target or kill or injure enemy personnel using a sonic signal, it is necessary to vibrate the target at or near its resonant frequency. Since the resonant frequency of commonly encountered structural targets is relatively low, typically 5-20 hertz, a low frequency sonic beam is required. In addition, the sonic beam must have sufficient range to be effective as a weapon. While these two criteria are simple to state, they are not easy to implement. The reason is Rayleigh's Law which may be written in equation form as follows:
δ=1.22 λ/sinφ
where
δ equals the radius of the central disc of energy,
λ equals the wavelength of the focused beam and
φ equals the angle subtended by the lens at the focal distance. For example, Rayleigh's Law predicts that the lens diameter required to focus a 10 hertz wave to within a 50 foot diameter zone of focus at a range of one mile is about 26,484 feet or about five miles.
Until recently, Rayleigh's Law was thought to be an absolute bar to the long-range propogation of a low frequency wave. Recently, however, it has been recognized that if two colinear sound beams are introduced into a nonlinear transmission medium, the interaction between them results in the production of the difference frequency. Thus, if the frequency of one of the beams is f and the frequency of the other beam is 2f, then the difference frequency component will also be f and may be used to augment the lower frequency sound beam. Moreover, the difference frequency component will have the range characteristics of the higher frequency component. However, this augmentation, commonly referred to as parametric pumping, will only take place if the phase difference between the two signals at the starting point of the interaction is approximately 90°. Otherwise, the component produced by the non-linear interaction will tend to oppose the lower frequency signal. The theoretical basis for these conclusions is set forth in an article by O. V. Rudenko and S. I. Soluyan entitled Theoretical Foundations of Nonlinear Acoustics (English translation) Consultant's Bureau, New York 1977, pp. 145-157. Applicant is not aware of any system which utilizes these principles to focus low frequency sonic signals over relatively large distances much less one that does so with sufficient power to destroy remote targets or kill or injure enemy personnel.
SUMMARY OF THE INVENTION
According to the present invention, I have developed a sonic weapon system which takes advantage of the interaction between colinear beams in a nonlinear medium to transmit low frequency sonic signals to remote targets, structural or human, with sufficient power to destroy them. The basic system includes a high level sonic source, means for separating the raw output from the sonic source into discrete frequency components, means for adjusting the phasing between these components and means for focusing them on the target.
The sonic source may comprise any sound source having a sufficient power output capacity to maintain destructive levels at the target and render the transmission medium, typically air, nonlinear. Commercially available jet and nuclear engines are sufficient for this purpose and their use is presently preferred.
Although nonlinear augmentation as between a fundamental signal frequency f and a pump signal frequency 2 f is known, it is desirable for weapon systems applications to provide still further augmentation. This may be effected by adding a second pump signal having a frequency (4 f) twice that of the first pump signal (2 f), a third pump signal (8 f) having a frequency twice that of the second pump signal (4 f), and so on. For the same reason and with the same effect that the 2 f pump signal augments the fundamental signal, the 4 f pump signal will augment the 2 f pump signal which, in turn, augments the fundamental signal. Similarly, the 8 f pump signal will augment the 4 f pump signal which augments the 2 f pump signal, and so on. As is the case between the 2 f pump signal and the fundamental signal, each successive pump signal must be 90° out of phase with the signal it augments.
The result is a low frequency sonic wave having the range characteristics of the highest frequency pump signal. The frequency of the highest frequency pump signal is, in turn, only limited by the expected losses due to divergence, sound absorption, transfer of energy to higher harmonics, etc. Based on these considerations, a maximum pump frequency of about 5,000 Hertz is presently preferred.
The frequency selector and phase controller serves to separate the raw output from the sonic source into the required fundamental and pump signal frequencies. The frequency selector and phase controller preferably comprises a combination of tubes, fans and masks. The input ends of the tubes are positioned to receive the raw output from the source such that the source output is distributed substantially equally among the tubes. A fan and a mask are disposed in the output end of each of the tubes, the mask being fixed relative to the tube.
The fan and mask in each tube are dimensioned such that as the fan rotates, it will alternately pass and block the flow of air through its corresponding tube. For example, a semicircular mask having a diameter equal to the internal diameter of the tube and a fan having a single matching semicircular blade are preferably used to generate the lower frequency components. Thus, as the blade rotates it will alternately pass through a position in which it is fully overlapped by the mask thus leaving half the output opening exposed, and a second position in which no portion of the blade is overlapped by the mask and the tube opening is fully blocked. This results in the generation of air pulses, the frequency of the pulses being dependent on the frequency of rotation of the fan blade. Since practical design limitations limit the maximum fan rotation speed, semicircular blades and masks will preferably not be used to generate the higher frequency components. According to the invention, this is overcome by adding additional mask sections and fan blades whereby each rotation of the fan blade results in the production of two or more pulses.
All the fans are preferably driven from a single rotating member through suitable gearing arrangements. The advantage of using a single rotating member, referred to herein as the fan speed controller, is that the fundamental and pump signal frequencies may be varied in step by simply varying the rotation rate of the controller.
Phasing is preferably accomplished by introducing a differential into the gearing for each fan. The differential permits each fan to be advanced or retarded relative to the others and thus may be used to control the relative timing and hence phase of the air pulses emanating from individual tubes.
The preferred sonic lens comprises a concave honeycomb array, each unit of the array comprising a hexagonal tubular structure closed at one end. By preselecting the cross-sections and lengths of the individual units, each unit may be tuned to enhance the reflection of a particular sonic frequency. Preferably, the array will have a number of honeycomb units tuned to each of the frequency components emanating from the frequency selector. Means are also preferably included for adjusting the pan and tilt of the individual honeycomb units whereby individual focusing of the honeycomb units may be effected. Also preferably included are means for adjusting the depth of each honeycomb unit relative to the others for fine tuning the phasing of the reflected signals.
The system is operated by focusing the output from the frequency selector and phase controller on the sonic lens and then focusing the sonic lens on the target. Upon activation of the source, the frequency selector will separate the raw output into discrete frequency components comprising a fundamental frequency at or near the resonant frequency of the target and successively higher pump frequencies. These components in turn strike the lens which then focuses them on the target. By selecting a sonic source with sufficient output to render the transmission medium nonlinear, the pump signals will augment the fundamental signal during transmission with the result being a high energy, low frequency sonic signal at the point of impact.
The destructive capability of the system during firing is maximized by adjusting the fan speed controller to match the fundamental frequency of the frequency selector and phase controller with the resonant frequency of the target. For this purpose, the preferred system also includes a laser interferometer for measuring the vibration frequency of the target. After appropriate signal conditioning, the information from the interferometer may be used to regulate the fan speed controller as required. Since accurate phasing is essential to effective operation, phasing is also preferably monitored during firing and adjusted as required. For example, signals from pressure sensors positioned to sense the amplitude peaks of each frequency component may be compared and this information used to implement phase control.
In one embodiment of the invention, level control of the individual frequency components is introduced by regulating the size of the opening to the individual tubes of the frequency selector. Portability may also be introduced as by using two flat bed trucks, one for the sound source and frequency selector and the other for the sonic lens and laser feedback system. The preferred embodiment also includes a computer for adjusting the various system parameters as required.
These as well as further features of the sonic weapon system according to the present invention will become more fully apparent from the following detailed description and annexed drawings of the preferred embodiment and suggested modifications thereof.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 is a diagrammatic illustration of the preferred parametrically pumped sonic weapon system according to the present invention;
FIG. 2A is a partially diagrammatic side elevation of the preferred frequency selector and phase controller;
FIG. 2B is a front elevation of the frequency selector and phase controller of FIG. 2A;
FIG. 3A is a front elevation of the tube 30a in FIG. 2 wherein the fan blade is positioned to pass air;
FIG. 3B is a view similar to FIG. 3A except that the fan blade is positioned to block air;
FIG. 4 is a front elevation of the preferred sonic lens;
FIG. 5 is a perspective view of one of the honeycomb units which make up the lens of FIG. 4, the arrows indicating axes of motion;
FIG. 6 is a perspective view of the preferred sonic weapon system in operation;
FIG. 7 is a diagrammatic illustration of a computer system for regulating the operation of the preferred sonic weapon system;
FIG. 8 is a front elevation of the tubes 30a and 30b in FIG. 2B showing an alternative means for effecting phase control; and
FIG. 9 is a front elevation of one of the tubes shown in FIG. 2B illustrating an alternative means for generating high level, discrete frequency sound waves.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawings, FIG. 1 is a diagrammatic illustration of the preferred sonic weapon system 10 in accordance with the present invention. As shown, the system 10 includes a high intensity sound source 12, a frequency selector and phase controller unit 14 for separating the source signal into preselected frequency components having predetermined phase relations, a sonic lens 16 for focusing the output signals from the unit 14 on a target 18, and a laser feedback system 19 for detecting variations in the vibration frequency of the target 18 and using this information to adjust the output signals from the unit 14 to maximize the destructive capability of the system 10.
The power output of the source 12 must be sufficient to destroy the target 18. In addition, the sound pressure level of the source signal must be adequate to render the signal transmission medium nonlinear, since, as is discussed above, medium nonlinearity must exist for parametric pumping to take place. As will be apparent hereinafter, it is not absolutely necessary to rely solely on the intensity of the source signal to render the medium nonlinear. However, when the intensity of the signal form the sonic source 12 is relied on, it is estimated that for the frequency band of interest in an air medium, the nonlinear effect becomes significant at sound pressure levels of about 140 db. Since the intensity from the sonic source 12 required to destroy structural targets will generally be greater than 140 db, typically 160-190 db, a source 12 capable of destroying such targets will also be sufficient to render the air medium nonlinear. Various commercially available apparatus, such as rocket and nuclear engines, satisfy these criteria.
Before the design and construction of an appropriate frequency selector and phase controller 14 and sonic lens 16 may be implemented, it is necessary to know the approximate fundamental or base frequency, the approximate frequency of the highest frequency pump signal, the desired effective range of the sonic blast, the desired effective target area of the sonic blast on impact, the diameter of the sonic lens and, finally, the characteristics of the medium.
As is noted above, the destructive capability of the sonic weapon system 10 is maximized when energy transfer from the sonic blast to the target 18 takes place at the resonant frequency of the target. Since the resonant frequency of most structures is typically 5-20 hertz, a base or fundamental frequency of 5 hertz is desirable. Assuming the preferred air medium, a maximum pump signal frequency of about 5,000 hertz is presently preferred since at higher frequencies attenuation losses are so great that the contribution from any such signal would be insignificant. For weapons applications, a 50 feet diameter zone of focus at the point of impact is presently preferred. Referring to Rayleigh's equation above, and recognizing that sin φ≈ lens diameter/range for the ranges of interest, it is apparent that the diameter of the sonic lens 16 is directly dependent on the desired range of the weapon. When the desired portability of the system 10 is taken into account, a lens diameter of 50 feet is presently preferred. Solving Rayleigh's equation using these parameters yields an effective range of about 5,000 feet, which is considered strategically acceptable.
Referring now to FIG. 2, the preferred frequency selector and phase controller 14 is shown. As illustrated, the unit 14 preferably comprises a plurality of tubular elements 30, here shown to be eleven tubular elements 30a-30k, each having a mask 32 and a fan 34 at one end 35 thereof, the masks and fans being unnumbered in the tubes 30h-30k for purposes of clarity. The speed of the fans 34 is variably controlled by a fan speed controller 40 and, for reasons that will be more fully apparent hereinafter, the masks 32 are preferably fixed relative to the tubes 30.
To accommodate the output of the sonic source 12, it is presently contemplated that each of the tubular elements 30 will have a diameter of approximately 10 feet. Since the diameter at the output of an engine of the types contemplated for use as the source 12 is approximately 10 feet, the unmasked or input ends 36 of the tubular members 30 are preferably connected to the sonic source 12 by a frustoconical connecting member 38 which has its narrow end joined to the output of the sonic source 12 and its widened end joined to the input ends 36 of the tubular members 30.
As discussed above, in order for the sonic weapon system 10 to be effective, the unit 14 must be capable of separating the raw output from the sonic source 12 into discrete frequency components comprising the fundamental frequency (5 hertz), a first pump signal having a frequency twice the base frequency (10 hertz), a second pump signal having a frequency twice that of the first pump signal (20 hertz), and additional pump signals, the frequency of each being twice that of the preceding pump signal, with the final pump signal having a frequency in the desired range, here selected to be about 5,000 hertz. In addition, augmentation of the fundamental frequency will not take place unless each frequency component is 90° out of phase with the next lowest frequency component. In other words, the 10 hertz pump signal must be 90° out of phase with the 5 hertz signal, the 20 hertz pump signal 90° out of phase with the 10 hertz pump signal, and so on. While the unit 14 could be designed to generate discrete frequency components having purely sinusoidal wave forms, this is not necessary. All that is necessary is that the selected wave forms have cyclical maxima which satisfy the specified frequency requirements. For example, sound pulses having a pulse repetition frequency meeting the above requirements would suffice. Accordingly, throughout the specification and claims, the term "frequency" is to be understood as the repetition rate of the selected wave form, whether it be sinusoidal, pulse, triangular, etc. The discrete frequency components at the output of each of the tubes comprising the unit 14 are best characterized as triangular waves. Referring to Table I below, the desired output frequencies of each of the eleven tubes 30a-30k illustrated in FIG. 2 is shown wherein the 5 hertz output signal from the tube 30a represents the fundamental frequency and the 5,120 hertz output signal from the tube 30k represents the highest pump frequency.
TABLE I______________________________________Tube Speed of Rota- Mask Output Fre-30 tion in RPM's Sections quency (hertz)______________________________________a 300 1 5b 600 1 10c 1,200 1 20d 2,400 1 40e 4,800 1 80f 4,800 2 160g 4,800 4 320h 4,800 8 640i 4,800 16 1,280j 4,800 32 2,560k 4,800 64 5,120______________________________________
As may be best seen in FIG. 2B, the fans 34a-34e disposed in the ends 35 of the tubular elements 30a-30e each consists of a single semicircular blade 42, the diameter of each blade 42 being equal to the internal diameter of its corresponding tube 30. The masks 32 disposed in the ends 35 of the tubes 30a-30e preferably each consist of a single mask section 43 of the same size and shape as the fan blades 42a-42e. For purposes of clarity, only the fan blade 42c and mask section 43c are numbered in FIG. 2.
Thus, as the blades 42a-42e rotate, each will pass through a first position in which the blade 42 is fully overlapped by its corresponding mask section 43 (FIG. 3A) and a second position in which there is no overlap between the blade 42 and its mask section 43 (FIG. 3B). It will thus be apparent that in the first position half of the opening 44 is exposed while in the second position the opening 44 is completely blocked. Thus, as air is blown through the tubes 30a-30e by the sonic source 12, the masks 32a-32e and fans 34a-34e cooperate to alternately pass and block the exit of air through the openings 44 thus forming air pulses at the output of these tubes. Clearly, the frequency of these pulses depends on the speed of rotation of the fans 34 which, as already noted, is regulated by the fan speed controller 40. Thus, if the fan 34a is rotated at 300 rpm, the frequency of the air pulses emanating from the end 35 of the tube 30a will be 5 hertz. Likewise, if the fan 34b is rotated at 600 rpm, the frequency of the air pulses emanating from the tube 30b will be 10 hertz. It will likewise be apparent that by successively doubling the speed of rotation of the fans 34c-34e up to a maximum speed of 4,800 rpm, the frequency of the air pulses emanating from the tubes 30c-30e will be 20 hertz, 40 hertz, and 80 hertz, respectively. (See Table I.)
Because of anticipated design problems, it is not presently desirable to rotate any of the fans 34 at speeds above 4,800 rpm and, therefore, frequencies above 80 hertz cannot be generated by using semicircular masks and fans with increased fan speeds. In accordance with the present invention, this problem is preferably overcome by maintaining the speed of rotation of the fans 34 in the tubes 30f-30k at 4,800 rpm while doubling the number of fan blades 42 and mask sections 43 in each successive tube. For example, referring again to FIG. 2B, it may be seen that the fan 34f is comprised of two fan blades 42f, each blade comprising a quarter circle having a radius equal to the internal radius of the tube 30f. Likewise, the mask 32f is also comprised of two quarter-circle sections 43f each having a radius equal to the internal radius of the tube 30f. It will thus be apparent that during each rotation of the fan 34f, the baldes 42f will twice assume positions in which the mask sections 43f completely overlap the blades and twice assume positions in which no portion of the mask sections 43f overlap the fan blades 42f. Consequently, two air pulses will emanate from the tube 30f for each full rotation of the fan 34f. If, as is presently preferred, the speed of rotation of the fan blade 34f is 4,800 rpm, it will be apparent that the frequency of the pulses emanating from that tube will be 160 hertz (see Table I). By successively doubling the number of fan blades 42 and mask sections 43 in each of the remaining tubes 30g-30k while maintaining the fan speed at 4,800 rpm, the frequency of the pulses emanating from these tubes will be 320 hertz, 640 hertz, 1,280 hertz, 2,560 hertz, 5,120 hertz, respectively (see Table I).
As noted above, rotation of the fans 34 is effected by the fan speed controller 40. Controller 40 is, in turn, driven by an appropriate prime mover, the sonic source 12 being presently preferred. The rotational speed at the output of the controller 40 is preferably selected as 4,800 rpm to match the highest required fan speed, with rotation of the individual fans 34 preferably being accomplished through suitable gearing arrangements. Since the design and construction of a suitable fan speed controller 40 and suitable gearing arrangements are well within the capabilities of the skilled art worker, further descriptions thereof are deemed unnecessary and none are given. When fan speed control is effected on this basis, it will be apparent that the frequency of the output signals emanating from the unit 14 may be accurately controlled by varying the primary rotational speed of the fan speed controller 40 and that the required frequency ratios between the fundamental and pump signals will be maintained as the speed of the controller 40 is varied.
It is presently preferred that rotation be imparted to the fans 34 at their peripheries since the conventional approach of rotating the fans at their centers is complicated by the magnitude of the pressures involved. For example, the fan blades 42 of the fans 34 could be secured at their peripheries to the internal annular surface of an external annular gear supported for rotation in its corresponding tube by suitable bearings. As shown in FIG. 2A, the masks 32 are preferably secured to the tubes 30 on the outward facing side of the fan 34 although they could, if desired, be disposed on the inward facing side as well.
While phase control can be introduced into the system 10 in a variety of ways, the preferred approach is to include a differential in the gearing for each tube fan 34. Then, if a particular fan requires phase advance or retardation, the differential gearing for that fan may be adjusted as desired. Since the design and construction details of such differentials are well known to those skilled in the art, a further description thereof is deemed unnecessary and none is given.
To maintain the required 90° phase separation between the different frequency components generated by the unit 14, pressure sensors 39 (FIG. 2) are preferably disposed at the ends 35 of each of the tubes 30 such that the pressure changes resulting from the alternate blockage and passage of air through the tubes 30 may be sensed. (For purposes of clarity, the sensors 39 are not shown in tubes 30j and 30k). The time differential between pressure peaks for the different frequency components may then be compared to determine whether the desired 90° phase relation is present. The differential gearings to the fans 34 may be adjusted to correct any errors.
The unit 14 may also include means for regulating the levels of the signals emanating therefrom. This can be accomplished, for exanple, by introducing diaphragms at the inlet ends 36 of the tubes 30 following the example of diaphragms used in cameras to control the diameter of the lens opening.
Referring now to FIG. 4, the preferred sonic lens 16 for focusing the signals emanating from the tubes 30 on the target 18 is shown. To be effective, the sonic lens 16 must be capable of focusing each of the different frequency components emanating from the unit 14. In addition, the lens 16 will preferably also be capable of effecting fine control of the phasing amongst the reflected components.
As shown in FIG. 4, the preferred sonic lens 16 comprises a concave honeycomb array. It may be seen in FIG. 5 that each unit of the array comprises a preferably hexagonal tubular structure 60 closed at one end 62. Preferably, the cross-sectional area of the tubes and the tube lengths are adjusted to provide tuning of the discrete frequency components incident thereon, a preferably equal number of individual honeycombs 60 being tuned to each frequency.
As shown by the arrows in FIG. 5, each honeycomb unit 60 is preferably supported for horizontal rotation (pan adjustment), vertical rotation (tilt adjustment) and front to back linear motion (depth adjustment). Pan and tilt adjustment of the individual honeycombs 60 gives the lens 16 the capability for individually focusing each honeycomb on the target 18. A pan adjustment of ±30° and tilt adjustment of ±20° should be sufficient for this purpose. The depth adjustment permits fine phase adjustment of the discrete frequency components generated by the unit 14 by allowing the starting point of the nonlinear interaction between these components to be varied. The phase adjustment introduced by the front to back linear motion of the individual honeycomb units is, of course, in addition to the phase differential introduced by the differential gearing arrangements discussed above in connection with the unit 14. Since it is contemplated that the depth adjustment of the individual honeycomb units will be used to effect fine phase adjustments only, and considering the relatively long wavelengths of the focused signals and the short travel distance between the unit 14 and the lens 16, a front to back linear travel of ±2 feet should be sufficient.
The phasing of the various frequency components reflected from the lens 16 may be checked by using pressure sensors 82 (FIG. 5) similar to the pressure sensors 39 on the unit 14 (FIG. 2). As shown in FIG. 5 the sensors 82 are preferably disposed at the open ends of each of the honeycomb units 60. Again, these sensors serve to check phasing by measuring the time differential between pressure peaks for the different frequency components, any necessary adjustments being made by adjusting the relative depths of the tubes 60 in the array as is more fully discussed above.
Suitable arrangements for effecting pan, tilt and depth adjustments are well known to those skilled in the art and such arrangements may be used herein. For example, commercial grade movie cameras have this capability. On this basis, a further description of the means for adjusting the orientation of the individual honeycomb units 60 is deemed unnecessary. Suffice it to say that all connections will preferably be made to the backs 62 of the individual units 60, the backs being selected solely on the basis of accessibility.
The sonic source 12, frequency selector and phase controller 14 and sonic lens 16 may, by themselves, be effectively used as a sonic weapon and these three components comprise the basic embodiment of the present invention. However, as noted above, energy transfer from the system 10 to the target 18 is maximized when the fundamental frequency of the sonic blast is matched to the resonant frequency of the target 18. Moreover, it must be recognized that as fissures, cracks, etc. begin to appear, the resonant frequency of the target may change. Therefore, and as shown in FIG. 1, the preferred sonic weapon system 10 includes a laser feedback system 19 for continuously sensing the resonant frequency of the target 18. The output signal from the system 19 is then used to adjust the fan speed controller 40 to match the fundamental frequency of the unit 14 to the resonant frequency of the target 18.
As diagrammatically illustrated in FIG. 1, the preferred laser feedback system 19 includes a laser 20, an interferometer 22, a frequency analyzer 24 and a band pass filter 26. The output from the laser 20 is split. The first beam is directed at the target and reflected therefrom to the interferometer 22, while the second beam is introduced directly into the interferometer. As is well known, by employing a photocell or similar device, the interferometer 22 can measure movement of the target 18 based on changes in the light pattern produced when the two laser beams are combined. Laser interferometers having sufficient resolution for incorporation in the sonic weapon system 10 are commercially available. For example, the Model 5526A laser interferometer marketed by Hewlett-Packard is capable of measuring distance with a resolution of one millionth of an inch. Also acceptable is Hewlett-Packard's Model 5501A which can measure distance with a resolution of six-ten-millionths of an inch. Based on preliminary estimates, this is at least a thousand times more accurate than is required for the system 10.
While the range of these instruments, approximately 200 feet, is limited by the range of the lasers incorporated therein, their range can be increased by using a more powerful laser as, for example the Keuffel and Esser Rangemaster. The Rangemaster, which operates on a different principle than the lasers incorporated in the Hewlett-Packard interferometers, has a range of up to about forty miles.
The frequency analyzer 24 is, as shown, connected to the output of the interferometer 22 and serves to determine the frequency of motion of the structure based on variations in the light pattern resulting from interference of the two laser beams. Thus, the output of the frequency analyzer 24 is a signal indicative of the frequency of motion of the target 18. Before applying this signal to the input of the fan speed controller 40, it is desirable to filter the signal to reduce unwanted system noise. As presently preferred and shown, this is accomplished by using the band pass filter 26 which serves to eliminate frequencies outside the range of interest. Since the design and construction of frequency analyzers 24 and band pass filters 26 suitable for incorporation in the system 10 are well known to those skilled in the art, further descriptions thereof are deemed unnecessary.
The frequency of the laser beam directed to the target 18 is preferably chosen for maximum ability to penetrate haze, dust, and other atmospheric disturbances. Based on these consideration, a helium-neon laser, operating in the red portion of the visible spectrum, is presently preferred. To insure the accuracy necessary to obtain a meaningful signal at the output of the frequency analyzer 24, the laser 20 and interferometer 22 should be kept as stationary as possible and isolated from ground vibrations. When designing the optical system, care should be taken to insure that only the light beam reflected from the target 18 can enter the interferometer 22. This latter feature is a characteristic of commercially available laser interferometers such as those discussed hereinabove.
Referring now to FIG. 6, the preferred sonic weapon system 10 together with means for transporting the weapon system to the target site are illustrated. As shown, the sonic source 12 and frequency selector and phase controller 14 are mounted on a first flatbed truck 80. The sonic lens 16 and the laser feedback system 19 are mounted on a second flatbed truck 82. The trucks will be driven to a site within the range of the sonic lens 16 and positioned such that the reflecting surface of the lens is directed at the target 18 and the unit 14 is directed at the lens but offset from the axis thereof. Accordingly, the assembly comprised of the source 12 and the unit 14 is preferably movably mounted on the flatbed truck 80 such that pan and tilt adjustments can be made. Likewise, the sonic lens 16 is also preferably movably mounted on the truck 82 for pan and tilt whereby the orientation of the lens may be adjusted. Since these pan and tilt adjustments may become defocused due to source vibrations during firing, means are preferably provided for monitoring them during firing and readjusting them as necessary.
Operation commences with the operator sighting the target 18 by using a sight 84 on the laser 20 provided for this purpose. The mechanisms for rotating and tilting the sonic lens 16 and for adjusting the relative orientations of the individual honeycomb units 60 thereof will preferably be operatively connected to track the laser 20 whereby sighting the target in the laser will simultaneously focus the lens. At or prior to this point, the laser feedback system 19 and the fan speed controller 40 are activated, the primary rotational speed of the controller 40 being initially selected to match the estimated resonant frequency of the target 18. Firing is commenced by activating the source 12.
As firing continues, the laser feedback system 19 senses variations in the resonant frequency of the target 18 and readjusts the speed of the controller 40 to vary the fundamental frequency of the unit 14 as required.
Preferably, the outputs from the pressure sensors 39 and 82 are also continuously monitored to insure that the desired 90° phase differential between successive frequency components prevails, the necessary adjustments being made on a continuous basis during firing.
It will be apparent from the foregoing that effective operation of the sonic weapon system 10 requires the continuous readjustment of a number of parameters. This, combined with the desirability of rapid readjustment for maximizing the destructive capability, dictates that the number of manual operations be minimized. Accordingly, it is presently preferred that the sonic weapon system 10 be computer controlled.
As diagrammatically illustrated in FIG. 7, the computer 90 receives signals from the laser tracking mechanism, the laser feedback system 19, and the pressure sensors 39 and 82, and processes this information to provide output signals indicative of the adjustments required. After suitable conditioning, these output signals are used to adjust the physical orientation of the unit 14 relative to the sonic lens 16; adjust the pan and tilt of the individual honeycomb units 60 for optimum focus; adjust the fan speed controller 40 to keep the system fundamental frequency in step with the resonant frequency of the target 18; and adjust the differential gearings to the individual tube fans 34 and the depth of the units 60 to maintain 90° phasing. As shown in FIG. 7, the computer 90 is also preferably connected to one or more output devices, such as the CRT 92, for accommodating monitoring of system operation. The computer controller is also preferably connected to an input device, such as the terminal 94, for feeding basic information, such as the target range and expected target resonant frequency into the computer, and for accommodating overrides when necessary. Since the design, implementation and programming of a suitable computer system for carrying out these functions is well within the capabilities of the skilled art worker once the method and parameters of the operation of the system 10 are known, further descriptions thereof are deemed unnecessary.
While computer control is preferred, the system 10 could be operated without the computer by having the operator monitor the signals which would otherwise be inputted to the computer and manually effect adjustment either directly or through appropriate mechanical-electronic/electrical controls. Most preferably, the system 10 will be provided with the capability for both computer and manual control to accommodate operation when the computer is down.
Preliminary calculations have been carried out based on the sonic weapon system 10 to assess its efficacy. These calculations assumed a power transmission efficiency of 30% based on expected losses from atmospheric attentuation, beam spreading, loss of energy to harmonics, etc. It was also assumed that the target structure consisted of a building 50×50×100 feet high with four concrete walls one foot thick. For a resonant frequency of approximately 5 hertz, these calculations indicate that it will take approximately 13.2 seconds to destroy the entire structure, that approximately 11 gallons of jet fuel will be consumed, and that the required sound level at the target will be approximately 169 db. Similar calculations were carried out for a building 50×50×100 feet high with walls two feet thick. Assuming a resonant frequency of 10 hertz, these calculations indicate that the entire structure could be destroyed in about 6.2 seconds, that approximately 84 gallons of jet fuel will be consumed and that the sound pressure level at the target must be about 181 db.
In addition to destroying structures, the weapon system 10 could be effectively utilized to selectively disable or kill enemy troops depending upon the sound level selected. Since troop disablement requires less power and higher frequencies, a system limited to this application could use a smaller lens and a less powerful sonic source. Apart from wartime applications, it will be apparent that the system 10 has peace time uses as well, building demolition being one example. If used for this purpose, the sonic source need not be as powerful as the source 12 required for the system 10 since the required transmission range is not as great.
Once the preferred sonic weapon system 10 described hereinabove is known, those skilled in the art will appreciate that various additions and modifications may be made thereto without departing from the spirit and scope of this invention. For example, while phase control of the unit 14 is preferably accomplished by employing differential gearing, this is not absolutely necessary. For example, phasing can be effected by adjusting the relative orientations of the masks 32 at the ends 35 of the tubes 30. Thus, as shown in FIG. 8 for the case of the tubes 30a and 30b, by rotating the mask 32b one quarter turn relative to the mask 32a, it will be apparent that the signal exiting the tube 32a will lead the signal exiting the tube 32b by 90°. It will be further apparent that by rotating each successive mask 32c-32k one quarter turn relative to the preceding one, each frequency component exiting the unit 14 will lag the next lower one by 90° and the desired phasing will have been achieved.
In a further modification of the unit 14, the conventional fans 34 illustrated in FIG. 2 are replaced with fans having blades which push air in both directions. When this embodiment is used, a separate sound source such as the sonic source 12 would not be used and fan blades 42 would themselves generate sound. For example, as shown in FIG. 9, the fan 100 could be substituted for the fans 34 used to generate the five low frequency components in FIG. 2. As shown, half of the fan 100 has blades 102 oriented for pushing air in one direction while the other half 104 are oriented for pushing air in the reverse direction. It will be apparent from FIG. 9 that the fan blades 102 and 104 contribute to the air flow as they come out from behind the mask 32. For example, if all the blades which push air forward are exposed at one time there would be a maximum forward thrust of air. As the fan rotated, there would be a combination of both forward and reverse blades exposed which would slow the forward thrust. At a still later point, only those blades which were pushing air in the reverse direction would be exposed. The principal advantage of this approach is that the resulting sound pressure waves will be approximately triangular in shape and thus will more closely approximate sinusoidal air flow. When this modification is employed, energy input could be derived, for example, from the source utilized as the sound source 12 in the FIG. 1 embodiment, the only difference being that the source now serves to rotate the fan blades. The arrangement illustrated in FIG. 9 may be utilized to generate the higher frequency components by adding additional opposed blade sections, the number of opposed blade sections required being equal to the number of mask sections required in the FIG. 2 embodiment as set forth in Table I. Phasing of a plurality of fans 100 could be introduced by differential gearing, relative rotation of the masks, or any other suitable techniques.
The FIG. 9 embodiment may be further modified by providing fan blades and masks at both ends of the tube. This arrangement would be more truly resonant than those discussed above with the length and cross-section of the tube and the phasing of the fan blades and masks providing highly selective sound filtering and sound generation capabilities.
As noted above, it is not necessary to rely solely on the intensity of the sound generated by the sonic source 12 to render the transmission medium, typically air, nonlinear. Thus, for example, the transmission medium may be rendered nonlinear or its nonlinearity enhanced by periodically introducing shock waves along the transmission path. Such shock waves, which are familiar when a body passes through air at supersonic speeds or highly compressed air is suddenly released, result in a rapid rise in pressure that is propagated through the medium. It is presently contemplated that such shock waves will be used to enhance the nonlinearity of the air medium by introducing them into the transmission path in synchronization with the fundamental frequency of the system 10. Since, as is discussed above, the conversion efficiency obtainable by nonlinear parametric pumping is dependent on medium nonlinearity, enhancing the nonlinearity of the medium will increase the overall efficiency of the system 10.
Still further changes and modifications may be made. For example, while the tubes 60 which make up the lens 16 have been described as having preferably hexagonal cross-sections, this is not necessary and other cross-sectional configurations, such as circular cross-sections, may be substituted. In any event, because of the high sonic levels and numerous moving parts, aerospace design techniques will preferably be employed throughout.
Since these as well as further changes and modifications may be made within the scope of the present invention, the above description should be construed as illustrative and not in a limiting sense, the scope of the invention being defined by the following claims.
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A system for transmitting a parametrically pumped sonic signal through a transmission medium to a remote location is disclosed. The preferred system, which is particularly intended for use as a sonic weapon, comprises a sound source; means for separating the sound into a plurality of discrete frequency components including a fundamental component and at least one additional component, each additional component having a frequency twice that of the next lowest frequency component; means for adjusting the phase difference between each frequency component and the next lowest frequency component to substantially 90°; means for colinearly focusing the components on the remote location; and means for rendering the transmission medium nonlinear between the focusing means and the remote location.
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CROSS REFERENCE TO RELATED APPLICATIONS
This application claims the benefit of U.S. Provisional Application No. 61/138,439, filed Dec. 17, 2008, which is incorporated by reference.
This application is related to U.S. patent application Ser. No. 12/484,083, filed Jun. 12, 2009, entitled “Spatial-Temporal Event Correlation For Location-Based Services,” which is incorporated by reference.
If there are any contradictions or inconsistencies in language between this application and the cases that have been incorporated by reference that might affect the interpretation of the claims in this case, the claims in this case should be interpreted to be consistent with the language in this case.
FIELD OF THE INVENTION
The present invention relates to telecommunications in general, and, more particularly, to location-based services.
BACKGROUND OF THE INVENTION
Location-based services are services provided based on the location of objects. The most prevalent location-based service is Enhanced 911 (or E911) services. The Enhanced 911 service provides 911 operators and emergency responders with information such as the identification of the person calling and the location of the caller. All mobile telephones sold in the United States today have this feature.
Location-based services include, for example and without limitation, satellite navigation devices that let a user know the location of the closest hospital or gas station to a user. Location-based services may also alert enterprises, such as gas stations, as to when a potential customer is within a certain distance. The enterprise may then send targeted advertisements to a traveler, such as discounts, etc.
Still other location-based services are targeted to the tracking of objects, such as, for example and without limitation, tracking of packages, tracking a fleet of vehicles, or determining the number of people who are in a given area for allotting government services where they may be most needed.
The problem is how to protect users' privacy as they use location-based services.
Protecting user privacy is done by a user creating a series of rules for access to the user's information. These rules set privacy settings based on, for example and without limitation, the recipient of the user's information, where the user may be located, the time, etc.
In the prior art, the privacy settings are maintained in a location-based privacy system such as the one in FIG. 3 . In FIG. 2 , object 201 - 1 (here a person) travels along path 202 - 1 through space 101 - 4 , space 101 - 5 , and space 101 - 3 . As user 201 - 1 travels along this path, user 201 - 1 sends out “location objects” which indicate where the user is located. In accordance with the illustrative embodiment of the present invention, user 201 - 1 does this by the use of location generator 301 , and user 201 - 1 has defined different location-based service privacy settings for each space.
Because of the different privacy settings, location-based privacy system 300 checks the rules for each location object to determine whether or not a given location recipient should receive each location object. Location server 302 checks with rule maker 304 to determine whether or not it should send the location object to location recipient 303 .
SUMMARY OF THE INVENTION
The present invention provides a method determining the privacy settings for location-based services without some of the disadvantages of the prior art. This is done by establishing a session between the location generator and the location recipient.
The session is created by a validator that is capable of keeping track of the rules for a stream of location objects created by a location generator. The validator determines what information to send to the location recipient without having to determine the rules for each location object and each location recipient every time a new location object is received by the location server.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 depicts an illustrative map in accordance with the illustrative embodiment of the present invention.
FIG. 2 depicts an illustrative map in accordance with the illustrative embodiment of the present invention.
FIG. 3 depicts a schematic diagram of the salient components of location-based services privacy system 300 in accordance with the prior art.
FIG. 4 depicts a schematic diagram of the salient components of location-based services privacy system 400 in accordance with the illustrative embodiment of the present invention.
FIG. 5 depicts a schematic diagram of the salient components of location-based services privacy system 400 in accordance with the illustrative embodiment of the present invention.
FIG. 6 depicts a flowchart of the salient tasks associated with the operation of the illustrative embodiment of the present invention.
FIG. 7 depicts a flowchart of the salient tasks associated with the operation of task 604 in accordance with the illustrative embodiment of the present invention.
FIG. 8 depicts a flowchart of the salient tasks associated with the operation of task 605 in accordance with the illustrative embodiment of the present invention.
DETAILED DESCRIPTION
FIG. 1 depicts illustrative map 100 in accordance with the illustrative embodiment of the present invention.
Map 100 is a rectangular area in which we are interested for the purposes of the illustrative embodiment of the present invention. Map 100 comprises areas 101 - 1 through 101 - 6 .
Although, in accordance with the illustrative embodiment of the present invention, map 100 represents some physical space, it will be clear to one skilled in the art after reading this disclosure, how to make and use alternative embodiments of the present invention in the space is not a physical space, for example and without limitation, the space is instead a virtual space.
Although, in accordance with the illustrative embodiment of the present invention, map 100 represents space in two dimensions (2-D), it will be clear to one skilled in the art after reading this disclosure, how to make and use alternative embodiments of the present invention in the space is not a two dimensional (2-D) space but instead the space is any number of dimensions, for example and without limitation, three dimensions (3-D), four dimensions (4-D), etc.
Although map 100 is a rectangular area, it will be clear to one skilled in the art after reading this disclosure, how to make and use alternative embodiments of the present invention in which map 100 is any shape or any size.
Although areas 101 - 1 through 101 - 6 are a rectangular areas, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which areas 101 - 1 through 101 - 6 are any shape or any size.
Although areas 101 - 1 and 101 - 4 overlap, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which areas 101 - 1 and 101 - 4 do not overlap, overlap completely, or overlap with other areas.
Although areas 101 - 2 and 101 - 4 overlap, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which areas 101 - 2 and 101 - 4 do not overlap, overlap completely, or overlap with other areas. It will also be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention
FIG. 2 depicts map 100 in accordance with the illustrative embodiment of the present invention. Map 100 comprises areas 101 - 1 through 101 - 6 , object 201 - 1 , and path 202 - 1 .
Although FIG. 2 depicts one object, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which there are any number of objects.
Although FIG. 2 depicts one path, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which there are any number of paths.
Although object 201 - 1 is depicted as a person, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which object 201 - 1 can be any object, for example, and without limitation: a person, a sensor, a vehicle, an animal, a telecommunications terminal, a stationary object, etc.
Although path 202 - 1 is depicted as going through areas 101 - 4 , 101 - 5 , and 101 - 3 of the map, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which path 202 - 1 can travel through any area of map 100 .
Although object 201 - 1 is depicted as traveling along path 202 - 1 , it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which object 201 - 1 can travel along any path and through any area of map 100 .
In accordance with the illustrative embodiment of the present invention, object 201 - 1 travels along path 202 - 1 through areas 101 - 4 , 101 - 5 , and 101 - 3 of map 100 . As it travels along this path, the location object 201 - 1 is noted and tracked. In accordance with the illustrative embodiment of the present invention, the location is noted by satellite trilateralization, such as, for example, and without limitation, global positioning system (GPS). Other techniques for determining location include, for example and without limitation, triangulation of endpoints in cellular or wireless networks, proximal device broadcast, purchasing transactions (such as those by credit card or debit card), vehicle-to-vehicle networks, radio signals, etc. In accordance with the illustrative embodiment of the present invention, the location is then tracked by sending periodic updates through a wireless network, such as, for example and without limitation, a mobile telephone or data network, a packet radio network, a IEEE 802.11 (Wi-Fi) network, etc.
FIG. 3 depicts a schematic diagram of the salient components of location-based services privacy system 300 in accordance with the prior art. FIG. 3 comprises location generator 301 , location server 302 , location recipient 303 , and rule maker 304 .
FIG. 4 depicts a schematic diagram of the salient components of location-based services privacy system 400 in accordance with the illustrative embodiment of the present invention. FIG. 4 comprises location generator 301 , location server 302 , location recipient 303 , rule maker 304 , and validator 401 .
For the purpose of this specification, a “location generator” is defined as any device (hardware and/or software) or event that provides an indication of its location. Examples of location generators include, for example and without limitation, global positioning system (GPS) receiver units, including those in mobile telecommunications terminals, triangulation of endpoints in cellular or wireless networks, purchasing transactions (such as those by credit card or debit card), vehicle-to-vehicle networks, radio signals, etc.
For the purpose of this specification, a “location recipient” is defined as any device (hardware and/or software) or person that receives the location information of a location generator. Examples of location recipients include, for example and without limitation, emergency service providers who use location information to locate people in need, a device used by a parent to track his or her child, providers of a location-based services, etc.
For the purpose of this specification, “location information” is defined as information regarding the location of a location generator. This includes, for example and without limitation, a location object, a subset of the information in a location object, the exact coordinates of a location generator, the name of a place of where a location generator is located, a street address, etc.
Although in accordance with the illustrative embodiment of the present invention, FIG. 4 comprises one location generator, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which there are any number of location generators.
Although in accordance with the illustrative embodiment of the present invention FIG. 4 comprises one location server, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which there are any number of location servers.
Although in accordance with the illustrative embodiment of the present invention, FIG. 4 comprises one rule maker, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which there are any number of rule makers.
Although in accordance with the illustrative embodiment of the present invention, FIG. 4 comprises one location recipient, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which there are any number of location recipients.
Although in accordance with the illustrative embodiment of the present invention, FIG. 4 comprises one validator, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which there are any number of validators.
Although in accordance with the illustrative embodiment of the present invention, validator 401 is inside of location server 302 , it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which validator 401 is located elsewhere, for example and without limitation, between location server 302 and location recipient 303 , between location generator 301 and location server 302 , etc.
In accordance with the illustrative embodiment of the present invention, validator 401 is implemented by the means of an event processor.
For the purpose of this specification, an “event processor” is defined as hardware and software that performs event processing, event filtering, and event correlation.
In accordance with the illustrative embodiment of the present invention, event processing refers to operations performed by an information system, for example and without limitation, operations to receive, distribute, store, modify, generate, or discard events. In accordance with the illustrative embodiment of the present invention, event filtering is a type of event processing in which an event is forwarded or blocked to a recipient based on a property of the event or some other computational context.
In accordance with the illustrative embodiment of the present invention, event correlation is a type of event processing in which an event is evaluated primarily with respect to other events but also system state or context, in order to produce related events. These related events ideally have the characteristics that there is a reduction in the volume of events and/or the information content of the new events is transformed to a more relevant value.
It will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention, in which validator 401 is implemented by another means.
FIG. 5 depicts a schematic diagram of the salient components of location-based services privacy system 400 in accordance with the illustrative embodiment of the present invention. FIG. 5 comprises location generator 301 , location server 302 , location recipient 303 , rule maker 304 , validator 401 , and session 501 .
Although in accordance with the illustrative embodiment of the present invention, FIG. 5 comprises one session, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which there are any number of sessions.
Although in accordance with the illustrative embodiment of the present invention, session 501 is between location generator 301 , validator 401 , and location recipient 303 , it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which the session may comprise other components, for example and without limitation, rule maker 304 .
Although in accordance with the illustrative embodiment of the present invention, session 501 comprises one location generator, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which the session may comprise any number of location generators.
Although in accordance with the illustrative embodiment of the present invention, session 501 comprises one validator, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which the session may comprise any number of validators.
Although in accordance with the illustrative embodiment of the present invention, session 501 comprises one location recipient, it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which the session may comprise any number of location recipients.
FIG. 6 depicts a flowchart of the salient tasks associated with the operation of the illustrative embodiment of the present invention.
In accordance with the illustrative embodiment of the present invention, the tasks outlined in FIG. 6 are performed at validator 501 . However, it will be clear to one skilled in the art, after reading this disclosure how to make and use other implementations of the present invention in which the some or all of the steps are performed by another device, for example, and without limitation, location generator 301 , rule maker 304 , a separate event processor, etc.
At task 601 , validator 501 receives a first request. Although, in accordance with the illustrative embodiment of the present invention, this is received from location recipient 303 , it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which the first request received from another source.
In accordance with the illustrative embodiment of the present invention, the validator 501 will receive an indicium of the location generator as part of this request. In accordance with the illustrative embodiment of the present invention, an indicium of the location generator is some indication of where the location generator may be located. These are, for example, and without limitation, the name of the object to be located, the X and Y coordinates at which the object is located, a name for the place where the object is located (such as “home,” “work,” “school,” etc.), a store where a purchase may have occurred, or any signal that may tell where the object is located.
At task 602 , validator 501 receives a first location object. Although, in accordance with the illustrative embodiment of the present invention, the first location object is received from location recipient 303 , it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which the first request received from another source.
At task 603 , validator 501 receives a first rule. Although, in accordance with the illustrative embodiment of the present invention, the first rule is received from rule maker 304 , it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which the first request received from another source.
At task 604 , validator 501 generates a first function. This is further detailed in FIG. 7 .
At task 605 , validator 501 establishes a session between location object and location recipient. This step is further detailed in FIG. 8 .
At task 606 , a session is terminated when the conditions of the function are no longer met. For example and without limitation, if the condition of the function is “Let my spouse know my exact location after 9 p.m. and before 8 a.m.,” and it is 8 a.m. the session between the location generator and the location recipient will be terminated. It will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention that perform task 606 .
It will be clear to one skilled in the art, after reading this disclosure, how to make and use other implementations of the present invention in which one or more of the steps are omitted or are performed in a different order than the one presented or simultaneously.
FIG. 7 depicts a flowchart of the salient tasks associated with the operation of task 604 in accordance with the illustrative embodiment of the present invention.
At task 701 , the rules of location generator are determined. In accordance with the illustrative embodiment of the present invention, this task is performed based on the rules received from rule maker 304 . In accordance with the illustrative embodiment of the present invention the location generator would have general rules relating to the dissemination of location information to other parties. For example and without limitation, a user of location generator 301 may want to prohibit the distribution of location objects to all parties (except for emergency services).
In accordance with the illustrative embodiment of the present invention, rules include, for example and without limitation, policies and settings that are set by the user, are default settings, or are set by some other party. These rules define the relationship between the components and parties.
At task 702 , rules of location recipient are determined. In accordance with the illustrative embodiment of the present invention, this task is performed based on the rules received from rule maker 304 . In accordance with the illustrative embodiment of the present invention, the location recipient would have general rules relating to the dissemination of location information to other parties. For example and without limitation, location recipient may be a large organization and only certain members of that group may be allowed access to location objects.
At task 703 , the relationship of between location generator and location recipient is determined. In accordance with the illustrative embodiment of the present invention, this task is performed based on the rules received from rule maker 304 . In accordance with the illustrative embodiment of the present invention, the location recipient would have general rules relating to the dissemination of location information to other parties based in particular on a relationship between the two parties. Examples of these relationship queries are, for example and without limitation, “Allow my friends know that I am within five miles of them,” or “Let my spouse know my exact location,” etc.
At task 704 , the relationship of between location generator and a user of the location recipient is determined. In accordance with the illustrative embodiment of the present invention, this task is performed based on the rules received from rule maker 304 . In accordance with the illustrative embodiment of the present invention, the location recipient would have general rules relating to the dissemination of location information to other parties based in particular on a relationship between the location generator and a user of the location recipient. Examples of these queries are, for example and without limitation, “Send my present location to the medical center, but only allow my physician to view my location,” “Allow my supervisor and my assistant to know my location, but do not allow anyone else at my job to see my location,” etc.
At task 705 , the rules and relationship between location generator and location recipient as product of time are determined. In accordance with the illustrative embodiment of the present invention, this task is performed based on the rules received from rule maker 304 . In accordance with the illustrative embodiment of the present invention, the location recipient would have general rules relating to the dissemination of location information to other parties based in particular on a relationship between the two parties as a product of time. Examples of these relationship queries are, for example and without limitation, “Allow my friends know my location during the weekend,” “Let my spouse know my exact location after 9 p.m. and before 8 a.m.,” “Allow my employer to know my location within 500 meters between the hours of 8:30 am and 5:30 pm.,” etc.
At task 706 , rules and relationship between location generator and location recipient as product of location is determined. In accordance with the illustrative embodiment of the present invention, this task is performed based on the rules received from rule maker 304 . In accordance with the illustrative embodiment of the present invention, the location recipient would have general rules relating to the dissemination of location information to other parties based in particular on a relationship between the two parties as a product of location. Examples of these relationship queries are, for example and without limitation, “Allow my friends know that I am within five miles of them,” “Let my spouse know my exact location unless I am in Atlantic City,” “Allow my employer to know whether or not I am at a work site,” etc.
At task 707 , the function based on determined rules and determined relationships is generated. It will be clear to one skilled in the art, after reading this disclosure that the generated function is capable of handling operations that are combinations of the above operations, for example and without limitation, “Send my location to the medical center, on Monday between 9 am and 5 pm, when I am in New Jersey, and only allow physician to view this information,” “Allow my spouse to view my location only when I am within 5 miles of my home Monday through Friday, but do not allow other members of my household to view this information,” etc. It will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which task 707 is performed.
In accordance with the illustrative embodiment of the present invention, the following examples, without limitation, are those in which rules of the present invention are enacted using Extensible Markup Language (XML). It will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which a different language is used.
The following example is one in which some hotels to are permitted access to the user's location when the user is at an airport, regardless of the airport's location.
<rule id=“NM32848”>
<conditions>
<identity>
<one domain=“hertz.com”/>
<one domain=“avis.com”/>
<one domain=“budget.com”/>
</identity>
<gp:location-condition>
<gp:location profile=“rpid-condition”>
<rpid:place-type>
<lt:airport/>
</rpid:place-type>
</gp:location>
</gp:location-condition>
</conditions>
<transformations/>
</rule>
</ruleset>
Example 1
Access to User Location at Airport
In the following example “sphere” is to allows user bob@example.net to access the user's location information. This rule keeps valid even if the user's home moves.
<rule id=“NM32848”>
<conditions>
<identity>
<many>
<except id=“sip:bob@example.net”/>
</many>
</identity>
<gp:location-condition>
<gp:location profile=“rpid-condition”>
<rpid:sphere>
<rpid:home/>
</rpid:sphere>
</gp:location>
</gp:location-condition>
</conditions>
<transformations/>
</rule>
Example 2
Granting Access to User's Location Based on “Sphere”
It will be clear to one skilled in the art, after reading this disclosure, how to make and use other implementations of the present invention in which one or more of the steps are omitted or are performed in a different order than the one presented or simultaneously.
FIG. 8 depicts a flowchart of the salient tasks associated with the operation of task 605 in accordance with the illustrative embodiment of the present invention. In accordance with the illustrative embodiment of the present invention, task 801 through task 806 are performed by the function at validator 401 . It will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention in which task 801 through task 806 are performed elsewhere.
Although, in accordance with the illustrative embodiment of the present invention, FIG. 8 depicts four tests to determine permissions between location generator 301 and location recipient 303 , it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention, in which any number of tests are performed.
At task 801 , the function determines whether the location recipient has any permission to access the location object. If it does have permission, the decision process proceeds to task 802 . If it does not, it proceeds to task 805 .
At task 802 , the function determines whether the location recipient has permission to access location object given the current or other location of the location generator. If it does have permission, the decision process proceeds to task 803 . If it does not, it proceeds to task 805 .
At task 803 , the function determines whether the location recipient has permission to access the location object at current or other time. If it does have permission, the decision process proceeds to task 804 . If it does not, it proceeds to task 805 .
At task 804 , the function determine the appropriate resolution that location recipient may access location object. In accordance with the illustrative embodiment of the present invention, different location recipients have different permissions regarding the exactness of the location of the location generator. For example, and without limitation, a location generator may give permissions such as, “Allow my friends know that I am within five miles of them, but do not inform them of my location” “Let my spouse know my exact location,” or “Allow my employer to know that I am in New Jersey, but do not give my employer my exact location,” etc.
At task 805 , a session is NOT established. Although in accordance with the illustrative embodiment of the present invention, after task 805 , the system returns to step 801 , it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention where the system proceeds to another point, for example and without limitation, the system proceeds to the end point.
At task 806 , a session is established. it will be clear to one skilled in the art, after reading this disclosure, how to make and use alternative embodiments of the present invention that perform task 806 .
It will be clear to one skilled in the art, after reading this disclosure how to make and use other implementations of the present invention in which one or more of the steps are omitted or are performed in a different order than the one presented or simultaneously.
It is to be understood that the disclosure teaches just one example of the illustrative embodiment and that many variations of the invention can easily be devised by those skilled in the art after reading this disclosure and that the scope of the present invention is to be determined by the following claims.
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A method for determining the privacy settings for location-based services without some of the disadvantages of the prior art is disclosed. This is done by establishing a session between the location generator and the location recipient. The session is created by a validator that is capable of keeping track of the rules for a stream of location objects created by a location generator. The validator determines what information to send to the location recipient without having to determine the rules for each location object and each location recipient every time a new location object is received by the location server.
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BACKGROUND OF THE INVENTION
(1) Field of the Invention
The present invention pertains to a manually manipulated illuminator used in microsurgery, and in particular ophthalmic surgery.
(2) Description of the Related Art
Although all types of surgery require a great deal of concentration and manual dexterity from the surgeon, perhaps one of the most intense types of surgery is ophthalmic surgery, or surgery of the eye. In ophthalmic surgery, the reduced size of the microsurgical instruments used and the minute area within the eye in which the surgery is performed demand a great deal from the surgeon's patience and skills. When considering that any unanticipated difficulties in using prior art microsurgical instruments in performing ophthalmic surgery could, in the least, add to the difficulty and mental strain of the surgeon in performing the surgery, or in the most, lead to complications in the functioning of the patient's eye, any modification to a microsurgical instrument making it easier for the surgeon to use is a significant contribution to the field of ophthalmic surgery.
In typical ophthalmic surgery, it is necessary that a light source be provided inside the patient's eye so that the rear wall of the eye, or other interior area of the eye where surgery is to be performed, is well illuminated enabling the surgeon to easily view the area of surgery. Most common ophthalmic surgery procedures involve first making a small incision into the eye interior for insertion of the illuminator, and making a second small incision into the eye interior for insertion of the instrument to be used by the surgeon in performing the particular surgery. With one hand, the surgeon must hold the light probe inserted through the first incision in the eye and with the other hand, the surgeon must hold the microsurgical instrument inserted through the second incision in the eye.
The typical microsurgical illuminator comprises a handle with a small cannula or cylindrical metal sleeve projecting from a distal end of the handle. An optic fiber having a proximal end connected to a source of light passes through the center of the handle and the cannula. The distal end of the optic fiber is positioned adjacent the distal end of the illuminator cannula. The distal end surface is planar and the plane of the distal end of the optic fiber is positioned normal to the center axis of the illuminator cannula and the center axis of the optic fiber passing through the cannula. As explained in the U.S. Pat. No. 4,878,487, it is preferable that the end surface of the fiber be ground to a smooth, flat surface that is perpendicular to the longitudinal axis 30 of the probe tip to limit the diffusion of light transmitted through the end surface and ensure the light beam is emitted generally straight ahead.
The incision made in the eye for insertion of the illuminator is very small, usually just large enough to permit the insertion of the illuminator cannula, typically a 20 gauge needle, through the incision. During surgery, there must be a close fit around the illuminator by the eye wall. The incision must seal around the instrument in order to maintain fluid pressure in the eye to keep the eye inflated. The fluid pressure is provided by saline solution supplied to the eye interior under a pressure head. With the incision being this small, the surgeon usually experiences a certain degree of difficulty in introducing the distal end surfaces of the illuminator cannula and optic fiber into the eye incision. This is primarily due to the incision being a slit incision and the distal end surface of the prior art illuminator being a flat, planar surface normal to the center axis of the illuminator cannula and optic fiber. This "difficulty" in introduction can cause severe inward deformation of the eye wall. This deformation may lead to the creation of a retinal detachment in this area.
SUMMARY OF THE INVENTION
It is an object of the present invention to eliminate the difficulties usually experienced by the surgeon in attempting to insert a microsurgical illuminator through an incision made in the eye by providing a modified construction of the illuminator distal end.
The microsurgical illuminator of the present invention is comprised of a handle, a cannula projecting from the distal end of the handle, and a length of optic fiber passing through the handle and the cannula. The proximal end of the optic fiber is provided with a connector for connecting the proximal end to any of the available sources of light typically used with microsurgical illuminators. The distal end of the optic fiber and the distal end of the illuminator cannula are both provided with flat, beveled surfaces. By beveled, what is meant is that the distal end surface of the optic fiber and the distal, annular end surface of the cannula are both formed at an oblique angle to the center axes of the cannula and the portion of the optic fiber passing through the cannula. In the preferred embodiment, the oblique angle formed by these end surfaces is 15° from a plane positioned normal or perpendicular to these axes. Forming these distal end surfaces with this oblique angle gives the illuminator distal end a leading edge that is much more easily inserted into an eye incision and significantly simplifies the task of inserting a microsurgical illuminator into an eye incision provided for the illuminator. The angled distal end surfaces also significantly reduce trauma to the tissues of the eye surrounding the incision.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a fragmentary, side elevation view, partially in section, of the microsurgical illuminator of the present invention; and
FIG. 2 is an enlarged side elevation view, partially in section, of the distal end of the microsurgical illuminator shown in FIG. 1.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The microsurgical illuminator 10 shown in FIG. 1 is described herein as used in ophthalmic surgery. However, it should be understood that this description is illustrative only and that the illuminator of the present invention may be used in other types of surgery and in other environments than that described.
With reference to FIG. 1, the microsurgical illuminator 10 of the present invention is basically comprised of a handle 12, a cannula or probe tip 14 projecting from the handle, and a length of optic fiber 16 passing the handle and cannula and having a length extending from the handle.
The handle 12 is elongated and has opposite distal 18 and proximal 20 ends. A center bore 22 having a center axis extends through the interior of the handle between its opposite ends. The exterior surface 24 of the handle has a circumferential dimension approximately that of a pen or pencil providing a familiar and comfortable feel to the surgeon's hand when holding the handle. A portion 26 of the handle exterior surface is ribbed or grooved, providing a gripping surface.
The cannula or probe tip 14 is a rigid, tubular sleeve preferably constructed of surgical steel. As shown in FIG. 2, the tip also has an interior bore 28 having a center axis that coaxial with the center axis of the handle. A end 30 of the tip is received in the interior bore of the handle at the handle distal end and is securely held therein. The tip projects axially from the handle distal end 18 for a significant portion of its length to a distal end 32 of the tip. The distal end of the tip can best be seen in FIG. 2, and is formed with a beveled, flat annular surface 34 surrounding the center bore 28 of the tip. In the preferred embodiment of the invention, the flat annular surface 34 at the tip distal end lies in a plane positioned at an angle of 15° to a plane normal or perpendicular to the center axis of the tip. However, in variations of the tip distal end surface 34, the annular surface may be positioned at an angle to the normal plane ranging between 30° and 5°.
The optic fiber 16 employed in the preferred embodiment of the illuminator is a single strand optic fiber. The fiber has a significant length, and has opposite proximal 36 and distal 38 end surfaces at the opposite ends of its length. A flexible, insulating tubing 40 surrounds the fiber and extends along the fiber from a proximal end 42 of the tubing at the fiber proximal end 36, to a distal end 44 of the tubing that ends at the proximal end 30 of the cannula tip 14. The optic fiber 16 extends axially beyond the tubing distal end 44 through the interior of the cannula tip 14 to the distal end 38 of the fiber positioned at the cannula tip distal end 32. As best seen in FIG. 2, the optic fiber distal end 38 has a flat, beveled planar surface. The angle of the optic fiber distal end surface 38 corresponds to the angle of the flat annular surface 34 of the tip distal end. In the preferred embodiment, the distal end surface 38 of the optic fiber is oriented at an angle of 15° to a planar surface that is positioned normal or perpendicular to the center axis of the optic fiber and the center axis of the cannula tip. In alternate embodiments of the invention, the angle formed between the optic fiber distal end surface 38 and the planar surface normal or perpendicular to the fiber and tip center axis may range between 30° and 5°.
Although an annular spacing is shown between the exterior of the optic fiber distal end 38 and the interior bore 28 of the tip, it should be understood that FIG. 2 is enlarged many times and that in the preferred embodiment, the optic fiber will fit snug in friction engagement in the interior bore of the tip. The angular orientation of the optic fiber distal end surface 38 and the tip annular end surface 34 gives the cannula tip a projecting leading edge 46 that can be used to locate an incision made for the tip in the eye and to then insert the tip through the incision. This leading edge as well as the entire outer annular edge of the cannula tip is rounded or radiused to further decrease trauma to the eye associated with insertion.
The proximal end 36 of the optic fiber is secured in the center of a light source connector 48. The connector has a plug end 50 that may have an exterior configuration complimentary to a connecting socket 52 of a commercially available light source 54. There are many different available light sources 54 used in microsurgery, and the connector plug 50 can be altered so that the illuminator 10 of the invention may be used with any of these available light sources. As is conventional in light source connectors for optic fiber illuminators, the proximal end of the optic fiber 36 extends completely through the connector 48 and its end surface 36 is positioned in the same plane as the proximal end surface 56 of the connector plug 50.
With the light source turned on and the connector plug 50 inserted into the socket 52, the light emitted within the light source is transmitted through the optic fiber 16 to its distal end 38. The light is then emitted from the distal end 38 of the optic fiber and may be used to illuminate an area of surgery. The tip leading edge 46 may be used to locate an incision made in the eye for the tip and to insert the tip through the incision. It can be appreciated that by needing only to insert the leading edge 46 into the incision, use of the illuminator of the invention in inserting the cannula tip distal end into the incision is much more easily performed than inserting the flat, planar end surface of the optic fiber and annular tip as done in the prior art. Moreover, because the angle of the optic fiber distal end surface in the preferred embodiment is only 15°, it does not appreciably diffuse the light emitted from the surface.
While the present invention has been described by reference to a specific embodiment, it should be understood that modifications and variations of the invention may be constructed without departing from the scope of the invention defined in the following claims.
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A manually manipulated illuminator used in microsurgery comprises an optic fiber that transmits light through the instrument and emits the light through a beveled end surface of the fiber, the beveled end surface having a leading edge that facilitates insertion of the end surface through an incision.
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CROSS REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to U.S. application Ser. No. 10/933,922, filed Sep. 2, 2004; U.S. provisional application Ser. No. 60/505,337, filed Sep. 23, 2003; and to Swedish Patent Application No. 0302368.6, filed Sep. 3, 2003. The prior applications are incorporated herein by reference in their entirety.
TECHNICAL FIELD
[0002] The present invention relates to novel compounds, to pharmaceutical compositions comprising the compounds, to processes for their preparation, as well as to the use of the compounds for the preparation of a medicament against 5-HT 2A receptor-related disorders.
BACKGROUND
[0003] Many disorders and conditions of the central nervous system are influenced by the adrenergic, the dopaminergic, and the serotonergic neurotransmitter systems. For example, serotonin (5-HT; 5-hydroxytryptamine) has been implicated in a number of disorders and conditions which originate in the central nervous system.
[0004] The 5-HT 2A receptor has been implicated as a therapeutic target for the treatment or prevention of abnormalities of the serotonergic system, including psychotic disorders such as schizophrenia (A. Carlsson, N. Waters and M. L. Carlsson, Biol. Psychiatry, 46, 1388-1395 (1999); G. J. Marek and G. K. Aghajanian, Biol. Psychiatry, 44, 1118-1127 (1998); E. Sibelle, Z. Sarnyai, D. Benjamin, J. Gal, H. Baker and M. Toth, Mol. Pharmacol., 52, 1056-1063 (1997)). Abnormality of this system has also been implicated in a number of human diseases such as mental depression (Arias B, Gutierrez B, Pintor L, Gasto C, Fananas L, Mol. Psychiatry (2001) 6, 239-242), migraine, epilepsy and obsessive-compulsive disorder (Luisa de Angelis, Curr. Opin. Invest. Drugs (2002) 3 (1) 106-112). 5-HT 2A antagonists may also be useful in the treatment of sleep disorders such as insomnia and obstructive sleep apnea, anorexia nervosa (Ziegler A, Gorg T, Lancet (1999) 353, 929), cardiovascular conditions such as hypertension, vasospasm, angina, Raynaud's phenomenon and thrombotic illness including stroke, glaucoma (T. Mano et al. and H. Takaneka et al., Invest. Ophthamol. Vis. Sci., 1995, vol. 36, pages 719 and 734, respectively) and in the inhibition of platelet aggregation. Evidence also implies that selective 5-HT 2A receptor antagonists may also be useful in the treatment of alcohol and cocaine dependence (Maurel S, De Vry J, De Beun R, Schreiber, Pharmacol. Biochem Behav (1999) 89-96; McMahon L R, Cunningham K A, J. Pharmacol Exp Ther (2001) 297, 357-363).
[0005] No publications disclose the use of the compounds according to the present invention against 5-HT 2A receptor-related disorders.
SUMMARY
[0006] One object of the present invention is a compound of the Formula (I)
wherein
[0007] X is selected from aryl and heteroaryl, optionally independently substituted with one or more of C 1-6 -alkyl, C 1-6 -alkoxy, methylenedioxy, aryl, halogen, and halo-C 1-6 -alkyl;
[0008] Y is selected from C-Z and N;
[0009] Z is selected from hydrogen, C 1-6 -alkyl, C 1-6 -alkoxy, and halogen;
[0010] R 1 is either a group
wherein R 2 is either hydrogen; or C 2-6 -alkenyl, provided that o is 1; or aryl optionally independently substituted with one or more of C 1-6 -alkoxy, halogen, cyano, and methylenedioxy, provided that o is 1-3; or aryl-C 1-6 -alkyl provided that o is 0; or aryloxy optionally independently substituted with one or more of C 1-6 -alkoxy and halogen, provided that o is 2-3; or heteroaryl optionally independently substituted with one or more of C 1-6 -alkyl and C 1-6 -alkoxy; or heterocyclyl optionally independently substituted with one or more of C 1-6 -alkyl and C 1-6 -alkoxy;
[0020] m is 0 or 1;
[0021] n is 1 or2;
[0022] o is 0, 1, 2, or 3; or
[0023] R 1 is a group
wherein
[0024] R 3 is hydrogen or C 1-6 -alkyl;
[0025] R 4 is C 1-6 -alkyl, aryl optionally independently substituted with one or more of C 1-6 -alkyl and C 1-6 -alkoxy; or heteroaryl-C 1-6 -alkyl;
[0026] p is 0 or 1; and
[0027] pharmaceutically acceptable salts, hydrates, solvates, geometrical isomers, tautomers, optical isomers, and prodrug forms thereof.
[0028] It is preferred that X is selected from
phenyl, optionally independently substituted with one or more of methyl, methoxy, methylenedioxy, phenyl, chloro, fluoro, and trifluoromethyl; and thienyl.
[0031] It is even more preferred that X is selected from phenyl, 3-methylphenyl, 2-methoxyphenyl, 3-methoxyphenyl, 4-methoxyphenyl, 3,4-methylenedioxyphenyl, 1,1′-biphenyl-4-yl, 4-chlorophenyl, 4-fluorophenyl, 2-thienyl, and 4-trifluoromethylphenyl.
[0032] It is preferred that Z is selected from hydrogen, methyl, chloro, and methoxy.
[0033] It is preferred that R 2 is selected from
hydrogen; vinyl; indanyl; phenyl, optionally independently substituted with one or more of methyl, methoxy, bromo, fluoro, cyano, and methylenedioxy; phenylethyl; phenoxy, optionally independently substituted with one or more of methoxy, fluoro, chloro, and bromo; indolyl, optionally independently substituted with one or more of methoxy; thienyl; and hexahydro-1H-isoindole-1,3(2H)-dione.
[0043] It is even more preferred that R 2 is selected from hydrogen, vinyl, phenyl, 2-indanyl, 3-methylphenyl, 3,4,5-trimethoxyphenyl, 4-bromophenyl, 4-fluorophenyl, 1-phenylethyl, phenoxy, 2,6-dimethoxyphenoxy, 4-fluorophenoxy, 3-indolyl, 5-methoxy-3-indolyl, 2-thienyl, and hexahydro-1H-isoindole-1,3(2H)-dione.
[0044] It is preferred that m+n is 1 or 2.
[0045] It is preferred that R 3 is selected from hydrogen and methyl.
[0046] It is preferred that R 4 is selected from methyl, 2-indanyl, and 2-methyl-3-(3,4-methylenedioxyphenyl)-n-propyl.
[0047] Preferred compounds are given in Examples 1-40.
[0048] Another object of the present invention is a process for the preparation of a compound as mentioned above, which process comprises the following steps:
[0049] a) reaction of a compound of Formula (IV)
[0050] wherein
[0051] Y is selected from C—Z and N;
[0052] Z is selected from hydrogen, C 1-6 -alkyl, C 1-6 -alkoxy, and halogen;
[0053] with a Grignard reagent of Formula X—MgBr and then reduction with a reducing agent such as sodium borohydride
[0054] wherein
[0055] X is selected from aryl and heteroaryl, optionally independently substituted with one or more of C 1-6 -alkyl, C 1-6 -alkoxy, methylenedioxy, aryl, halogen, and halo-C 1-6 -alkyl;
[0056] to give a compound of Formula (V)
[0057] wherein X, Y, and Z are as defined above,
[0058] b) amidation_by reaction of the compound of Formula (V) with either a carboxylic acid of Formula (VI) or of Formula (VII) in the presence of a coupling agent such as carbonyldiimidazole
[0059] wherein
[0060] m is 0 or 1;
[0061] n is 1 or 2;
[0062] p is 0 or 1;
[0063] R 3 is hydrogen or C 1-6 -alkyl;
[0064] to give a compound of Formula (VIII) and (IX), respectively,
[0065] wherein X, Y, Z, m, n, p, and R 3 are as defined above,
[0066] c) cyclization of the compound of Formula (VEII) with phosphorous oxychloride or the compound of Formula (IX) with trifluoroacetic anhydride, respectively, to give a compound of Formula (X) or (XI), respectively,
[0067] wherein X, Y, Z, m, n, p, and R 3 are as defined above,
[0068] d) deprotection of the compound of Formula (X) or (XI), respectively, under acidic conditions, to give compounds of Formula (XII) or (XIII), respectively,
[0069] wherein X, Y, Z, m, n, p, and R 3 are as defined above; and, optionally, either of steps e) and f)
[0070] e) alkylation of the compound of Formula (XII) or (XIII), respectively, via displacement of a leaving group according to e1) and e2):
[0071] e1) reaction of the compound of Formula (XII) with an alkylating agent of the Formula R 2 —(CH 2 ) o -LG in the presence of a tertiary amine such as N-ethyldiisopropylamine, wherein R 2 is selected from C 2-6 -alkenyl, provided that o is 1; aryl optionally independently substituted with one or more of C 1-6 -alkyl, C 1-6 -alkoxy, halogen, cyano, and methylenedioxy, provided that o is 1-3; ary -C 1-6 -alkyl, provided that o is 0; aryloxy optionally independently substituted with one or more of C 1-6 -alkoxy and halogen, provided that o is 2-3; heteroaryl optionally independently substituted with one or more of C 1-6 -alkyl and C 1-6 -alkoxy; or heterocyclyl optionally independently substituted with one or more of C 1-6 -alkyl and C 1-6 -alkoxy, o is 0, 1, 2, or 3, and LG is a leaving group, to give a compound of Formula (XIV); or
[0072] e2) reaction of the compound of Formula (XIII) with an alkylating agent of the Formula R 4 -LG in the presence of a base (e.g., N-ethyldiisopropylamine), wherein R 4 is aryl optionally independently substituted with one or more of C 1-6 -alkyl and C 1-6 -alkoxy, or heteroaryl-C 1-6 -alkyl; and LG is as defined above, to give a compound of Formula (XV)
[0073] wherein X, Y, Z, m, n, o, p, R 2 , R 3 , and R 4 are as defined above;
[0074] f) alkylation of the compound of Formula (XII) or (XIII), respectively, via reductive amination according to f1) and f2):
[0075] f1) reaction of the compound of Formula (XII) with an aldehyde of the formula R 2 —(CH 2 ) q —CHO, wherein R 2 is as defined above and q is 1-2, acetophenone or 2-indanone then a reducing agent such as sodium triacetoxyborohydride, to give a compound of Formula (XIV); or
[0076] f2) reaction of the compound of Formula (XII) with an aldehyde of the formula R 5 —CHO, wherein R 5 is heteroaryl-C 1-6 -alkyl, preferably 1-methyl-2-(3,4-methylenedioxyphenyl)ethyl, or 2-indanone and then a reducing agent such as sodium triacetoxyborohydride, to give a compound of Formula (XV).
[0077] Another object of the present invention is a compound as mentioned above for use in therapy, especially for use in the prophylaxis or treatment of a 5-HT 2A receptor-related disorder.
[0078] Another object of the present invention is a pharmaceutical formulation comprising a compound as mentioned above as active ingredient, in combination with a pharmaceutically acceptable diluent or carrier, especially for use in the prophylaxis or treatment of a 5-HT 2A receptor-related disorder.
[0079] Another aspect of the present invention is a method for treating a human or animal subject suffering from a 5-HT 2A receptor-related disorder. The method can include administering to a subject (e.g., a human or an animal, dog, cat, horse, cow) in need thereof an effective amount of one or more compounds of any of the formulae herein, their salts, or compositions containing the compounds or salts.
[0080] The methods delineated herein can also include the step of identifying that the subject is in need of treatment of the 5-HT 2A receptor-related disorder. Identifying a subject in need of such treatment can be in the judgment of a subject or a health care professional and can be subjective (e.g., opinion) or objective (e.g., measurable by a test or diagnostic method).
[0081] Another object of the present invention is a method for the prophylaxis of a 5-HT 2A receptor-related disorder, which comprises administering to a subject in need of such treatment an effective amount of a compound as mentioned above.
[0082] Another object of the present invention is a method for modulating 5-HT 2A receptor activity, which comprises administering to a subject in need of such treatment an effective amount of a compound as mentioned above.
[0083] Another object of the present invention is the use of a compound as mentioned above for the manufacture of a medicament for use in the prophylaxis or treatment of a 5-HT 2A receptor-related disorder.
[0084] The compounds as mentioned above may be agonists, partial agonists or antagonists for the 5-HT 2A receptor. Preferably, the compounds of the present invention act as 5-HT 2A receptor antagonists. More preferably, the compounds of the present invention act as selective 5-HT 2A receptor antagonists.
[0085] Examples of 5-HT 2A receptor-related disorders are schizophrenia, mental depression, migraine, epilepsy, obsessive-compulsive disorder, sleep disorders such as insomnia and obstructive sleep apnea, anorexia nervosa, cardiovascular conditions such as hypertension, vasospasm, angina, Raynaud's phenomenon and thrombotic illness including stroke, glaucoma, alcohol and cocaine dependence.
[0086] The compounds and compositions are useful for treating diseases, including schizophrenia, mental depression, migraine, epilepsy, obsessive-compulsive disorder, sleep disorders such as insomnia and obstructive sleep apnea, anorexia nervosa, cardiovascular conditions such as hypertension, vasospasm, angina, Raynaud's phenomenon and thrombotic illness including stroke, glaucoma, alcohol and cocaine dependence. In one aspect, the invention relates to a method for treating or preventing an aforementioned disease comprising administrating to a subject in need of such treatment an effective amount of a compound or composition delineated herein.
[0087] The following definitions shall apply throughout the specification and the appended claims.
[0088] Unless otherwise stated or indicated, the term “C 1-6 -alkyl” denotes a straight or branched alkyl group having from 1 to 6 carbon atoms. Examples of said lower alkyl include methyl, ethyl, n-propyl, iso-propyl, n-butyl, iso-butyl, sec-butyl, t-butyl and straight- and branched-chain pentyl and hexyl. For parts of the range “C 1-6 -alkyl” all subgroups thereof are contemplated such as C 1-5 -alkyl, C 1-4 -alkyl, C 1-3 -alkyl, C 1-2 -alkyl, C 2-6 -alkyl, C 2-5 -alkyl, C 2-4 -alkyl, C 2-3 -alkyl, C 3-6 -alkyl, C 4-5 -alkyl, etc. “Halo-C 1-6 -alkyl” means a C 1-6 -alkyl group substituted with one or more halogen atoms. Likewise, “aryl-C 1-6 -alkyl” means a C 1-6 -alkyl group substituted with one or more aryl groups.
[0089] Unless otherwise stated or indicated, the term “C 1-6 alkoxy” denotes a straight or branched alkoxy group having from 1 to 6 carbon atoms. Examples of said lower alkoxy include methoxy, ethoxy, n-propoxy, iso-propoxy, n-butoxy, iso-butoxy, sec-butoxy, t-butoxy and straight- and branched-chain pentoxy and hexoxy. For parts of the range “C 1-6 -alkoxy” all subgroups thereof are contemplated such as C 1-5 -alkoxy, C 1-4 -alkoxy, C 1-3 -alkoxy, C 1-2 -alkoxy, C 2-6 -alkoxy, C 2-5 -alkoxy, C 2-4 -alkoxy, C 2-3 -alkoxy, C 3-6 -alkoxy, C 4-5 -alkoxy, etc.
[0090] Unless otherwise stated or indicated, the term “C 2-6 -alkenyl” denotes a straight or branched alkenyl group having from 2 to 6 carbon atoms. Examples of said alkenyl include vinyl, allyl, 1-butenyl, 1 -pentenyl, and 1-hexenyl. For parts of the range “C 2-6 -alkenyl” all subgroups thereof are contemplated such as C 2-5 -alkenyl, C 2-4 -alkenyl, C 2-3 -alkenyl, C 3-6 -alkenyl, C 3-5 -alkenyl, C 3-4 -alkenyl, C 4-6 -alkenyl, C 4-5 -alkenyl, etc.
[0091] Unless otherwise stated or indicated, the term “halogen” shall mean fluorine, chlorine, bromine or iodine.
[0092] Unless otherwise stated or indicated, the term “aryl” refers to a hydrocarbon ring system having at least one aromatic ring. Examples of aryls are phenyl, pentalenyl, indenyl, indanyl, isoindolinyl, chromanyl, naphthyl, fluorenyl, anthryl, phenanthryl and pyrenyl. The aryl rings may optionally be substituted with C 1-6 -alkyl. Examples of substituted aryl groups are 2-methylphenyl and 3-methylphenyl. Likewise, “aryloxy” refers to an aryl group bonded to an oxygen atom.
[0093] The term “heteroaryl” refers to a hydrocarbon ring system having at least one aromatic ring having one or more ring atoms that are a heteroatom such as O, N, or S, and the remaining ring atoms are carbon. Examples of heteroaryl groups include furyl, pyrrolyl, thienyl, oxazolyl, isoxazolyl, imidazolyl, thiazolyl, isothiazolyl, pyridinyl, pyrimidinyl, quinazolinyl, indolyl, pyrazolyl, pyridazinyl, quinolinyl, benzofuranyl, dihydrobenzofuranyl, benzodioxolyl, benzodioxinyl, benzothiazolyl, benzothiadiazolyl, and benzotriazolyl groups.
[0094] The term “heterocyclyl” refers to a hydrocarbon ring system containing 4 to 8 ring members that have at least one heteroatom (e.g., S, N, or O ) as part of the ring. It includes saturated, unsaturated, and nonaromatic heterocycles. Suitable heterocyclic groups include the above-mentioned heteroaryl groups, pyrrolidinyl, piperidyl, azepinyl, morpholinyl, thiomorpholinyl, pyranyl, dioxanyl, and hexahydro-1H-isoindole-1,3(2H)-dione groups.
[0095] The term “leaving group” refers to a group to be displaced from a molecule during a nucleophilic displacement reaction. Examples of leaving groups are bromide, chloride methanesulfonate, hydroxy, methoxy, thiomethoxy, tosyl, or suitable protonated forms thereof (e.g., H 2 O, MeOH), especially bromide and methanesulfonate.
[0096] The term “reducing agent” refers to a substance capable of reducing another substance and it itself is oxidized. Examples of reducing agents include, but are not limited to, hydrogen, sodium, potassium, sodium borohydride, sodium cyanoborohydride, sodium triacetoxyborohydride, lithium aluminiumhydride, and diisobutylaluminium hydride. “Coupling agent” refers to a substance capable of catalyzing a coupling reaction, such as amidation, or esterification. Examples of coupling agents include, but are not limited to, carbonyldiimidazole, dicyclohexylcarbodimide, pyridine, 4-dimethylaminopyridine, and triphenylphosphine.
[0097] “Acidic condition” refers to a reaction condition in which the reaction is carried out in the presence of a certain amount of acid. Examples of acids include, but are not limited to, inorganic acids, such as hydrogen chloride, hydrogen bromide, hydrogen iodide, sulfuric acid, nitric acid, phosphoric acid; and organic acids such as formic acid, acetic acid, propanoic acid, hydroxyacetic acid, lactic acid, pyruvic acid, glycolic acid, maleic acid, malonic acid, oxalic acid, benzenesulfonic acid, toluenesulfonic acid, methanesulfonic acid, trifluoroacetic acid, fumaric acid, succinic acid, malic acid, tartaric acid, citric acid, salicylic acid, p-aminosalicylic acid, pamoic acid, benzoic acid, ascorbic acid and the like. “Pharmaceutically acceptable” means being useful in preparing a pharmaceutical composition that is generally safe, non-toxic and neither biologically nor otherwise undesirable and includes being useful for veterinary use as well as human pharmaceutical use.
[0098] “Treatment” as used herein includes prophylaxis of the named disorder or condition, or amelioration or elimination of the disorder once it has been established.
[0099] “An effective amount” refers to an amount of a compound that confers a therapeutic effect on the treated subject. The therapeutic effect may be objective (i.e., measurable by some test or marker) or subjective (i.e., subject gives an indication of or feels an effect).
[0100] The term “prodrug forms” means a pharmacologically acceptable derivative, such as an ester or an amide, which derivative is biotransformed in the body to form the active drug. Reference is made to Goodman and Gilman's, The Pharmacological basis of Therapeutics, 8 th ed., Mc-Graw-Hill, Int. Ed. 1992, “Biotransformation of Drugs”, p. 13-15.
[0101] The following abbreviations have been used:
[0102] ACN means acetonitrile,
[0103] AP means atmospheric pressure chemical ionisation,
[0104] BOC means tert-butoxycarbonyl,
[0105] (Boc) 2 O means di-tert-butyl dicarbonate,
[0106] CDI means carbonyldiimidazole,
[0107] DCM means dichloromethane,
[0108] DEA means diethylamine,
[0109] DEPT means distortion enhancement polarization transfer,
[0110] DIBAL-H means diisobutylaluminium hydride,
[0111] DMF means dimethylformamide,
[0112] DMSO means dimethyl sulfoxide,
[0113] DPAT means dipropylaminotetraline,
[0114] HPLC means high performance liquid chromatography,
[0115] Hunig's base means N-ethyldiisopropylamine,
[0116] MIBK means methyl isobutylketone,
[0117] POCl 3 means phosphorous oxychloride,
[0118] QC means quality control
[0119] Rt means retention time,
[0120] TEA means triethylamine,
[0121] TFA means trifluoroacetic acid,
[0122] TFAA means trifluoroacetic anhydride,
[0123] THF means tetrahydrofuran,
[0124] TLC means thin layer chromatography.
[0125] All isomeric forms possible (pure enantiomers, diastereomers, tautomers, racemic mixtures and unequal mixtures of two enantiomers) for the compounds delineated are within the scope of the invention. Such compounds can also occur as cis- or trans-, E- or Z- double bond isomer forms. All isomeric forms are contemplated.
[0126] The compounds of the formula (I) may be used as such or, where appropriate, as pharmacologically acceptable salts (acid or base addition salts) thereof. The pharmacologically acceptable addition salts mentioned above are meant to comprise the therapeutically active non-toxic acid and base addition salt forms that the compounds are able to form. Compounds that have basic properties can be converted to their pharmaceutically acceptable acid addition salts by treating the base form with an appropriate acid. Exemplary acids include inorganic acids, such as hydrogen chloride, hydrogen bromide, hydrogen iodide, sulfuric acid, phosphoric acid; and organic acids such as formic acid, acetic acid, propanoic acid, hydroxyacetic acid, lactic acid, pyruvic acid, glycolic acid, maleic acid, malonic acid, oxalic acid, benzenesulfonic acid, toluenesulfonic acid, methanesulfonic acid, trifluoroacetic acid, fumaric acid, succinic acid, malic acid, tartaric acid, citric acid, salicylic acid, p-aminosalicylic acid, pamoic acid, benzoic acid, ascorbic acid and the like. Exemplary base addition salt forms are the sodium, potassium, calcium salts, and salts with pharmaceutically acceptable amines such as, for example, ammonia, alkylamines, benzathine, and amino acids, such as, e.g. arginine and lysine. The term addition salt as used herein also comprises solvates which the compounds and salts thereof are able to form, such as, for example, hydrates, alcoholates and the like.
[0127] For clinical use, the compounds of the invention are formulated into pharmaceutical formulations for oral, rectal, parenteral or other mode of administration. Pharmaceutical formulations are usually prepared by mixing the active substance, or a pharmaceutically acceptable salt thereof, with conventional pharmaceutical excipients. Examples of excipients are water, gelatin, gum arabicum, lactose, microcrystalline cellulose, starch, sodium starch glycolate, calcium hydrogen phosphate, magnesium stearate, talcum, colloidal silicon dioxide, and the like. Such formulations may also contain other pharmacologically active agents, and conventional additives, such as stabilizers, wetting agents, emulsifiers, flavouring agents, buffers, and the like.
[0128] The formulations can be further prepared by known methods such as granulation, compression, microencapsulation, spray coating, etc. The formulations may be prepared by conventional methods in the dosage form of tablets, capsules, granules, powders, syrups, suspensions, suppositories or injections. Liquid formulations may be prepared by dissolving or suspending the active substance in water or other suitable vehicles. Tablets and granules may be coated in a conventional manner.
[0129] In a further aspect the invention relates to methods of making compounds of any of the formulae herein comprising reacting any one or more of the compounds of the formulae delineated herein, including any processes delineated herein. The compounds of the formula (I) above may be prepared by, or in analogy with, conventional methods.
[0130] The processes described above may be carried out to give a compound of the invention in the form of a free base or as an acid addition salt. A pharmaceutically acceptable acid addition salt may be obtained by dissolving the free base in a suitable organic solvent and treating the solution with an acid, in accordance with conventional procedures for preparing acid addition salts from base compounds. Examples of addition salt forming acids are mentioned above.
[0131] The compounds of formula (I) may possess one or more chiral carbon atoms, and they may therefore be obtained in the form of optical isomers, e.g. as a pure enantiomer, or as a mixture of enantiomers (racemate) or as a mixture containing diastereomers. The separation of mixtures of optical isomers to obtain pure enantiomers is well known in the art and may, for example, be achieved by fractional crystallization of salts with optically active (chiral) acids or by chromatographic separation on chiral columns.
[0132] The chemicals used in the synthetic routes delineated herein may include, for example, solvents, reagents, catalysts, and protecting group and deprotecting group reagents. The methods described above may also additionally include steps, either before or after the steps described specifically herein, to add or remove suitable protecting groups in order to ultimately allow synthesis of the compounds. In addition, various synthetic steps may be performed in an alternate sequence or order to give the desired compounds. Synthetic chemistry transformations and protecting group methodologies (protection and deprotection) useful in synthesizing applicable compounds are known in the art and include, for example, those described in R. Larock, Comprehensive Organic Transformations , VCH Publishers (1989); T. W. Greene and P. G. M. Wuts, Protective Groups in Organic Synthesis, 3 rd Ed., John Wiley and Sons (1999); L. Fieser and M. Fieser, Fieser and Fieser's Reagents for Organic Synthesis , John Wiley and Sons (1994); and L. Paquette, ed., Encyclopedia of Reagents for Organic Synthesis , John Wiley and Sons (1995) and subsequent editions thereof.
[0133] The necessary starting materials for preparing the compounds of formula (I) are either known or may be prepared in analogy with the preparation of known compounds. The dose level and frequency of dosage of the specific compound will vary depending on a variety of factors including the potency of the specific compound employed, the metabolic stability and length of action of that compound, the patient's age, body weight, general health, sex, diet, mode and time of administration, rate of excretion, drug combination, the severity of the condition to be treated, and the patient undergoing therapy. The daily dosage may, for example, range from about 0.001 mg to about 100 mg per kilo of body_weight, administered singly or multiply in doses, e.g. from about 0.01 mg to about 25 mg each. Normally, such a dosage is given orally but parenteral administration may also be chosen.
[0134] The details of one or more embodiments of the invention are set forth in the accompanying drawings and the description below. Other features, objects, and advantages of the invention will be apparent from the description and drawings, and from the claims.
DETAILED DESCRIPTION
[0135] In the examples described below, all reagents were commercial grade and were used as received without further purification, unless otherwise specified. The chemicals were bought from Sigma-Aldrich (The old brickyard, New road, Gillingham, Dorset, SP8 4XT, UK), Lancaster (Eastgate, White Lund, Morecambe, Lancashire, LA3 3DY, UK), and Acros (Bishop Meadow road, Loughborough, leicestershire, LE11 5RG, UK). Commercially available anhydrous solvents were used for reactions conducted under inert atmosphere. Reagent grade solvents were used in all other cases, unless otherwise specified. Column chromatography was performed on Matrex® silica gel 60 (35-70 micron). TLC was carried out using pre-coated silica gel F-254 plates (thickness 0.25 mm). 1 H NMR spectra were recorded on a Bruker Avance250 at 250 MHz. Chemical shifts for 1 H NMR spectra are given in part per million and either tetramethylsilane (0.00 ppm) or residual solvent peaks were used as internal reference. Splitting patterns are designated as follows: s, singlet; d, doublet; t, triplet; q, quartet; p, pentet; m, multiplet; br, broad. Coupling constants are given in Hertz (Hz). Only selected data are reported. The 13 C NMR spectra were recorded at 62.5 MHz. DEPT experiments were used to help assign 13 C NMR resonances where necessary. Chemical shifts for 13 C NMR spectra are expressed in parts per million and residual solvent peaks were used as internal reference. HPLC analyses were performed using a Waters Xterra MS C18 column (100×4.6 mm, 5μ) eluting with a gradient of 5% ACN in 95% water to 95% ACN in 5% water (0.2% TFA buffer) over 3.5 mins, then 95% ACN in 5% water (0.2% TFA buffer) for a further 2.5 mins at a flow rate of 3 ml/min on a Waters 600E or Gilson system with monitoring at 254 nm. Reverse phase preparative HPLC was carried out using a Xterra MS C18 column (100×19 mm, 5 μm) eluting with a gradient of 5% ACN in 95% water to 95% ACN in 5% water (0.05% DEA) over 12.0 mins, then 95% ACN in 5% water (0.05% DEA) for a further 5.0 mins at a flow rate of 25 ml/min with monitoring at 254 nm. The fractions that contained the desired product were concentrated under reduced pressure and the resultant residue was lyophilised from a mixture of dioxane and water. Electrospray MS spectra were obtained on a Micromass platform LCMS spectrometer. Compounds were named using AutoNom 2000.
EXAMPLE 1
2-(3-{4-[1-(4-fluorophenyl)imidazo[1,5-a]pyridin-3-yl]piperidin-1-yl}propyl)hexahydro-1H-isoindole-1,3(2H)-dione
[0136] To a solution of the 1-(4-fluorophenyl)-3-piperidin-4-ylimidazo[1,5-a]pyridine (synthesized according to General procedure A; step 1-4) (157 mg, 0.53 mmol) and Hunig's base (276 μl, 0.58 mmol) in dry acetonitrile (12 ml) and dry methanol (1 ml) was added 3-(1,3-dioxooctahydro-2H-isoindol-2-yl)propyl methanesulfonate (167 mg, 0.58 mmol). The reaction mixture was heated to 100° C. for 18 hrs. The reaction mixture was evaporated and the crude was diluted with water and extracted with AcOEt. The organic layers were combined washed with brine, dried over MgSO 4 and concentrated. The residue was purified by flash chromatography on silica gel eluting with a mixture of AcOEt/methanol (10:0) to (9:1) and afforded the desired product (47 mg, 18%) as a brown solid.
[0137] 1 H-NMR (250 MHz, MeOD): 1.28-1.52 (m, 4H, CH), 1.68-1.98 (m, 5H, CH), 2.01-2.13 (m, 2H, CH), 2.14-2.19 (m, 3H, —CH), 2.41-2.49 (m, 2H, CH), 2.48-2.57 (m, 2H, CH), 2.76-2.92 (m, 2H, CH), 2.94-3.12 (m, 3H, CH), 3.39-3.57(m, 2H, CH), 6.55 (dd, 1H, J=7.5 Hz, J=5 Hz, Harom), 6.70 (dd, 1H, J=5 Hz, Harom), 7.02-7.18 (m, 2H, Harom), 7.63-7.86 (m, 4H, Harom), HPLC 100%, Rt=1.94 min. MS (AP) m/z 489.33 (M+H).
EXAMPLE 2 (GENERAL PROCEDURE A)
1-phenyl-3- [1-(2-phenylethyl)piperidin-4-yl]imidazo [1,5-al pyridine
[0138] Step 1
[0000] 1-Phenyl-1-pyridin-2-ylmethanamine
[0139] A solution of 2-cyanopyridine (1 g, 9.6 mmol) in dry toluene (30 mL) under nitrogen was cooled to 0° C. The phenylmagnesium bromide (3.53 ml, 10.6 mmol) was added dropwise over 30 min and the reaction mixture was warmed up to room temperature and stirred for 1 h. The reaction mixture was then cooled down to 0° C. and isobutanol (12 mL) was added dropwise keeping the temperature below 5° C. The reaction mixture was cooled to 0-5° C. and sodium borohydride (510 mg, 13.5 mmol) was added portionwise. The reaction mixture was allowed to warm up to room temperature and stirred overnight. The reaction mixture was quenched with methanol/water and concentrated in vacuo to remove the toluene. The mixture was extracted with DCM and the organic layers dried over magnesium sulphate were concentrated under vacuum to yield the desired amine as a yellow oil (2 g crude). The amine was used without further purification.
[0140] 1 H-NMR(250 MHz, CDCl 3 ) δ=2.33 (br, 2H, NH 2 ), 5.26 (s, 1H, CH), 7.12-7.61 (m, 8H, Harom), 8.58 (d, 1H, J=5 Hz, Harom). 13 C-NMR(62.5 MHz, DMSO-d 6 ) δ=61.0, 121.6, 121.9, 127.0, 127.2, 128.6, 136.6, 144.6, 149.1, 163.3. HPLC 92.7%, Rt=1.35 min. MS (AP) m/z 184.05 (M+H).
[0141] Step 2
[0000] 4-[(1-Phenyl-pyridin-2-yl-methyl)-carbamoyl]piperidine-1-carboxylic acid tert-butyl ester
[0142] To a stirred solution of Boc-isonipecotic acid (1.7 g, 13.8 mmol) in dry DCM (50 mL) was added a suspension of CDI (2.23 g, 13.8 mmol) in DCM (20 mL). The reaction mixture was stirred for 30 min. A solution of 1-phenyl-1-pyridin-2-ylmethanamine from Step 1 (1.7 g, 9.2 mmol) in dry DCM (50 mL) was then added and the reaction mixture was stirred overnight at room temperature. The reaction mixture was extracted with DCM, washed with water. The organic layers were combined and dried over magnesium sulphate then concentrated in vacuo to yield the desire amide as a yellow powder (3.3 g, 91%).
[0143] 1 H-NMR(250 MHz, CDCl 3 ) δ=1.46 (s, 9H, tBu), 1.55-1.75 (m, 2H, 2-CH), 1.79-1.93 (m, 2H, 2-CH), 2.31-2.39 (m, 1H, CH), 2.68-2.87 (m, 2H, 2-CH), 4.07-4.23 (m, 2H, 2-CH), 6.12 (d, 1H, J=7.5 Hz, CHNH), 7.17-7.32 (m, 6H, Harom), 7.62 (dt, 1H, J1=7.5 Hz, J2=2.5 Hz, Harom), 7.75 (brd, 1H, J1=7.5 Hz, Harom), 8.57 (dd, 1H, J1=5 Hz, J2=2.5 Hz Harom), HPLC 99%, Rt=1.97 min. MS (AP) m/z 396.19 (M+H).
[0144] Step 3
[0000] 4-(1-Phenyl-imidazo[1,5-a]pyridin-3-yl)-piperidine-1-carboxylic acid tert-butyl ester
[0145] To a cooled (ice/water) solution of the amide (300 mg, 0.76 mmol) and pyridine (380 μl, 4.7 mmol) in DCM (5 ml) was added dropwise POCl 3 (84 μl, 0.9 mmol). The reaction mixture was stirred overnight at room temperature. The mixture was washed with water and extracted with DCM. The organics were dried over magnesium sulfate and concentrated in vacuo to yield the desired cyclised product (257 mg, 89%). The compound was used without further purification.
[0146] 1 H-NMR(250 MHz, CDCl 3 ) δ=1.48 (s, 9H, tBu), 1.95-2.11 (m, 4H, 4-CH), 2.89-3.08 (m, 2H, 2-CH), 3.12-3.27 (m, 1H, CH), 4.25-4.38 (m, 2H, 2-CH), 6.53 (dt, 1H, J1=5 Hz, J2=2.5 Hz, Harom), 6.72 (dt, 1H, J1=5 Hz, J2=2.5 Hz, Harom), 7.43 (dt, 2H, J1=7.5 Hz, J2=2.5Hz Harom), 7.74 (dd, 2H, J1=7.5 Hz, J2=2.5 Hz, Harom), 7.85 (dd, 2H, J1=7.5 Hz, J2=2.5 Hz, Harom), 8.57 (brd, 1H, J=5 Hz, Harom), HPLC 100%, Rt=2.15 min. MS (AP) m/z 378.18 (M+H).
[0147] Step 4
[0000] 1-Phenyl-3-piperidine-4-yl-imidazo [1,5-a ]pyridine
[0148] To a solution of 4-(1-Phenyl-imidazo[1,5-a]pyridin-3-yl)-piperidine-1-carboxylic acid tert-butyl ester (1.0 g, 2.65 mmol) in dry methanol (1 ml) was added a 4M solution of HCl in dioxane (5.3 mL, 21.0 mmol). The reaction mixture was stirred for 4 hrs at room temperature. The solvent was removed in vacuo and the solid residue triturated with diethyl ether. The solid was removed by filtration and dried to give the amine hydrochloride. The compounds were stored as the HCl salt (831 mg, 100%).
[0149] 1 H-NMR(250 MHz, CDCl 3 ) δ=2.31-2.42 (m, 2H, 2-CH), 2.61-2.80 (m, 2H, 2-CH), 2.81-2.93 (m, 2H, 2-CH), 3.18-3.27 (m, 1H, CH), 3.51-3.70 (m, 2H, 2-CH), 6.51 (dt, 1H, J1=5 Hz, J2=2.5 Hz, Harom), 6.72 (dt, 1H, J1=5 Hz, J2=2.5 Hz, Harom), 7.44 (dt, 2H, J1=7.5 Hz, J2=2.5 Hz Harom), 7.81 (dd, 2H, J1=7.5 Hz, J2=2.5 Hz, Harom), 7.96 (dd, 2H, J1=7.5 Hz, J2=2.5 Hz, Harom), 8.57 (brd, 1H, J=5 Hz, Harom), HPLC 82%, Rt=1.47 min. MS (AP) m/z 278.12 (M+H).
[0150] Step 5
[0151] To a solution of 1-phenyl-3-piperidin-4-yl-imidazo [1,5-a]pyridine (365 mg, 1.32 mmol) and Hunig's base (574 μl, 3.3 mmol) in dry acetonitrile (10 ml) was added 2-(bromoethyl)benzene (150μl, 1.10 mmol). The reaction mixture was heated to 100° C. for 14hrs. The reaction mixture was evaporated and the crude product was diluted with water and extracted with AcOEt. The organic layers were combined washed with water, dried over MgSO 4 and concentrated. The residue was purified by flash chromatography on silica gel eluting with a mixture of hexane/AcOEt (3:7) to (0:10) followed by AcOEt/methanol (10:0) to (9:1) and afforded the desired compound (178 mg, 36%) as a yellow solid.
[0152] 1 H-NMR (250 MHz, CDCl 3 ): 2.28-2.41 (m, 2H, 2-CH), 2.73-2.89 (m, 2H, 2-CH), 3.17-3.38 (m, 5H, 5-CH), 3.62-3.84 (m, 4H, 4-CH), 6.62 (dd, 1H, J=7.5 Hz, J=2.5 Hz, Harom), 6.80 (dd, 1H, J=7.5 Hz, J=2.5 Hz, Harom), 7.28-7.36 (m, 6H, Harom), 7.48 (dd, 2H, J=7.5 Hz, J=2.5 Hz, Harom), 7.86 (dd, 4H, J1=7.5 Hz, J2=5 Hz, Harom), HPLC 100%, Rt=1.90 min. MS (AP) m/z 382.33 (M+H).
EXAMPLE 3
3-{1-[2-(4- fluorophenyl)ethyl]piperidin 4-yl}-1-(3-methoxyphenyl)imidazo[1,5-a]pyridine
[0153] To a solution of 1-(3-methoxy-phenyl)-3-piperidin-4-yl-imidazo [1,5-a]pyridine (synthesized according to General procedure A; step 1-4) (100 mg, 0.32 mmol) and Hunig's base (169 μl, 0.97 mmol) in dry acetonitrile (5 ml) and dry methanol (1 ml) was added methanesulfonic acid 2-(4-fluorophenyl)-ethyl ester (71 mg, 0.325 mmol). The reaction mixture was heated to 100° C. for 2 days. The reaction mixture was evaporated and the crude was diluted with water and extracted with AcOEt. The organic layers were combined washed with water, dried over MgSO 4 and concentrated. The residue was purified by flash chromatography on silica gel eluting with a mixture of hexane/AcOEt (3:7) to (0:10) followed by AcOEt/methanol (10:0) to (9:1) and afforded the desired product (14 mg, 10%) as a brown solid.
[0154] 1 H-NMR (250 MHz, MeOD): 0.81-0.93 (m, 4H, 2-CH 2 ), 1.63-1.76 (m, 4H, CH 2 ), 1.78-1.91 (m, 2H, CH 2 ), 2.07-2.19 (m, 1H, —CH), 2.18-2.27 (m, 2H, CH 2 ), 4.11 (s, 3H, OCH 3 ), 5.35 (dd, 1 H, J=7.5 Hz, Harom), 5.49 (dd, 2H, J=7.5 Hz, Harom), 5.65 (dd, 2H, 2Harom), ), 5.90-6.00 (m, 5H, 5Harom), 6.43 (d, 1H, J=7.5 Hz, Harom), 6.82-6.79 (d, 1H, J1=5 Hz, Harom), HPLC 98%, Rt=2.04 min. MS (AP) m/z 430.29 (M+H).
EXAMPLE 4
7-methyl-1-phenyl-3-[1-(2-phenylethyl)piperidin-4-yl]imidazo[1,5-a]pyridine
[0155] To a solution of 7-methyl-3-(piperidin-4-yl)-1-phenyl-imidazo[1,5-a]pyridine (synthesized according to General procedure A; step 1-4) (1 g, 3.43 mmol) and Hunig's base (3.59 ml, 20.6 mmol) in dry acetonitrile (10 ml) and dry methanol (2 ml) was added 2-(bromoethyl)benzene (468 μl, 3.43 mmol). The reaction mixture was heated to 100° C. over the weekend. The reaction mixture was evaporated and the crude was diluted with water and extracted with AcOEt. The organic layers were combined washed with water, dried over MgSO 4 and concentrated. The residue was purified by flash chromatography on silica gel eluting with a mixture of AcOEt/hexane (8:2) to (10:0) and afforded the desired product (25.2 mg, 2%) as a brown gum.
[0156] 1 H-NMR (250 MHz, MeOD): 1.72-1.89 (m, 2H, 2-CH), 1.90-2.04 (m, 2H, 2-CH), 2.05-2.22 (m, 2H, 2-CH), 2.34 (s, 3H, CH 3 ), 2.54-2.73 (m, 2H, 2-CH), 2.74-2.92 (m, 2H, 2-CH), 2.92-3.04 (m, 2H, 2-CH), 3.13-3.25 (m, 1H, 1-CH), 6.37 (d, 1H, J=7.5 Hz, Harom), 7.15-7.32 (m, 6H, 6Harom), 6.89 (dd, 2H, J=7.5 Hz, 2Harom), 7.52 (s, 1H, Harom), 7.74 (dd, 1H, J=7.5 Hz, Harom), 7.86 (dd, 2H, J1=7.5 Hz, J2=2.5Hz, Harom), HPLC 89%, Rt=1.97 min. MS (AP) m/z 396.32 (M+H).
EXAMPLE 5
1-(4-chlorophenyl)-3-[1-(2-phenylethyl)piperidin4-yl]imidazo[1,5-a]pyridine
[0157] To a solution of 1-(4-chloro-phenyl)-3-piperidin-4-yl-imidazo[1,5-a]pyridine (synthesized according to General procedure A; step 1-4) (100 mg, 0.32 mmol) and Hunig's base (140μl, 0.8 mmol) in dry acetonitrile (2 ml) and dry methanol (2 ml) was added 2-(bromoethyl)benzene (36.5μl, 0.267 mmol). The reaction mixture was heated to 100° C. for 18hrs. The reaction mixture was evaporated and the crude was diluted with water and extracted with AcOEt. The organic layers were combined washed with water, dried over MgSO 4 and concentrated. The residue was purified by flash chromatography on silica gel eluting with a mixture of hexane/AcOEt (3:7) to (0: 10) followed by AcOEt/methanol (10:0) to (9:1) and afforded the desired product (32 mg, 24%) as a brown solid.
[0158] 1 H-NMR (250 MHz, CDCl 3 ): 2.28-2.41 (m, 4H, 4-CH), 3.11-3.19 (m, 2H, 2-CH), 3.23-3.38 (m, 2H, 2-CH), 3.39-3.48 (m, 2H, 2-CH), 3.56-3.68 (m, 1H, CH), 3.72-3.86 (m, 2H, 2-CH), 6.72 (dd, 1H, J=7.5 Hz, Harom), 6.90 (dd, 1H, J=7.5 Hz, Harom), 7.21-7.36 (m, 5H, 5Harom), 7.48 (dd, 2H, J=7.5 Hz, Harom), 7.73-7.84 (m, 3H, 3Harom), 8.24 (d, 1H, J1=5 Hz, Harom), HPLC 96%, Rt=2.13 min. MS (AP) m/z 416.30 (M+H).
EXAMPLE 6
1-(4-methoxyphenyl)-3-[1-(2-phenylethyl)piperidin4-yl]imidazo[1,5-a]pyridine
[0159] To a solution of 1-(4-methoxyphenyl)-3-piperidin-4-ylimidazo[1,5-a]pyridine (synthesized according to General procedure A; step 1-4) (170 mg, 0.55 mmol) in dry acetonitrile (2 ml) was added Hunig's base (0.261 ml, 1.5 mmol) and 2-(bromoethyl)benzene (92.5 mg, 0.5 mmol). The reaction mixture was heated to reflux for two days. DCM (50 ml) was added and the solution washed with water (50 ml). The organic layers were combined, washed with brine, dried over MgSO 4 and concentrated. The residue was purified by flash chromatography on silica gel eluting with a mixture of methanol/AcOEt (1:9) and afforded the desired product (12.6 mg, 6%) as brown solid.
[0160] HPLC 99%, Rt=1.92 min. MS (AP) m/z 412.28 (M+H).
GENERAL PROCEDURE B FOR EXAMPLE 7-40 (LIBRARY COMPOUNDS)
DETAILS OF SYNTHESIS OF EXAMPLES 7-40
[0161] As mentioned above, the process for the preparation of the compounds is as follows:
Step A)—Synthesis Of Pyridinylmethylamines Of Formula (V)
[0162] The cyanopyridine of Formula (IV) (0.1 mol) was dissolved in dry toluene (300 ml) and cooled to 0-5° C. The Grignard reagent (0.11 mol) was added dropwise over 30 minutes to give a thick creamy precipitate. The reaction was stirred for a further 30 minutes at 0-5° C. then isobutanol (120 ml) was added dropwise keeping the temperature below 0-5° C. to give a clear brown solution. The reaction was cooled to 0-5° C. and sodium borohydride (0.14 mol) added portionwise and the whole stirred at room temperature overnight. The reaction was quenched with methanol/water and concentrated in vacuo to remove the toluene. The mixture was extracted with DCM and the organics dried over magnesium sulfate before concentrating in vacuo. Purification was carried out by flash column chromatography on silica eluted with ethyl acetate and ethyl acetate/3% TEA mixtures. An alternative purification involved dissolving the residue in diethyl ether and extraction into dilute HCl. The acidic solution was washed three times with diethyl ether and then basified with 1N sodium hydroxide and the product extracted with diethyl ether. The organics were dried over magnesium sulfate and concentrated in vacuo to yield the pyridinylmethylamine of Formula (V).
[0000] Step B)—Synthesis Of Amides Of Formula (VIII) And (IX)
[0163] The BOC protected amino acid of Formula (VI) or (VII) (15 mmol) was dissolved in dry DCM (25 ml) and CDI (15 mmol) added. The reaction was stirred for 30 minutes and then a solution of the pyridinylmethylamine of Formula (V) (15 mmol) in DCM (5 ml) was added. The mixture was stirred overnight. The solution was washed with water, dried over magnesium sulfate and concentrated in vacuo to yield the desired amide of Formula (VII) or (IX). The amide was used without further purification.
[0000] Step c)—Cyclization to Give the Imidazopyridine of Formula (X) or (XI)
[0164] For Cyclic Amino Acids POCl 3 (8.5 mmol) was added dropwise to a cooled (ice/water) solution of the amide of Formula (VIII) (7.2 mmol) and pyridine (44.5 mmol) in dry DCM (35 ml). The mixture was stirred overnight at room temperature. The mixture was washed with water (2×10 ml). The organics were dried over magnesium sulfate and concentrated in vacuo to yield the desired cyclised product of Formula (X). Purification was carried out by column chromatography on silica eluted with petrol:ethyl acetate
[0165] For Open Chain Amino Acids
[0166] The amide of Formula (IX) (2 mmol) was dissolved in dry DCM (10 ml) and pyridine (4 mmol) added. TFAA (2 mmol) was dissolved in dry DCM (2.5 ml) and added dropwise to the mixture at room temperature. The reaction was stirred for 1 h at room temperature. The mixture was washed with water (2×10 ml). The organics were dried over magnesium sulfate and concentrated in vacuo to yield the desired cyclised product of Formula (XI). Purification was carried out by column chromatography on silica eluted with petrol:ethyl acetate
[0000] Step d)—Deprotection to Give a Compound of Formula (XII) and (XIM
[0167] The BOC protected amine of Formula (X) or (XI) (8.86 mmol) was dissolved in (4N) methanolic HCl (15 ml) and stirred overnight at room temperature. The solvent was removed in vacuo and the solid residue triturated with diethyl ether. The solid was removed by filtration and dried to give the amine hydrochloride. The compounds were stored as the HCl salt and then converted to the free base of Formula (XII or (XIII) by aqueous sodium hydroxide for further reaction.
[0000] Step e)—Alkylation to Give an Amine of Formula (XIV) or (XV) Via Displacement of a Leaving Group
[0168] The free amine of Formula (XII) or (XIII) (0.2 mmol), alkylating agent (e g a bromide or methanesulfonate) (0.2 mmol) and Hunig's base (0.2 mmol) were heated in MIBK (2 ml) at 100° C. for 5 hours. The reaction was cooled and water added. The mixture was extracted with ethyl acetate (2×1 ml). The organics were dried over magnesium sulfate and concentrated in vacuo to yield the desired product of Formula (XIV) or (XV). Purification was carried out by automated preparative HPLC.
[0169] The reaction mixture was dissolved in DMSO (˜1.5 ml). This solution was loaded onto a 10 mm Xterra MS C 18 column at room temperature and eluted with the following gradient
Eluant A 0.05% DEA in water Eluant B 0.05% DEA in ACN min A B 0 95% 5% 1 95% 5% 6 5% 95% 10 5% 95% re-equilibrate to 95% A prior to next injection
[0170] Sample collection was triggered by U.V. absorbance, (thresholds set appropriated for the specific plates). The collected samples were analysed by LC-MS to ascertain the identity and purity of the constituents.
[0000] Step f)—Alkylation to Give an Amine of Formula (XIV) or (XV) Via Reductive Amination
[0171] The free amine of Formula (XII) or (XIII), aldehyde/ketone and sodium triacetoxyborohydride were mixed and shaken overnight at room temperature. The reaction was diluted with DCM, washed with IM sodium bicarbonate solution and then water. The aqueous phase was back extracted with DCM. The organics were combined and concentrated. Purification was carried out by automated preparative HPLC, to give a product of Formula (XIV) or (XIV).
EXAMPLE 7
1-(4-chlorophenyl)-7-methyl-3-piperidin4-ylimidazo[1,5-a]pyridine
[0172] Example 7 was synthesized according to general procedure B.
[0173] HPLC 96%, Rt=4.47 min. MS (AP) m/z 326 (M+H).
EXAMPLE 8
1-(3-methylphenyl)-3-[1-(2-phenylethyl)piperidin4-yl]imidazo[1,5-a]pyridine
[0174] Example 8 was synthesized according to general procedure B.
[0175] HPLC 88%, Rt=5.60 min. MS (AP) m/z 396 (M+H).
EXAMPLE 9
1-(2-methoxyphenyl)-3-[1-(2-phenylethyl)piperidin4-yl]imidazo[1,5-alpyridine
[0176] Example 9 was synthesized according to general procedure B.
[0177] HPLC 92%, Rt=5.09 min. MS (AP) m/z 412 (M+H).
EXAMPLE 10
3-{1-[2-(4-fluorophenyl)ethyl]piperidin4-yl}-1-(2-methoxyphenyl)imidazo[1,5a]pyridine
[0178] Example 10 was synthesized according to general procedure B.
[0179] HPLC 93%, Rt=5.15 min. MS (AP) m/z 430 (M+H).
EXAMPLE 11
7-chloro-1-(3-methoxyphenyl)-3-{1-[2-(3-methylphenyl)ethyl]piperidin4-yl}imidazo[1,5-a]pyridine
[0180] Example 11 was synthesized according to general procedure B.
[0181] HPLC 97%, Rt=6.07 min. MS (AP) m/z 461 (M+H).
EXAMPLE 12
1-(3-methoxyphenyl)-3-{1-[2-(2-thienyl)ethyl]piperidin4-yl}imidazo[1,5-a]pyridine
[0182] Example 12 was synthesized according to general procedure B.
[0183] HPLC 85%, Rt=5.34 min. MS (AP) m/z 418 (M+H).
EXAMPLE 13
7-chloro-3-[1-(2,3-dihydro-1 H-inden-2-yl)pyrrolidin-3-yl]-1-(4-methoxyphenyl)imidazo[1,5-a]pyridine
[0184] Example 13 was synthesized according to general procedure B.
[0185] HPLC 88%, Rt=5.55 min. MS (AP) m/z 444 (M+H).
EXAMPLE 14
3-{1-[2-(2,6dimethoxyphenoxy)ethyl]piperidin4-yl}-1-(4-fluorophenyl)imidazo[1,5-a]pyridine
[0186] Example 14 was synthesized according to general procedure B.
[0187] HPLC 90%, Rt=5.09 min. MS (AP) m/z 476 (M+H).
EXAMPLE 15
7-chloro-1-(3-methoxyphenyl)-3-[1-(2-phenylethyl)piperidin4-yl]imidazo[1, 5-a]pyridine
[0188] Example 15 was synthesized according to general procedure B.
[0189] HPLC 95%, Rt=5.78 min. MS (AP) m/z 446 (M+H).
EXAMPLE 16
3-[1-(4-chlorophenyl)imidazo[1,5-a]pyridin-3-yl]-N-methylpropan-1-amine
[0190] Example 16 was synthesized according to general procedure B.
[0191] HPLC 96%, Rt=4.12 min. MS (AP) m/z 300 (M+H).
EXAMPLE 17
3-(1-allylpiperidin-4-yl)-7-chloro-1-phenylimidazo[1,5-a]pyridine
[0192] Example 17 was synthesized according to general procedure B.
[0193] HPLC 97%, Rt=5.24 min. MS (AP) m/z 352 (M+H).
EXAMPLE 18
3-{1-[3-(4-fluorophenoxy)propyl]piperidin-3-yl}-1-(2-methoxyphenyl)imidazo[1,5-a]pyridine
[0194] Example 18 was synthesized according to general procedure B.
[0195] HPLC 92%, Rt=4.61 min. MS (AP) m/z 460 (M+H).
EXAMPLE 19
1-(4-fluorophenyl)-3-[1-(2-phenylethyl)piperidin4-yl]imidazo[1,5-a]pyridine
[0196] Example 19 was synthesized according to general procedure B.
[0197] HPLC 88%, Rt=5.39 min. MS (AP) m/z 400 (M+H).
EXAMPLE 20
1-(1,3-benzodioxol-5-yl)-7-chloro-3-{1-[2-(3,4,5-trimethoxyphenyl)ethyl]piperidin4-yl}imidazo[1,5-a]pyridine
[0198] Example 20 was synthesized according to general procedure B.
[0199] HPLC 96%, Rt=5.32 min. MS (AP) m/z 551 (M+H).
EXAMPLE 21
7-chloro-3-{1-[2-(1H-indol-3-yl)ethyl]piperidin-4-yl}-1-(3-methoxyphenyl)imidazo[1,5-alpyridine
[0200] Example 21 was synthesized according to general procedure B.
[0201] HPLC 94%, Rt=5.51 min. MS (AP) m/z 486 (M+H).
EXAMPLE 22
1-(3-methoxyphenyl)-3-[1-(3-phenylpropyl)pyrrolidin-3-yl]imidazo[1,5-a]pyridine
[0202] Example 22 was synthesized according to general procedure B.
[0203] HPLC 86%, Rt=5.78 min. MS (AP) m/z 412 (M+H).
EXAMPLE 23
3-{1-[2-(5-methoxy-1H-indol-3-yl)ethyl]piperidin4-yl}-1-(2-methoxyphenyl)imidazo[1,5-a]pyridine
[0204] Example 23 was synthesized according to general procedure B.
[0205] HPLC 88%, Rt=4.72 min. MS (AP) m/z 481 (M+H).
EXAMPLE 24
2,3-dihydro-1H-inden-2-yl(methyl){3-[1-(3-methylphenyl)imidazo[1,5-a]pyridin-3-yl]propyl}amine
[0206] Example 24 was synthesized according to general procedure B.
[0207] HPLC 93%, Rt=5.04 min. MS (AP) m/z 396 (M+H).
EXAMPLE 25
2,3-dihydro-1H-inden-2-yl{3-[1-(3-methoxyphenyl)imidazo[1,5-a]pyridin-3-yl]propyl}methylamine
[0208] Example 25 was synthesized according to general procedure B.
[0209] HPLC 95%, Rt=4.57 min. MS (AP) m/z 412 (M+H).
EXAMPLE 26
7-chloro-3-{1-[2-(4-fluorophenyl)ethyl]piperidin-4-yl}-1-(2-methoxyphenyl)imidazo[1,5-a]pyridine
[0210] Example 26 was synthesized according to general procedure B.
[0211] HPLC 98%, Rt=5.67 min. MS (AP) m/z 464 (M+H).
EXAMPLE 27
2,3-dihydro-1H-inden-2-yl{2-[1-(4-fluorophenyl)imidazo[1,5-a]pyrazin-3-yl]ethyl}methylamine
[0212] Example 27 was synthesized according to general procedure B.
[0213] HPLC 87%, Rt=3.68 min. MS (AP) m/z 387 (M+H).
EXAMPLE 28
3-(1,3-benzodioxol-5-yl)-N-{2-[1-(2-methoxyphenyl)imidazo[1,5-a]pyridin-3-yl]ethyl}-2-methylpropan-1-amine (racemic)
[0214] Example 28 was synthesized according to general procedure B.
[0215] HPLC 89%, Rt=5.15 min. MS (AP) m/z 444 (M+H).
EXAMPLE 29
2,3-dihydro-1H-inden-2-yl(methyl)[3-(1-phenylimidazo[1,5-a]pyridin-3-yl)propyl]amine
[0216] Example 29 was synthesized according to general procedure B.
[0217] HPLC 90%, Rt=4.65 min. MS (AP) m/z 382 (M+H).
EXAMPLE 30
1-(3-methylphenyl)-3-[1-(3-phenoxypropyl)piperidin-3-yl]imidazo[1,5-a]pyridine
[0218] Example 30 was synthesized according to general procedure B.
[0219] HPLC 98%, Rt=5.53 min. MS (AP) m/z 426 (M+H).
EXAMPLE 31
3-{1-[2-(4-bromophenyl)ethyl]piperidin4-yl}-7-methyl-1-phenylimidazo[1,5-a]pyridine
[0220] Example 31 was synthesized according to general procedure B.
[0221] HPLC 80%, Rt=6.05 min. MS (AP) m/z 474 (M+H).
EXAMPLE 32
1-(4-fluorophenyl)-3-[1-(1-phenylethyl)piperidin-4-yl]imidazo [1,5-a]pyridine (racemic) Example 32 was synthesized according to general procedure B.
[0222] HPLC 96%, Rt=5.58 min. MS (AP) m/z 400 (M+H).
EXAMPLE 33
3-(1-allylpiperidin-4-yl)-1-(4-chlorophenyl)imidazo[1,5-a]pyridine
[0223] Example 33 was synthesized according to general procedure B.
[0224] HPLC 97%, Rt=5.21 min. MS (AP) m/z 352 (M+H).
EXAMPLE 34
2-{2-[4-(1-biphenyl-4-ylimidazo[1,5-a]pyridin-3-yl)piperidin-1-yl]ethyl}hexahydro-1H-isoindole-1,3(2H)-dione
[0225] Example 34 was synthesized according to general procedure B.
[0226] HPLC 91%, Rt=5.84 min. MS (AP) m/z 533 (M+H).
EXAMPLE 35
3-[1-(2,3-dihydro-1H-inden-2-yl)pyrrolidin-3-yl]-1-(3-methoxyphenyl)imidazol1,5-a]pyridine
[0227] Example 35 was synthesized according to general procedure B.
[0228] HPLC 88%, Rt=5.65 min. MS (AP) m/z 410 (M+H).
EXAMPLE 36
3-[1-(3-phenylpropyl)piperidin-4-yl-1-(2-thienyl)imidazo[1,5-a]pyridine
[0229] Example 36 was synthesized according to general procedure B.
[0230] HPLC 96%, Rt=5.36 min. MS (AP) m/z 402 (M+H).
EXAMPLE 37
7-chloro-1-(2-methoxyphenyl)-3-{1-[2-(3,4,5-trimethoxyphenyl)ethyllpiperidin-4-yl}imidazo[1,5-a]pyridine
[0231] Example 37 was synthesized according to general procedure B.
[0232] HPLC 96%, Rt=5.28 min. MS (AP) m/z 537 (M+H).
EXAMPLE 38
1-(1,3-benzodioxol-5-yl)-7-chloro-3-{1-[2-(5-methoxy-1H-indol-3-yl)ethyl]piperidin-4-yl}imidazo[1,5-a]pyridine
[0233] Example 38 was synthesized according to general procedure B.
[0234] HPLC 96%, Rt=5.25 min. MS (AP) m/z 530 (M+H).
EXAMPLE 39
1-(1,3-benzodioxol-5-yl)-7-chloro-3-{1-[2-(2,6dimethoxyphenoxy)ethyl]piperidin4-yl}imidazo[1,5-a]pyridine
[0235] Example 39 was synthesized according to general procedure B.
[0236] HPLC 98%, Rt=5.41 min. MS (AP) m/z 537 (M+H).
EXAMPLE 40
1-(1,3-benzodioxol-5-yl)-3-{1-[2-(5-methoxy-1H-indol-3-yl)ethyl]piperidin4-yl}imidazo[1,5-a]pyridine
[0237] Example 40 was synthesized according to general procedure B.
[0238] HPLC 87%, Rt=4.83 min. MS (AP) m/z 495 (M+H).
EXAMPLE 41
[0239] Preparation of Tablets
Ingredients mg/tablet 1. Active compound of formula (I) 10.0 2. Cellulose, microcrystalline 57.0 3. Calcium hydrogen phosphate 15.0 4. Sodium starch glycolate 5.0 5. Silicon dioxide, colloidal 0.25 6. Magnesium stearate 0.75
[0240] The active ingredient 1 is mixed with ingredients 2, 3, 4 and 5 for about 10 minutes. The magnesium stearate is then added, and the resultant mixture is mixed for about 5 minutes and compressed into tablet form with or without film-coating.
[0241] Primary screening and IC 50 determination
[0242] CHO cells expressing 5-HT 2A receptors seeded in 384 well plates are pre-loaded with Fluo-4AM fluorescent dye and then incubated with compound (10 μM for primary screen) for 15 min. Fluorescent intensity is recorded using a Fluorometric imaging plate reader (FLIPR384, Molecular Devices) and inhibition of the peak response evoked by 5-HT (EC 70 concentration) is calculated.
[0243] IC 50 determinations are performed utilizing the same finctional assay as described for primary screening (15 min antagonist compound pre-incubation), applying the compounds in the dose range of 3 nM to 10 μM.
[0244] In Vitro Receptor Pharmacology—Selectivity Determinations
[0245] The affinity constants of compounds were determined using recombinant human serotonin receptors stably expressed in fibroblast cell lines (CHO or HEK293), measuring the ability of the compounds to displace radio-labelled tracers using scintillation proximity assays or filter binding assays. For 5-HT 1B , 5-HT 2B and 5-HT 2C receptor binding studies 3 H-LSD was used as radio ligand, for 5-HT 2 A and 5-HT 6 3 H-5-HT was used as tracer, while the binding constant to 5-HT 1A was determined using 3 H-8-OH-DPAT. The non-selective serotonin receptor antagonist mianserine was used as reference substance.
[0246] The activity at 5-HT 2C receptors was studied in a FLIPR based assay, measuring the effect of compounds on 10 nM 5-HT induced Ca 2+ -currents.
[0000] Biology Summary
[0247] The calculation of the K i values for the inhibitors was performed by use of Activity Base. The Ki value is calculated from IC 50 using the Cheng Prushoff equation (with reversible inhibition that follows the Michaelis-Menten equation): K i =IC 50 (1+[S]/K m ) [Cheng, Y. C.; Prushoff, W. H. Biochem. Pharmacol. 1973, 22, 3099-3108]. The compounds of formula (1) exhibit IC 50 values for the 5-HT2A receptor in the range from 1 nM to 10 μM.
[0248] Seven 5-HT 2A antagonist lead compounds were identified in FLIPR-based functional screening of the 5-HT 2A receptor. Four of these compounds were tested in equilibrium displacement binding measurements. The results of this study show that Example 2 and Example 4 are high affinity ligands for the 5-HT 2A receptor subtype, with K i values of 6 and 14, respectively (n=3). Both these compounds appear to be at least 20 fold selective over five other serotonin receptors assayed (5-HT 2C , 5-HT 2B , 5-HT 1A , 5-HT 6 and 5-HT 1B ). Furthermore, Example 2 and Example 4 appear highly selective at 5-HT 2A versus the 5-HT 2C receptor in terms of efficacy. Reversibility of inhibition of the 5-HT 2A response was demonstrated for all compounds tested.
Functional K i (nM) Binding K i (nM) Example 5-HT 2A 5-HT 1A 5-HT 1B 5-HT 2A 5-HT 2B 5-HT 2C 5-HT 6 Example 2 20.6 >1000 >1000 5.9 444 >1000 >1000 Example 4 8.2 >1000 >1000 13.6 267 >1000 >1000
[0249] The table shows the selectivity of two example compounds for the 5-HT2A over other serotonin-binding receptors.
[0250] A number of embodiments of the invention have been described. Nevertheless, it will be understood that various modifications may be made without departing from the spirit and scope of the invention. Accordingly, other embodiments are within the scope of the following claims.
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Compounds of Formula (I):
wherein X, Y, Z, and R 1 are as described herein, processes for preparing the compounds, pharmaceutical compositions comprising the compounds, and use of the compounds and compositions in the prophylaxis or treatment of a 5-HT 2A receptor-related disorder.
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BACKGROUND OF THE INVENTION
[0001] The present invention relates to a derivate of the isothiazolinone, especially to a alkoxylpropylisothiazolinone compound, a preparing method thereof, and applications thereof for preparing marine antifouling coating and for using as bactericide.
[0002] Various marine organisms are adhered to the surfaces of the fishing nets, hull, underwater facilities and the like which were socked in seawater for a long period, and the adhesion of the marine organisms may cause the surfaces defiled, increase surface friction force, and accelerate its erode. The most general method of solving the problem of marine organisms defilement is to coat a coating having antifouling agent. Currently, a antifouling coating comprising organic tin and cuprous oxide are used widely all over the world, namely, a combination of a copolymer of the tributyltin methacrylate and methyl methacrylate and cuprous oxide (Cu 2 O) is used as an antifouling coating to coat the surfaces of the hull bottom and the like, so as to prevent effectively the harm of the marine organisms. The action mechanism thereof lies in a controlled releasing of the toxinic tributyltin oxide (TBT) and cuprous oxide which has exterminate function to the harmful adhesive substance such as barnacle, ascidian, seaweed and the like which tend to adhere to the surfaces of the hull and marine facilities. But, TBT can also cause sex variation and shell aberration of oyster, boold clam and mussel, and thus may damage severely the marine ecological environment and the marine aquiculture industry. The most noted self-polishing antifouling coating containing TBT is disclosed in EP-A-51930 which is a landmark in the exposure of the TBT copolymer. Thereafter, TBT antifouling coating occupied the antifouling coating market over 20 years. People began to realize that the organic tin compounds have so strong toxicity that they can pollute environment, even influence human health via food chain, till 1987. Due to such reason, it is required to develop a marine antifouling coating free of tin to replace the organic tin marine antifouling coating.
[0003] Furthermore, the antiseptics used in current market are various. They may be classified into chlorine-based antiseptic, triazole-based antiseptic and the like. But these antiseptics can cause some problems more or less during using. For example, while the quaternary ammonium salt-based antiseptics have extensive and highly effective sterilization ability, they also have disadvantages such as a high cost, apt to generate foam, and a drug resistance may be generated if they were used alone for a long time. Furthermore, the sterilization ability of such kind of antiseptic may decrease if they are used in water with higher hardness. Other kinds of antiseptics may have features of high toxicity, high residual and the like. However, our government has carried out various active means to cope with the high toxicity, high residual antiseptics, and has inhibited and restricted the vendition and employment thereof specifically. Accordingly, the nuisance-free antiseptics that have high efficiency, low toxicity, low residual or no residual toxicity are required urgently to be developed.
SUMMARY OF THE INVENTION
[0004] An object of the present invention is to provide an alkoxylpropylisothiazolinone, which is applied to prepare marine antifouling coating and antiseptics to compensate the demand mentioned above in prior art, and a preparation method thereof.
[0005] In order to achieve the object mentioned above, technical solutions used in the present invention are as follows:
[0006] An alkoxylpropylisothiazolinone, the molecular formula thereof is C 6 H 6 Cl 2 NO 2 SR, and the formula thereof is:
wherein, R is CH 3 , CH 2 CH 3 , CH(CH 3 ) 2 , CH 2 CH 2 CH 2 CH 3 , CH 2 CH 2 OCH 3 or CH 2 CH 2 OC 6 H 5 Cl.
[0007] The preparation method of the alkoxylpropylisothiazolinone comprises the following steps: reacting sodium polysulphide with methyl acrylate to obtain dimethyl dithiodipropionate, followed by aminolysis with alkoxyl propylamine to obtain N,N′-dialkoxylpropyldithio-dipropionamide, which is then reacted with sulfuric chloride to obtain the alkoxylpropyl-isothiazolinone.
[0008] In the preparation method of the alkoxylpropylisothiazolinone, the alkoxylpropylisothiazolinone is 4,5-dichloro-2-methoxypropyl-4-isothiazolin-3-one, 4,5-dichloro-2-ethoxypropyl-4-isothiazolin-3-one, 4,5-dichloro-2-isopropoxy-propyl-4-isothiazolin-3 -one, 4,5-dichloro-2-butoxypropyl-4-isothiazolin-3-one, 4,5-dichloro-2-methoxyethoxypropyl-4-isothiazolin-3-one or 4,5-dichloro-2-chlorophenoxyethoxypropyl-4-isothiazolin-3-one.
[0009] In the preparation method of the alkoxylpropylisothiazolinone, the alkoxylpropylamine is γ-methoxypropylamine, γ-ethoxypropylamine, γ-isopropoxypropylamine, γ-butoxypropylamine, γ-methoxyethoxypropylamine or γ-phenoxyethoxypropylamine.
[0010] The alkoxylpropylisothiazolinone of the present invention is used for preparation of marine antifouling coating.
[0011] The marine antifouling coating of the present invention is comprised of resin solution, plasticizer, one or more filler and one or more alkoxylpropylisothiazolinones of the present invention with the percent by weight of 20-60, 1-20, 1-30 and 1-50, respectively, wherein the resin of the resin solution is one or more selected from acrylic resin, chlorinated rubber, zinc acrylate resin and copper acrylate resin, the solvent is one or more selected from ethyl acetate, butyl acetate, xylene, toluene and butanol, and the concentration of the resin solution is in the range of 20%-60%.
[0012] The alkoxylpropylisothiazolinone of the present invention may be used as an antiseptic.
[0013] The application of the alkoxylpropylisothiazolinone that used as an antiseptic, wherein, the septic is staphylococcus aureus , coliform bacteria, or saccharomyces cerevisiae.
[0014] The alkoxylpropylisothiazolinone of the present invention may be used as an antiseptic for industrial cooling water.
[0015] The alkoxylpropylisothiazolinone of the present invention may be used as an antiseptic for the agricultural use.
[0016] The merits of the present invention is that the marine coating prepared with alkoxylpropylisothiazolinone of the present invention as the antifouling agent can be degraded and separated rapidly in the environment, and has limited bioavailability to the marine organisms with a little of accumulation in vivo organisms. It has significant antifouling efficiency and a longer lifespan. The preparation of such compound has merits of available raw material, low cost and a higher yield. When using as an antiseptic, the compound of the present invention has many merits such as high efficiency, broad spectrum, low toxicity, low residual and the like. The compound of the present invention can be degraded rapidly in the environment due to their bioactivity, with low toxicity or nontoxicity substance releasing, thus may not render the environment pollution.
DETAILED DESCRIPTION OF THE INVENTION
[0000] 1. Preparation of Dimethyl Dithiodipropionate
[0017] In a 500 ml three neck flask equipped with a stirrer, a condenser and a thermometer, 200 ml 10% (percentage by weight, hereinafter is the same) NaHCO 3 solution and 21.7 g (0.25 mol) methyl acrylate were added sequentially, then the system was cooled to −5-10° C. Keeping under the temperature, a cooling sodium polysulphide (0.19 mol, counted by Na 2 S) solution was dropped during 0.5-2 hours. After the dropwise addition, ice water bath was removed. The mixture was left standing under the room temperature for 5-6 hours. Then the reaction was over. The obtained mixture was allowed to stand and separate into two layers. The water layer was removed. A 120 ml (1 mol/L) Na 2 SO 3 solution was added to the oil layer. The mixture then reacted continuously for 2-5 hours under the temperature of 50° C. until the reaction was over. The resulting mixture was again allowed to stand and separate into layers. Then the water layer was removed, and the oil layer was washed with water. 26.8 g light yellow oily substance was obtained by vacuum distilling, the yield is 89.3%, the boiling point is 182-185° C./7 mmHg.
[0000] 2. Preparation of N,N′-Dimethoxylpropyldithiodipropionamide
[0018] In a 500 ml three neck flask equipped with a stirrer, a condenser and a thermometer, 26.7 g (0.3 mol) γ-methoxypropylamine, 2.5 ml triethylamine are added sequentially, the temperature of the reaction system was controlled to −5-5° C. and maintained. Then 23.8 g (0.1 mol) β-dimethyl dithiodipropionate prepared by the front step was dropped during 0.5-1.5 hours. After dropwise addition, the ice water bath was removed. The reaction was left standing for 24 hours under the room temperature, and then the reaction was over. A golden solid was obtained. And a light yellow solid product was yielded by vacuum filtration. After dried it was recrystallized with anhydrous alcohol. 24.1 g white chip crystal was obtained, and the yield is 68.4%, the boiling point is 103.3-105.1° C.
[0019] N,N′-diethoxylpropyldithiodipropionamide, N,N′-diisopropoxydithiodipropionamide, N,N′-dibutoxypropyldithiodipropionamide, N,N′-dimethoxyethoxypropyldithiodipropionamide or N,N′-diphenoxyethoxypropyldithiodipropionamide can be obtained, respectively, when the γ-methoxypropylamine in the embodiment is replaced with γ-ethoxypropylamine, γ-isopropoxypropylamine, γ-butoxypropylamine, methoxyethoxypropylamine or γ-phenoxyethoxypropyl-amine.
[0000] 3. Preparation of 4,5-Dichloro-2-Methoxypropyl-4-Isothiazolin-3-One
[0020] In a 250 ml three neck flask equipped with a stirrer, a condenser and a thermometer, 175 ml ethyl acetate and 18.0 g (0.05 mol) N,N′-diethoxylpropyldithiodipropionamide are added sequentially. Keeping the temperature of the system to −10-5° C., 40.0 g (0.3 mol) sulfuric chloride was dropped during 3 hours. The reaction is kept to be continued for 3 hours under the temperature, and then the temperature of the reaction system was raised slowly to the room temperature. The mixture was allowed to react for another 3 hours in the water bath under the temperature of 30-35° C. until the reaction was over. The resulting solution was added 50 ml water and then oscillated for 3 minutes. The resulting mixture was allowed to stand and separated to two layers. The organic phase was dried over anhydrous magnesium sulfate (15.0 g) for 15 minutes, and then filtrated. The solvent was removed from the filtrate by decompression via spin-evaporimeter. 15.4 g yellow thick liquid was obtained, the primary yield is 63.9%, the yield of the pure product separated by column is 56.6%.
[0021] 4,5-dichloro-2-ethoxylpropyl-4-isothiazolin-3-one, 4,5-dichloro-2-isopropoxy propyl-4-isothiazolin-3-one, 4,5-dichloro-2-butoxypropyl-4-isothiazolin-3-one, 4,5-dichloro-2-methoxyethoxypropyl-4-isothiazolin-3-one, or 4,5-dichloro-2-phenoxyethoxypropyl-4-isothiazolin-3-one can be obtained respectively, when the N,N′-dimethoxylpropyldithiodipropionamide in the embodiment is replaced with N,N′-diethoxylpropyldithiodipropionamide, N,N′-isopropoxypropyldithiodipropionamide, N,N′-diisopropoxydithiodipropionamide, N,N′-dibutoxypropyldithiodipropionamide, N,N′-dimethoxyethoxy propyldithiodipropionamide or N,N′-diphenoxyethoxy propyldithiodipropionamide.
[0022] The resulting product is characterized by nuclear magnetic resonance ( 1 H NMR) method. The characteristic peak thereof is shown in the following table:
compound Solvent H atom serial number δvalue Peak shape CDCl 3 1 2 3 4 5 3.3506 3.4147 1.9839 3.9073 6.2644 S T M T S CDCl 3 1 2, 3 4 5 1.2139 3.4662 1.9759 3.9243 T M M T CDCl 3 1, 2 3 4 5 6 1.1683 3.5661 3.4531 1.9593 3.9195 D M T M T CDCl 3 1 2 3 4, 5 6 7 0.9327 1.3899 1.5688 3.4354 1.9723 3.9165 T M M M M T CDCl 3 1 2 3 4 5 6 3.3970 3.5160 3.5569 3.5929 2.0046 3.9243 S T M M M T CDCl 3 1 2 3 4 5 6, 10 7, 9 4.1121 1.9820 3.7915 3.8571 3.8342 6.8591 7.2409 T M M M M M T
INDUSTRIAL APPLICATION
[0023] The alkoxylpropylisothiazolinone is used as antifouling for preparation of the marine antifouling coating:
[0024] The compound of the present invention is used for preparation of the marine antifouling coating which is comprised of resin solution, plasticizer, one or more filler and one or more compound of the present invention in the percent by weight of 20-60, 1-20, 1-30 and 1-50. Wherein the concentration range of the resin solution is 20%-60% (percentage by weight, hereinafter is the same). The acrylic resin solution which has film forming function such as chlorinated rubber solution, zinc acrylate resin solution and copper acrylate resin solution can be used; the solvent may be ethyl acetate, butyl acetate, xylene, toluene and butanol; the plasticizer may be vaseline, clorafin, dibutyl phthalate or dioctyl phthalate; the filler may be red iron oxide, talcum powder, titanium dioxide, gas phased silicon dioxide or zinc oxide. The antifouling coating of the present invension is prepared as follows: a mixture of 50 g acrylic resin in butyl acetate solution with the concentration of 40%, 2.5 g clorafin, 12 g red iron oxide, 2.5 g gas phase silicon dioxide, 33 g 4,5-dichloro-2-dibutoxy-propyl-4-isothiazolin-3-one was oscillated for 2 hours in the beaded paint oscillator having a glass bead, then the mixture was filtrated by a filter with 100 screen mesh. To measure the antifouling performance of the resulting antifouling coating, referring to Chinese National Standard “Testing method of the antifouling coating sample board socked in the shallow sea” (GB 5370-85), the obtained antifouling coating was coated on the mild steel testing sample board, with length of 250 mm, width of 150 mm, thickness of 2 mm, and the board was held by rectangular batten having grooves fixed with iron bolt at its both ends. The testing sample board was hung at the submerged cages culture area of Xunshan town in Rongcheng city for 2 years. A significant experimental result was achieved, as shown in the following table.
6 months 12 months 24 months blank sample board 20 40 100 sample board coated with 0 0 3 antifouling coating Note: 0, 3, 20, 40, 100 represent the adhesion area percent of the marine organisms on the sample boards.
The alkoxylpropylisothiazolinone of the present invention used as antiseptic:
[0025] The lowest bacteriostasis concentration of the six kinds of the alkoxylpropylisothiazolinone of the present invention is measured through the tube double dilution method. In a Φ18×180 mm tube, 5 ml aseptic culture medium was added, then 50 μl bacteria suspended liquid of coliform was injected to prepare culture solution of beef extract peptone having bacteria concentration of 10 7 cfu/ml, then 50 μl tetrahydrofuran solution containing 4,5-dichloro-2-isopropoxypropyl-4-isothiazolin-3-one with the concentration of 2 μg/ml, 4 μg/ml, 8 μg/ml, 16 μg/ml, 32 μg/ml were added respectively. After cultured for 24 hours under a constant temperature of 37° C., the lowest bacteriostasis concentration of 4,5-dichloro-2-isopropoxypropyl-4-isothiazolin-3-one against coliform bacteria was measured. The result is 8 μg/ml (the cfu is a colong forming unit, 1 cfu refer to one single colong formed on the agar plate after being cultured).
[0026] When the coliform bacteria of the present invention is replaced with saccharomyces cerevisiae or staphylococcus aureus , and the 4,5-dichloro-2-isopropoxypropyl-4-isothiazolin-3-one is replaced with 4,5-dichloro-2-methoxy-propyl-4-isothiazolin-3-one, 4,5-dichloro-2-ethoxypropyl-4-isothiazolin-3-one, 4,5-dichloro-2-butoxypropyl-4-isothiazolin-3-one, 4,5-dichloro-2-methoxyethoxypropyl-4-isothiazolin-3-one, or 4,5-dichloro-2-chlorophenoxyethoxypropyl-4-isothiazolin-3-one, a considerable experimental results are also received, which are shown in the following table.
[0027] The lowest bacteriostasis concentration of six kinds of alkoxylpropyliso-thiazolinone (unit:μg/ml)
staphylococcus coliform saccharomyces compound aureus bacteria cerevisiae 4,5-dichloro-2- 32 4 16 methoxypropyl-4- isothiazolin-3-one 4,5-dichloro-2-ethoxypropyl- 16 4 8 4-isothiazolin-3-one 4,5-dichloro-2- 16 8 8 isopropoxypropyl-4- isothiazolin-3-one 4,5-dichloro-2-butoxypropyl- 8 4 4 4-isothiazolin-3-one 4,5-dichloro-2- 16 16 16 methoxyethoxypropyl-4- isothiazolin-3-one 4,5-dichloro-2- 16 8 8 chlorophenoxy- ethoxypropyl-4-isothiazolin-3- one
[0028] The compound of the present invention may be used to control and sterilize alga, fungi and bacteria in the industrial cooling water system. First, chlorine was stopped adding into the circulating water system for 3 days before administration. The total amount of the heterotrophic bacteria in the circulating water was raised, and then the 4,5-dichloro-2-methoxyethoxypropyl-4-isothiazolin-3-one was thrown in, while the discharge of the water was stopped. The amount of the heterotrophic bacteria in water and the sterilization rate was measured at 4 hours, 12 hours, 24 hours, 36 hours after the medicament was added. The test result is shown in the following table. It indicates that the compound of the present invention can control and sterilize effectively the heterotrophic bacteria in the industry cooling water water.
the amount of the the heterotrophic the rate concentration bacteria (number/mL) of the time of of the the request of steriliza- sterilization medicament standardization tion (h) (mg/L) design virtual result % before the 0 5 × 10 5 3.0 × 10 7 0 medicament is added 4 50 5 × 10 5 2.0 × 10 5 99.33 12 50 5 × 10 5 4.0 × 10 4 99.87 24 50 5 × 10 5 3.0 × 10 4 99.90 36 50 5 × 10 5 3.3 × 10 4 99.89
[0029] When the 4,5-dichloro-2-methoxyethoxypropyl-4-isothiazolin-3-one of the present embodiment is replaced with 4,5-dichloro-2-methoxylpropyl-4-isothiazolin-3-one, 4,5-dichloro-2-ethoxylpropyl-4-isothiazolin-3-one, 4,5-dichloro-2-isopropoxy-propyl-4-isothiazolin-3-one, 4,5-dichloro-2-butoxypropyl-4-isothiazolin-3-one or 4,5-dichloro-2-phenoxyethoxypropyl-4-isothiazolin-3-one, the microorganism in industry cooling water can also be controlled and sterilized effectively.
[0030] Through the measurememt of drug action and field test, the alkoxylpropylisothiazolinone of the present invention is proved to have considerable sterilization and prophylaxis function to wheat scab and leaf spot of beet. Otherwise, it has also a good prevent function to the apple ring rot, tomato gray mold and cotton soreshin. For example, when the 4,5-dichloro-2-isopropoxypropyl-4-isothiazolin-3-one is used as bactericide, it is merely required 39 g pure medicament per mu ( 1/15 of a hectare) with the concentration of 250 ppm to control the leaf spot of bee, and the efficiency of the prevention and cure is up to 75.0%.
[0031] When the 4,5-dichloro-2-butoxypropyl-4-isothiazolin-3-one of the present embodiment is replaced with 4,5-dichloro-2-dimethoxyethoxypropyl-4-isothiazolin-3-one, 4,5-dichloro-2-ethoxylpropyl-4-isothiazolin-3-one, 4,5-dichloro-2-isopropoxy-propyl-4-isothiazolin-3-one, 4,5-dichloro-2-methoxyethoxylpropyl-4-isothiazolin-3-one or 4,5-dichloro-2-diphenoxyethoxypropyl-4-isothiazolin-3-one, a considerable effect of the prevention and cure can also be obtained.
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An alkoxylpropyl isothiazolinone of formula: C 6 H 6 Cl 2 NO 2 SR, in which R is CH 3 , CH 2 CH 3 , CH(CH 3 ) 2 , CH 2 CH 2 CH 2 CH 3 , CH 2 CH 2 OCH 3 or CH 2 CH 2 OC 6 H 5 Cl. A method for preparing the isothiazolinone by reacting sodium polysulphide with methyl acrylate to obtain dimethyl dithiodipropionate, followed by aminolysis with alkoxyl propylamine to obtain N,N′-dialkoxylpropyldithio-dipropionamide, which is then reacted with sulfuric chloride. The alkoxylpropyl-isothiazolinone of the invention can be used for preparing marine antifouling paint coating as antifoulant, and also used as bactericide.
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[0001] This application is the national phase under 35 U.S.C. § 371 of PCT International Application No. PCT/DE01/02127 which has an International filing date of Jun. 6, 2001, which designated the United States of America and which claims priority on German Patent Application number DE 100 29 762.5 filed Jun. 16, 2000, the entire contents of which are hereby incorporated herein by reference.
FIELD OF THE INVENTION
[0002] The invention generally relates to a high temperature resistant marking agent, especially ink, for application to a surface, especially a ceramic surface.
BACKGROUND OF THE INVENTION
[0003] Such an ink is known, for example, from U.S. patent specification 5,055,137. The known ink is used for the marking of bodies. The high temperature resistant ink can be applied to cold or hot surfaces. To achieve the high temperature resistance, a mixture of a large number of different oxides which each have a certain molecular mass is used. In addition, various additives such as graphite, metals, sulfides etc. are used as stabilizers.
SUMMARY OF THE INVENTION
[0004] An object of an embodiment of the present invention is to produce a high temperature resistant marking agent from a smaller number of less expensive chemicals.
[0005] An object may be achieved for a high temperature resistant marking agent according to an embodiment of the invention by the marking agent comprising
[0006] 17-20 parts by mass of iron(III) nitrate nanohydrate,
[0007] 14-15 parts by mass of potassium hexacyanoferrate(II) trihydrate,
[0008] 2.5-10 parts by mass of 25% strength ammonia solution and
[0009] 160-200 parts by mass of distilled water.
[0010] The chemicals used are inexpensive proanalysis chemicals and distilled water. These substances can be acquired in a cost-effective manner and are available in an adequate amount. The high temperature resistant marking agent does not comprise any high temperature corrosive constituents. After subjecting the marking agent to a temperature of more than 500° C., virtually only iron oxides are still present.
[0011] The markings produced with the new type of marking agent are readily legible both prior to being subjected to heat and also after being subjected to heat. The marking withstands are subjected to temperatures of up to 1500° C. Prior to being subjected to heat, the marking agent has a blue color. After being subjected to heat of about 500° C., the color changes to a brown shade. The marking agent can be produced under atmospheric conditions by the portion-wise addition and mixing of the individual chemicals with the distilled water.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0012] The invention is described in more detail below by reference to a working example.
[0013] The potassium hexacyanoferrate(II) trihydrate {K 4 [Fe(CN) 6 ].3H 2 O} is dissolved in a predetermined amount of distilled water {H 2 O}. Gentle warming assists the dissolution operation. The iron(III) nitrate nanohydrate {Fe(NO 3 ) 3 .9H 2 O} is then added in portions to the existing solution and thoroughly mixed. To neutralize the solution, a 25% strength ammonia solution {NH 3 } is added thereto. The solution is to be neutralized to a pH of 6 to 7. Following a prolonged standing period, settlement of solid constituents of the solution can be observed. For this reason, thorough mixing of the solution is required prior to each use.
[0014] In order to produce 100 g of the high temperature resistant marking agent, 188 g of iron(III) nitrate nanohydrate and 147 g of potassium hexacyanoferrate(II) trihydrate are necessary. To achieve a ready-to-use consistency of the finished marking substance, approx. 1600 ml of distilled water are required. For the neutralization, 25 ml of 25% strength ammonia solution are added.
[0015] The high temperature resistant marking agent can be applied, for example, by using a suitable stamp, paintbrush or fiber-tip pen to the surface of the body to be marked.
[0016] The marking substance can be used, for example, for the permanent marking of combustion chamber bricks present in gas turbines.
[0017] The invention being thus described, it will be obvious that the same may be varied in many ways. Such variations are not to be regarded as a departure from the spirit and scope of the invention, and all such modifications as would be obvious to one skilled in the art are intended to be included within the scope of the following claims.
DESCRIPTION
[0018] High temperature resistant marking agent, especially ink
[0019] The invention relates to a high temperature resistant marking agent, especially ink, for application to a surface, especially a ceramic surface.
[0020] Such an ink is known, for example, from U.S. Pat. specification 5,055,137. The known ink is used for the marking of bodies. The high temperature resistant ink can be applied to cold or hot surfaces. To achieve the high temperature resistance, a mixture of a large number of different oxides which each have a certain molecular mass is used. In addition, various additives such as graphite, metals, sulfides etc. are used as stabilizers.
[0021] The object of the present invention is to produce a high temperature resistant marking agent of the type mentioned at the beginning from a smaller number of less expensive chemicals.
[0022] The object is achieved for a high temperature resistant marking agent of the type mentioned at the beginning according to the invention by the marking agent comprising
[0023] 17-20 parts by mass of iron (III) nitrate nanohydrate,
[0024] 14-15 parts by mass of potassium hexacyanoferrate(II) trihydrate,
[0025] 2.5-10 parts by mass of 25% strength ammonia solution and
[0026] 160-10 parts by mass of distilled water.
[0027] The chemicals used are inexpensive proanalysis chemicals and distilled water. These substances can be acquired in a cost-effective manner and are available in an adequate amount. The high temperature resistant marking agent does not comprise any high temperature corrosive constituents. After subjecting the marking agent to a temperature of more than 500° C., virtually only iron oxides are still present. The markings produced with the new type of marking agent are readily legible both prior to being subjected to heat and also after being subjected to heat. The marking withstands being subjected to temperatures of up to 1500° C. Prior to being subjected to heat, the marking agent has a blue color. After being subjected to heat of about 500° C., the color changes to a brown shade. The marking agent can be produced under atmospheric conditions by the portionwise addition and mixing of the individual chemicals with the distilled water.
[0028] The invention is described in more detail below by reference to a working example.
[0029] The potassium hexacyanoferrate (II) trihydrate {K 4 [Fe(CN) 6 ].3H 2 O} is dissolved in a predetermined amount of distilled water {H 2 O}. Gentle warming assists the dissolution operation. The iron(III) nitrate nanohydrate {Fe(NO 3 ) 3 .9H 2 O} is then added in portions to the existing solution and thoroughly mixed. To neutralize the solution, a 25% strength ammonia solution {NH 3 } is added thereto. The solution is to be neutralized to a pH of 6 to 7. Following a prolonged standing period, settlement of solid constituents of the solution can be observed. For this reason, thorough mixing of the solution is required prior to each use.
[0030] In order to produce 100 g of the high temperature resistant marking agent, 188 g of iron(III) nitrate nanohydrate and 147 g of potassium hexacyanoferrate(II) trihydrate are necessary. To achieve a ready-to-use consistency of the finished marking substance, approx. 1600 ml of distilled water are required. For the neutralization, 25 ml of 25% strength ammonia solution are added.
[0031] The high temperature resistant marking agent can be applied, for example, by means of a suitable stamp, paintbrush or fiber-tip pen to the surface of the body to be marked.
[0032] The marking substance can be used, for example, for the permanent marking of combustion chamber bricks present in gas turbines.
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The invention relates to a high temperature resistant marking agent comprising a small number of inexpensive pro-analysis chemicals. Said chemicals are dissolved into precise mass parts in distilled water and can be applied, for example, by means of a stamp, a paint brush or a fibre tip pen. The marking agent can be used, for example, to mark the bricks of a combustion chamber.
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BACKGROUND OF THE INVENTION
The present invention broadly relates to a method for treating a copper or copper alloy substrate to improve resistance to both oxidation and chemicals. More particularly, the substrate is immersed in an aqueous solution containing chromium (VI) ions and phosphate ions.
Copper and copper based alloys are widely used in electrical and electronic applications. Among the more widespread electronic uses are the manufacture of leadframes from strip and the manufacture of conductive circuit traces from foil. The foil is either wrought, produced by mechanically reducing the thickness of a strip such as by rolling, or electrodeposited, produced by electrolytically depositing copper ions on a rotating cathode drum and then removing the deposition from the drum. The foil is bonded to a dielectric support layer which is either rigid such as FR-4 (a flame retardant epoxy), or flexible such as a polyimide. After lamination, circuit patterns are formed in the copper foil by selective etching.
Copper is a material of choice for electronic applications due to high electrical conductivity. One drawback with copper and its alloys is reactivity. The metal reacts with oxygen and tarnishes. The metal is also reactive with some of the chemical solutions encountered during the manufacture of electronic components such as hydrochloric acid and sodium hydroxide. Many anti-tarnish coatings to prevent oxidation of a copper foil prior to lamination are known. These coatings do not also impart improved chemical resistance, particularly after lamination.
Some typical anti-tarnish coatings, all of which are assigned to the same assignee as the present application and all of which are incorporated by reference in their entirety herein, include (1) mixtures of chromic acid and phosphoric acid; (2) sodium dichromate and phosphoric acid; and (3) a co-deposited layer of chromium and zinc.
U.S. Pat. No. 3,837,929 to Caule discloses an aqueous solution containing 3.5 grams per liter (g/l) to saturation of sodium or potassium dichromate mixed with 8-85% phosphoric acid (83-1436 g/l). A foil is immersed in the solution for at least two seconds and then rinsed. Preferably, as disclosed in U.S. Pat. No. 3,764,400, also to Caule, rinsing is in an alkaline solution (PH 8.5-11) at a temperature above 90° C. As further disclosed in U.S. Pat. No. 3,941,627, also to Caule, the treated foil is then laminated to a substrate with an adhesive.
The Caule coating provides the foil with good anti-tarnish resistance. However, the coating is applied prior to lamination and imaging of the foil to form lead traces. A necessary characteristic of the coating is limited acid resistance as disclosed in the '627 patent. The anti-tarnish coating is dissolved in an acid prior to imaging of the foil.
Another coating is disclosed in U.S. Pat. No. 4,647,315 to Parthasarathi which discloses a solution containing 0.02 to 1 g/l chromic acid and 0.02 to 1 g/l phosphoric acid. The solution is used at a temperature of from 60° C. to 90° C. and the foil immersed for 1-120 seconds.
The above coatings are applied non-electrolytically. An electrolytic coating comprising a co-deposited layer of chromium and zinc is disclosed in U.S. Pat. No. 5,022,968 to Lin et al. The substrate is immersed in an aqueous basic solution containing hydroxide ions, from 0.07 g/l to 7 g/l zinc ions and from about 0.1 g/l to 100 g/l of a water soluble hexavalent chromium salt. The concentration of either the zinc ions or the chromium (VI) ions or both, is less than 1.0 g/l. An electric current of from about 1 milliamp per square centimeter to about 1 amp per square centimeter is impressed across the electrolytic cell with the substrate forming the cathode. The electrolytically deposited coating provides an anti-tarnish coating readily removed in both dilute hydrochloric and sulphuric acids.
The above treatments are well suited for protecting a copper or copper alloy substrate prior to photoimaging. It is also desirable to provide an anti-tarnish coating to protect imaged circuit traces laminated to a printed circuit board from oxidation, exposure to chemicals, temperature cycling, and contaminants such as fingerprints, soils and residual chemicals. Unfinished printed circuit boards are frequently stored before being further processed and improved performance is achieved by minimizing tarnish during storage. The printed circuit boards may be multi-layer with a plurality of planar circuit traces separated by dielectric layers. The anti-tarnish coating of the invention enhances adhesion between circuit traces and the dielectric layer.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the invention to provide a method for treating a copper or copper alloy substrate which provides resistance to both tarnish and to chemicals. It is a feature of the invention that the method of treatment includes immersing the substrate in a solution containing both chromium (VI) ions and phosphate ions. Yet another feature of the invention is that further improvement is achieved by selected pretreatment or post treatment steps such as degreasing or rinsing in an aqueous alkali solution.
It is an advantage of the invention that the method of treatment prevents discoloration of laminated circuit traces. Yet another advantage of the invention is that both room temperature and high temperature tarnish resistance is improved. Still another advantage of the invention is that the coating promotes adhesion between copper alloys and polymeric materials. The anti-tarnish coating extends the shelf life of a printed circuit board. Yet another advantage of the invention is that the treatments are not limited to printed circuit boards and can be utilized on leadframes or other electrical or electronic components.
In accordance with the invention, there is provided a method for treating a copper or copper alloy substrate to improve oxidation resistance and chemical resistance. The method includes treating the substrate in an aqueous solution containing from about 0.1 to about 10 g/l of chromium (VI) ions and from about 1.5 to about 10 g/l of phosphate ions.
The objects, features and advantages discussed above will become more apparent from the specification and drawings which follow.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 shows in top planar view a printed circuit board having circuit traces treated according to the method of the invention.
FIG. 2 shows in cross-sectional representation the treated printed circuit board of FIG. 1.
FIG. 3 shows in cross-sectional representation a detailed view of a solder joint.
FIG. 4 shows in cross-sectional representation a multi-layer circuit board treated according to the method of the invention.
FIG. 5 shows in cross-sectional representation a plastic electronic package having a leadframe treated according to the method of the invention.
DETAILED DESCRIPTION OF THE INVENTION
In accordance with the invention, the tarnish and chemical resistance of copper and copper alloy substrates is improved by treating the substrate in an aqueous solution containing water soluble hexavalent chromium ions and phosphate ions. Any method of contacting the substrate with the aqueous solution is acceptable, such as spraying or immersion. Immersion is the preferred method of application. The aqueous solution contains from about 0.1 to about 10 g/l chromium (VI) ions and from about 1.5 to about 10 g/l phosphate ions. It is within the scope of the invention for the solution to contain various additives such as a surfactant or chelating agent. The water soluble hexavalent chromium ions may be provided from any suitable source such as chromic acid, sodium dichromate or potassium dichromate. The most preferred source is sodium dichromate.
The phosphate ions may be provided from phosphoric acid or an acid solution containing a phosphate salt. The latter include a solution of sulfuric acid and sodium, potassium or lithium phosphate. A preferred source of phosphate ions is phosphoric acid. Table 1 illustrates the preferred concentrations of chromium (VI) ions and phosphate ions and the corresponding concentration of the preferred ion contributors (sodium dichromate and phosphoric acid).
TABLE 1______________________________________ PreferredCompositional Ion ion sourceRange Concentration Concentration______________________________________BROAD .1-10 g/l Cr (VI) .28-28.6 g/l 1.5-10 g/l phosphate 2.9-19.2 g/lINTERMEDIATE 1.5-5 g/l Cr (VI) 1.4-14.3 g/l 1.5-5 g/l phosphate 2.9-9.6 g/lNARROW 0.8-1.5 g/l Cr (VI) 2.3-4.3 g/l 1.8-2.5 phosphate 3.5-4.8 g/l______________________________________
The substrate is immersed in the solution for a time effective to deposit a tarnish and chemically resistant coating. This time ranges from about 2 seconds to about 2 minutes and is dependent on both the copper alloy being treated and the severity of the anticipated environment. For typical electronic circuit or package assembly, an immersion time of from about 10 to 30 seconds is suitable. Any solution temperature from below ambient to boiling may be utilized. Superior chemical resistance is obtained at temperatures above about 50° C. and more preferably, above about 60° C. As the temperature of the aqueous solution is increased, the imparted chemical resistance improves and the etching rate of the substrate by phosphoric acid increases. While slight etching of the substrate is believed beneficial to improve the adhesion between the substrate and a polymer, more severe etching may change circuit trace line width and is to be avoided. Accordingly, at the preferred elevated temperatures, a lower concentration of phosphoric acid is utilized.
The anti-tarnish/chemical resistance properties of the coating are enhanced by pretreatment or post treatment. Degreasing in a suitable solvent improves the effectiveness of the solutions, as does a suitable electroclean. The solvents are preferably of the nonpolar type such as methylene chloride. The substrate is degreased by immersing the substrate in the solvent for a sufficient amount of time such as from about 1 to about 10 seconds. After immersing in the solvent, the substrate is rinsed in deionized water and treated according to the method of the invention.
Effective treatments may also include a post treatment. One suitable post treatment involves rinsing the substrate in deionized water followed by air drying. A preferred post treatment rinse is tap water for a few seconds followed by rinsing in an alkaline solution made from deionized water. One such alkaline solution contains diluted calcium hydroxide at a pH of from about 11 to about 13 and most preferably at about 12. After rinsing in the alkaline solution for a few seconds, the treated substrate is air dried.
The application of the treatments of the invention is seen with reference to the Figures. FIG. 1 shows in top planar view a printed circuit board 10 having a dielectric substrate 12 and a plurality of copper or copper alloy circuit traces 14. The printed circuit board 10 was formed by laminating a layer of copper or copper alloy foil to the substrate 12. The circuit traces 14 were then formed by photoimaging by any means known in the art.
Following lamination of the copper foil and photoimaging of the circuit traces, the foil and/or circuit traces are protected from oxidation and chemical attack by immersing the printed circuit board 10 in the anti-tarnish solution of the invention. The board 10 is then immersed in an aqueous solution containing chromium (VI) ions and phosphate ions. Subsequent to coating, the board is rinsed, preferably in tap water followed by deionized water containing calcium hydroxide. After drying, a thin layer of the anti-tarnish coating coats the circuit traces 14. This layer is believed to be a mixture of chromium, phosporous and oxygen. An immersion time of about 20 to 30 seconds is believed to produce an anti-tarnish layer having a thickness of from about 50 to about 250 angstroms.
Subsequent to the anti-tarnish treatment, electronic components 16 such as transistors, capacitors and integrated circuit packages are electrically interconnected to the circuit traces 14 such as by soldering. FIG. 2 shows in more detail the interconnection of an electronic component 16 to a printed circuit board 10. Electronic component 16 has leads 18 which are either flush against circuit traces 14 such as a "J-lead" or "gull lead" on a surface mount package or extend into an aperture formed in the circuit trace. The lead is then soldered to circuit trace 14 using a conventional solder, typically an alloy of lead and tin or of gold and tin. A preferred solder is a lead/tin alloy with a melting temperature of about 250° C.
The solder joint is more clearly seen in FIG. 3 which is an exploded view of the portion of FIG. 2 indicated by reference numeral 3. The lead 18 makes physical contact with circuit trace 14. An anti-tarnish coating 20 originally coated both the top of the lead and the sides of the leads. One advantage of the anti-tarnish coating of the invention over organic coatings such as benzotriazole, is a uniform coating 20 forms along the sides of the leads. This coating prevents undercutting of the circuit trace 14 by exposure to dilute acids.
The solder 22 may be capable of wetting and bonding to the anti-tarnish layer 20. If an inferior bond is formed, the coating 20 may be removed from the bonding surface of the circuit trace 14 as illustrated in FIG. 3. Suitable methods to remove the tarnish coating include combining the solder with an active flux such as a mildly to fully active rosin flux.
Alternatively, the bonding areas of the circuit traces 14 may be masked prior to the anti-tarnish treatment such that a coating is not applied to the solder areas of the circuit traces. Another alternative is to remove the anti-tarnish coating 20 from the solder areas such as by mechanical abrasion or chemical dissolution.
The anti-tarnish coating prevents the formation of copper oxides on the circuit traces. Applicants believe improved adhesion to a polymer results. Multi-layer circuits as illustrated in FIG. 4 and electronic packages as illustrated in FIG. 5 are also improved by the treatment of the invention. With reference to FIG. 4, a multi-layer printed circuit board 10' has a first dielectric substrate 12 to which are laminated a first set of circuit traces 14. The first set of circuit traces 14 are coated with the anti-tarnish coating 20 of the invention. A second dielectric layer 24 is then bonded to a face 26 of the first dielectric 12. The anti-tarnish coating 20 ensures that the second dielectric 24 is bonded to a metal rather than copper oxide which could flake from the circuit trace 14, leading to delamination. Additionally, copper catalyzes the degradation of polymers. The coating 20 forms a barrier preventing exposure of the second dielectric 24 to the copper of the circuit trace 14. A second copper or copper alloy substrate is then bonded to a surface 28 of the second dielectric 24. The second layer of metallic foil is then etched by photolithography into a desired pattern of second circuit traces 14' separated and electrically isolated from the first set of circuit traces 14 by the second dielectric 24. The second set of circuit traces 14' may also be protected from tarnish and chemical attack by the anti-tarnish coating 20 of the invention.
FIG. 5 shows yet another application of the treatment of the invention. Rather than treating a copper foil, a copper leadframe 30 is coated with the anti-tarnish coating 20 of the invention. Leadframes are typically made from copper or a copper alloy to maximize electrical conductivity and have a thickness of from about 0.13 to about 5.1 mm. The leadframe 30 has a plurality of leads terminating at inner lead ends 32 defining a central aperture. Frequently, a die paddle is located in the aperture for attachment of an integrated circuit device 36. The die paddle 34 is also preferably coated with the anti-tarnish coating 20. The coating 20 improves the adhesion of the leads and die attach paddle 34 to a molding resin 38. Improved adhesion minimizes the ingress of water along the leads and the accumulation of moisture under the die attach paddle 34. Preventing the accumulation of moisture under the die attach paddle 34 is desirable to prevent the "popcorn effect". When the package is heated such as during soldering, the moisture under die attach paddle expands, forming a bulge in the base of the package. Improved adhesion between the leads and the die attach paddle and the molding resin 38 minimizes or prevents the popcorn affect.
While the coated leadframe is particularly suited for plastic encapsulated electronic packages, metal packages such as disclosed in U.S. Pat. No. 4,939,316 to Mahulikar et al. which is incorporated herein in its entirety, are also benefited. This type of metal package has discrete base and cover components. A leadframe is disposed between the components and adhesively bonded to both. The coatings of the present invention would be expected to improve the adhesive bond to the leadframe. Additionally, the various package components could be similarly treated to achieve improved adhesion.
EXAMPLES
The resistance to tarnish and chemicals provided by the treatment of the invention is illustrated in Table 2. This data was generated by immersing copper alloy C110 (ectrolytic tough pitch copper having a nominal composition by weight of 99.90% minimum copper and a maximum oxygen content of 0.5%) alloy foil in a aqueous solution containing Na 2 Cr 2 O 7 .2H 2 O and H 3 PO 4 in the specified concentrations. The foil was immersed for 20 seconds, rinsed with tap water for a few seconds and then rinsed in deionized water containing Ca(OH) 2 at a pH of 12 and air dried.
Bake resistance was determined by heating the samples for 30 minutes in air to the specified temperatures and visually comparing to a control sample which was not heated. A rating of 1 indicates that the bake sample appears essentially the same as the control. Higher rating numbers indicating progressively more oxidation and tarnish.
Chemical resistance was evaluated by immersing the sample in the specified acid or alkali solution for 30 seconds. The test coupons were then immersed in ammonium sulfide (NH 4 ) 2 S. The appearance of blue spots indicated attack of the copper alloy substrate. A rating of 1 indicated the appearance of virtually no blue spots. Higher numbers indicated progressively more blue spotting, indicative of a less satisfactory coating.
TABLE 2__________________________________________________________________________Comparison of Different Anti-tarnish Treatments Bake Process Resistance (30 min) Chemical Resistance (30 min)Treatment Na.sub.2 Cr.sub.2 O.sub.7.2H.sub.2 O (g/l) H.sub.3 PO.sub.4 (g/l) Temp (°C.) 170° C. 190° C. 210° C. 0.12N HCl 0.24N 3N__________________________________________________________________________ NaOH1 34 574 Ambient 1 1 1 5 5 12 1 2 Ambient 1 3 3 5 5 33 1 2 50 1 1 1 1-2 2-3 14 1 2 60 1 -- 1 -- 1 15 3-4 29 Ambient 1 1 1 5 5 16 7 29 Ambient 1 1 3 3 4 17 3 8 60 1 1 1 1 1 1None -- -- -- 5 -- -- 5 -- 5Reference I 0.3 g/l CrO.sub.3 0.6 57 1 3-5 -- 2 3-4 1Reference II 34 574 Ambient 3 5 -- 4 4-5 1__________________________________________________________________________ *Treatments 1-7 and reference 1 includes solvent pretreat and alkaline post rinse. Reference 2 has only the post treatment.
The patents cited in this application are intended to be incorporated herein by reference
It is apparent that there has been provided in accordance with this invention a treatment for copper or copper alloy substrates which imparts improved oxidation and chemical resistance and fully satisfies the objects, means and advantages set forth herein before. While the invention has been described in combination with specific embodiments thereof, it is evident that many alternatives, modifications and variations will be apparent to those skilled in the art in light of the foregoing description. Accordingly, it is intended to embrace all such alternatives, modifications and variations as fall within the spirit and broad scope of the appended claims.
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There is provided a method of treating a copper or copper alloy substrate to provide improved resistance to both oxidation and to chemical attack. The substrate is immersed in an aqueous solution containing both chromium (VI) ion and phosphate ions. The treatment is particularly effective for protecting imaged printed circuit boards during storage, handling and use.
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This application is a continuation-in-part of application Ser. No. 70,150, filed Aug. 27, 1979, and now abandoned.
This invention relates to tools for installing scarifier teeth for ripping concrete, blacktop and the like.
BACKGROUND OF THE INVENTION
Scarifier teeth are normally installed in an angular position, as in a socket having a hole disposed at an angle, such as 45°, to the radius of a drum on which the socket is mounted, while an annular recess near the rear end of the hole is adapted to receive a spring which expands into the recess. This spring is contained in an annular slot near the rear of a rear stem of the tooth, which also has a body and, at the front end of the body, a tip of hard metal, such as tungsten carbide or an alloy having similar wear resistant qualities. This tip is predominantly circular, so as to fit into a central hole in the body, but has a conical point. The tip is normally held in place on the body by weld metal deposited around the periphery of the rear edge of the conical point.
The socket in which the tooth is installed has an at least partially open rear end, so that a pin, chisel or the like may be inserted into the socket to drive the tooth out of the hole when the tip is broken or worn, or the tooth should be replaced for some other reason. Normally, heavy hammers have been used to drive the teeth out of the sockets. The hole in the socket also has a bevel at its entrance, so as to compress the spring contained in the slot in the stem of the tooth, so that the tooth may be moved into the hole until the spring reaches the recess of the socket hole. Again, heavy hammers have been used in driving the teeth into the sockets, which has resulted in an undue amount of breakage of teeth, particularly the tips formed of relatively hard metal. In addition, the use of heavy hammers to drive worn or broken teeth out and to install new teeth requires an undue amount of time. Since the drum on which the sockets are located in both a radial and axial spaced relationship may be on the order of 3 feet in diameter and 8 to 10 feet wide, and may have on the order of 110 sockets and teeth, to drive out the broken or worn teeth with a heavy hammer and replace them again, with the use of a heavy hammer, requires an undue amount of time. Additional time is required, for heavy hammer operations, to drive out teeth that have been broken by installation with such a hammer and reinstalling new teeth. Certain users have experienced a necessity for replacing teeth for ripping asphalt every four hours, and to replace teeth for ripping concrete sometimes six times a day. Since the ripping machines are normally rented at a cost, in certain instances, of $500.00 per hour, excessive down time of the machines, particularly due to the amount of time involved in heavy hammer operations, is quite costly.
Among the objects of this invention are to provide a tool for installing scarifier teeth which enables a percussion instrument, such as an air hammer, to be utilized; to provide such a tool which is not required to engage the hard metal tip of the teeth, but rather a portion of the body of the teeth; to provide such a tool which does not tend to wedge on the tooth during installation; to provide such a tool which may be mounted on the drive pin of an air hammer, such as identical to that which may be used for driving the teeth out of the socket; to provide such a tool which may be readily manufactured, but with a variation to accommodate different styles of teeth, such as used for ripping concrete and for ripping blacktop; and to provide such a tool which is effective and efficient in operation and tends to have a relatively long, useful life.
U.S. Pat. No. 3,769,683 discloses a sliding hammer device provided with a pivoted loop which may be placed over a cutter bit for a mining, excavating or earth working machine to remove the bit when worn. A head member of the tool may be provided with a depression or recess which fits over the cone-shaped nose of that style of bit, with the hammer impacted against an appropriate flange to drive the tooth into a socket. However, the included angle between opposite interior surfaces of the conical recess is approximately 30°, i.e. the bevel on the inside of the recess is approximately 15° to the axis of the tool. Thus, such a tool is not adapted for use with scarifier teeth, since it tends to become wedged on the conical surfaces.
SUMMARY OF THE INVENTION
The foregoing problems attendant upon the installation of scarifier teeth are overcome by this invention through the use of a tool having a hole which will fit over a portion of the scarifier tooth, with a bevel at the outer edge of the hole, at an angle of at least 321/2° but preferably 35° with respect to the axis of the tool, so that the included angle between opposite sides of the frusto-conical surface provided by the bevel will be at least 65°. This angle was found to be critical, since attempts to engage a conical surface of a tooth by a conical bevel of the tool having a lesser angle resulted in wedging of the tool on the tooth, with considerable difficulty and particularly considerable time involved in dislodging the tool, sometimes accompanied by removal of the tooth from the socket. A tool of this invention is particularly adapted, with the assistance of an air hammer or the like, to install a tooth for ripping concrete, which is provided with a hard metal tip and weld metal by which the tip is attached to the body of the tool, but an outer bevel of the body adjacent the weld metal which has a lesser inclination to the axis of the tool than the remainder of the tool body. The inner bevel of the tool engages the outer bevel of the tooth for impact of the driving force for installation of the tooth, but does not become wedged on the tooth. Teeth for ripping blacktop are larger in diameter than teeth for ripping concrete and have a larger tip with a conical point, while the body is conical at an extremely acute angle but does have an outwardly flaring skirt adjacent the rear stem. A tool of this invention for installing such teeth has a larger and longer hole extending to one end in order to surround not only the tip but also a majority of the body, so that the inner bevel at the entrance of the hole will engage the flaring skirt of the body.
Each tool of this invention is also provided with a hole at the opposite end which is adapted to receive a drive pin, conveniently identical to that which may be utilized for driving teeth from the sockets through use of an air hammer.
THE DRAWINGS
Additional objects and other novel features of this invention will become apparent from the description which follows, taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a side elevation, on a reduced scale, of a rotatable drum on which is mounted a series of teeth for ripping concrete, blacktop or the like.
FIG. 2 is a fragmentary cross section of a portion of the drum and one of the sockets of FIG. 1, showing in full a tooth for ripping concrete installed in the socket, as well as a portion of a pin which is actuated by an air hammer and is adapted to drive the tooth from the socket.
FIG. 3 is a fragmentary cross section, with certain parts in full, showing the tooth of FIG. 2 and a tool constructed in accordance with this invention for installing the tooth in the socket, the tool being engaged by an air hammer pin which may be identical to that used for driving out the tooth.
FIG. 4 is a condensed longitudinal section, on an enlarged scale, of the tool of FIG. 3, showing also a portion of the air hammer pin.
FIG. 5 is a condensed side elevation, on a reduced scale, of an air hammer or air gun, with the drive pin mounted therein and a tool of this invention mounted on the drive pin.
FIG. 6 is a fragmentary cross section similar to FIG. 4, but showing a tooth for ripping blacktop being installed in a socket through the use of an alternative tool of this invention, as through a drive pin of an air hammer.
FIG. 7 is a longitudinal section of the tool of FIG. 6, on an enlarged scale, showing also a portion of the drive pin inserted therein.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
A series of scarifier teeth C, particularly adapted to be utilized for ripping concrete and also to be installed by a tool of this invention, are mounted, as in FIG. 1, in a series of sockets S on a rotatable drum D, which may be on the order of 3 feet in diameter, 8 to 10 feet wide and have on the order of 110 teeth distributed both circumferentially and axially about the drum. As in FIGS. 2 and 3, each socket S may be mounted on the outer surface 10 of the drum, as with a base 11 of the socket having a curvature corresponding to the outer surface of the drum and weld metal 12 extending around the periphery, or a suitable portion of the periphery, of base 11 to attach the socket to the drum. Since scarifier teeth are subject to considerable stress during rotation against the concrete or blacktop which is to be removed, the mounting of the sockets must be quite secure. Each socket may be provided with a hole 13 extending at an angle, such as 45°, to the radius of the drum, while a correspondingly angled, semicylindrical surface 14 surrounds the outer half of the hole 13 and provides sufficient thickness of metal around the hole to withstand the stresses imposed. Adjacent the inner end of hole 13 is an annular recess 15 for a purpose described below, while the lower portion of the rear end of hole 13 terminates in an abutment 16 formed by a lower corner 17 of the socket. The outer end of hole 13 may be provided with a bevel 18, as at 45°, to facilitate installation of a tooth C, as described below. The socket S is generally rectangular in configuration, except for the angled semicylindrical surface 14 and a 45° surface 19 surrounding the outer end of hole 13.
The tooth C illustrated in FIGS. 2 and 3, but in the installed position of FIG. 2, is particularly adapted for ripping concrete, as indicated. Tooth C has an outer tip 20, a body 21 and an inner stem 22 having a diameter slightly less than hole 13 in socket S. Tip 20 is made of a hard metal, such as tungsten carbide or an alloy having similar properties, and has a conical end, as shown, but is otherwise cylindrical, for insertion in a central hole within body 21 of the tooth. Body 21 is also conical but principally at an included angle on the order of 10°, while its outer end forms a shoulder 23. The top 20, when seated in the hole, is attached to the body of the tooth by weld metal 24, which normally does not extend outwardly to the edge of shoulder 23. Rearwardly of shoulder 23 is an outer bevel 25 which forms a frustoconical surface at an angle of approximately 25° to the axis of the tooth or an included angle of 50°. Bevel 25, although less than 35° to the axis, still cooperates in a unique manner with a tool of this invention, in a manner described later. Between body 21 and stem 22 is an interiorly rounded groove 26 which extends to a flare or skirt 27 of the stem, the latter being adapted to seat against the bevel 18 of socket S when the tooth is installed, as in the position of FIG. 2. Spaced from the lower end of the tooth is a groove 28 which receives an annular spring 29 having an overlapping joint 30 which permits the spring to retract and expand in the groove 28. On spring 29, a series of outwardly conical projections 31, having a blunt outer end, engage the inner wall of hole 13, while the tooth is being inserted in the socket, thereby reducing the frictional resistance to movement of the stem into hole 13. When the tooth is seated in the socket hole, as in FIG. 2, with the rear end of the tooth adjacent abutment 16, and the flare 27 seated against bevel 18, the projections 31 will expand into the recess 15, thereby retaining the tooth against dislodgement from the socket. As illustrated in FIG. 2, a drive pin 25 actuated by an air hammer, such as the Chicago Pneumatic Tool Company CP717 heavy duty air hammer, may be utilized in removing the tooth from the socket, as by impacts produced in the direction of the arrow 36, to cause the spring 29 to retract and the tooth to be driven from the socket. As in FIGS. 5 and 6, drive pin 35 is provided with a flange 37 spaced from its inner end, for the purpose of preventing its accidental release from an air hammer H, in a manner described later.
As indicated previously, a workman can drive out a number of teeth which need to be replaced from the socket and insert a new tooth in each socket, as in the position of FIG. 3, in which the spring 29 has engaged the bevel 18 and become compressed enough to retain the tooth in the socket until a tool T of this invention and adapted to be mounted on the same type of drive pin 35 used in removing the teeth from the socket, can be used to drive the tooth into the socket. As the tooth C is driven into the socket, spring 29 is further compressed and each tooth moved into the hole 13, until flare 27 seats against bevel 18 and spring 29 expands into recess 15. Such a tool T may be formed from a cylinder 40 of suitable metal by producing a hole 41 extending from one end 42 and also producing a bevel 43 which extends around the outer edge of the hole 41 at an angle of at least 321/2° but preferably 35° to the axis of the tool, so as to form an interior conical surface having an included angle of at least 65° and preferably 70°. The use of a bevel at an angle of 321/2° and preferably 35° to the axis of the tool is important because it has been found that the tool will wedge on the tooth if the angle of the interior bevel is less than 321/2° to the axis of the tool, i.e. if the included angle between the sides of the interior cone is less than 65°. Since placement of the tool directly against the tip 20 tends to result in destruction of the tip, similar to the destruction of the tip when the tool is attempted to be installed with a heavy hammer, the diameter of hole 41 of the tool is not only greater than the diameter of tip 20 but also preferably greater than the extension of weld metal 24, so that interior bevel 43 of the tool will engage outer bevel 25 of the tooth, at or adjacent the edge of shoulder 23. This avoids any tendency for the tool to tend to wedge on the tooth.
The same air hammer can be used to install the tooth as is used to remove the tooth. Thus, a cylindrical hole 44 extends from the opposite end of the tool for a distance sufficient to accommodate the drive pin, which may be the same drive pin as is used for driving out the tooth, as in FIG. 2, although it is somewhat preferable to use a different drive pin for driving out the teeth, since the end which engages the teeth tends to become upset and spread out. In addition, it may be found desirable to provide a separate drive pin for each tool, so that the tool may be fastened to the drive pin, as by a shim 45 of FIG. 4, to prevent the tool from being ejected from the drive pin if the trigger of the air hammer is accidentally pushed. The entrance of hole 44 may be provided with a bevel 46, as at 45°, to facilitate entry of the drive pin and/or the shim 45. Although one workman may drive out a series of teeth to be replaced, then change to a drive pin on which a tool of this invention is mounted, for installing new teeth in the empty sockets, a saving in time can be obtained if two air hammers are used by separate workmen, one operating an air hammer provided with a drive pin for driving out the teeth to be replaced and the other with a drive pin on which a tool of this invention is mounted, for installing the new teeth. Either workman may place the new teeth in the empty sockets, as in the position of FIG. 3.
As illustrated in FIG. 5, an air hammer H corresponding to the Chicago Pneumatic Tool Company air hammer CP717 has a barrel 50 and a handle 51, with which is associated a trigger 52, while an air hose 53 extends from the end of the handle. A drive pin 35, on which a tool T may be mounted is inserted in a reciprocating chuck (not shown) inside barrel 50, while a loop 54 of a coil spring 55 may be placed over flange 37 of the drive pin, to insure that the drive pin is not ejected from the hammer, in the event that the hammer is accidentally actuated.
A tooth A, shown in FIG. 6, may be installed in and removed from the same socket S in which the tooth C of FIGS. 2 and 3 is installed in and removed from. The tooth A is particularly adapted for ripping asphalt or blacktop, but is provided with a stem 22 identical to that of tooth C, i.e. having a flare 27 for abutting bevel 18 of the socket S and a groove 28 for receiving spring 29 having a joint 30 and projections 31. Spring 29 is compressed by bevel 18 as it moves into the hole 13 of socket S, but expands when it reaches recess 15 in the socket, as before. The tooth A has a tip which includes a conical outer end 59 and a frusto-conical portion 60, as well as a body 61. The diameter of the forward end of body 61, whose conical sides are inclined at an extremely small angle, such as on the order of 5° to the axis of the tooth, and of the rear end of the head of tip portion 60 are such that the weld metal 62 normally extends outwardly to the edge of the front of body 61. However, the rear end of body 61 is provided with a flaring skirt 63 which is inclined at an angle on the order of 35° to the axis of the tooth, i.e. the flaring skirt 63 has an exterior frusto-conical surface, the included angles between the sides of which are approximately 70°. A rounded groove 64 separates skirt 63 and flare 27 of stem 22.
For installing the tooth A with the same type of air hammer and drive pin, such as air hammer H and drive pin 35 of FIG. 5, tool T' of FIGS. 6 and 7 may be formed from a cylinder 70 having a central hole 71 which extends from one end 72 and which is of sufficient diameter to surround the tip and that portion of the body between the tip and the flaring skirt 63. The outer edge of hole 71 is provided with a bevel 73 which is inclined at an angle of at least 321/2° but preferably 35° to the axis of the tool, to form an interior frusto-conical surface, the included angle between the opposite sides of which is at least 65° but preferably 70°. As in FIG. 6, bevel 73 engages the skirt 63 of the tooth, so that not only do impacts transmitted to the tooth by engagement of bevel 73 with flaring skirt 63 drive the tooth A into the corresponding socket, but also the tool may be readily removed from the tooth without wedging, due to the angle of the bevel. A hole 74 which receives a drive pin 35 extends inwardly from the opposite end of cylinder 70, while a shim 75 may surround drive pin 35, for more securely attaching the drive pin to the tool. Shim 75 is conveniently wedged between the drive pin and hole 74, the outer end of which may be provided with a bevel 76, as at approximately 45°, to assist in insertion of the shim 66. The tool T' of FIGS. 6 and 7 may be used with an air hammer in the same manner as tool T of FIGS. 3-5, i.e. mounted on or attached to a drive pin 35 which is mounted in the air hammer, as in FIG. 6, with a spring loop 54 placed over flange 37 of the drive pin.
Although the tool of this invention is particularly adapted for installing scarifier teeth for concrete and blacktop, with the diameter and length of the hole which encircles a portion of the tool being provided in accordance with the diameter of the tooth to the surface to be engaged by the inner bevel of the tool, it will be understood that variations in the tool may be made to accommodate different designs of scarifier teeth, and particularly changes in the design of teeth for ripping concrete and of teeth for ripping blacktop. Thus, it will be understood that various changes may be made without departing from the spirit and scope of this invention.
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A tool for installing scarifier teeth in a hole in a socket attached to a drum, as by using an identical pin and air hammer as can be used for removing the teeth through an aperture at the rear of the socket. The tool has a circular hole with an inner bevel at an angle of not less than 321/2° but preferably 35° to the center line of the hole, while this bevel engages an outer bevel of a body of the tooth adjacent a shoulder to which weld metal attaches a tip of relatively hard metal to the body, or a flare or skirt of the body adjacent a stem of the tooth. The aforesaid holes in the body may be of different length and different diameter, depending on the distance from the point of the tip to the bevel or the flare or skirt. The opposite end of the tool is provided with a hole to receive a pin which may be impacted by an air hammer, while a shim may wedge the pin in this hole to prevent the tool from flying off the pin if the air hammer is accidentally triggered.
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CROSS-REFERENCE TO RELATED APPLICATIONS
Not Applicable.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
Not Applicable.
BACKGROUND OF THE INVENTION
1. Field of Invention
The invention pertains to a system for purification of contaminated liquids. More particularly, this invention pertains to a system for treatment utilizing a plurality of electric-driven membranes and pressure-driven membranes in a plurality of integrated configurations for removal of contaminants and deionization of liquids.
2. Description of the Related Art
In many areas of the world, treatment of saline water and industrial wastewater is necessary to obtain adequate and protect existing supplies of drinking water. In highly developed countries, recycling of waste liquids generated by industry is required by government regulations, and/or is preferred by industry to maximize recovery of useful liquids, to reduce costs of feed liquids, and to minimize waste discharge.
Currently, a number of systems are utilized for desalination and deionization applications, and for treating aqueous waste streams and aqueous/organic mixtures, including membrane-based technologies, distillation and evaporation, and ion exchange. Membrane-based desalting technologies may be categorized as pressure-driven reverse osmosis (RO) and nanofiltration (NF) and electrically-driven electrodialysis (ED). RO, NF, and ED have commonality in that these processes use semi-permeable membranes as key elements in performing the separation, resulting in significant energy savings compared to thermal processes such as distillation or evaporation, and substantial operational cost savings compared to ion exchange resin methods.
The pressure driven processes ultrafiltration (UF), RO, and NF rely on a semi-permeable membrane to separate one component of a solution from another by means of size exclusion, preferential transport, and pressure. UF typically rejects organics over 1,000 molecular weight (MW) while passing ions and small organics along with water, while RO provides separation of both ions and many small organics. NF provides separation in the range between UF and RO. NF membranes have a wide range of performance characteristics but typically reject organic solutes on the order of a nanometer or 10 angstroms in size as well as larger, highly charged multivalent ions such as sulfate and phosphate. NF will typically not efficiently retain or reject smaller species like chloride and organic acids
UF, NF, and RO systems provide varying filtration and separation efficiencies but many times may lack the ability to economically produce a deionized product liquid of sufficient quality or quantity for reuse in industry, discharge, or municipal use; additional treatment may also be required as some components of the liquid may fall outside the operating ranges where separations are the most efficient and economically feasible for these membrane processes
NF and RO processes have been widely utilized for a range of desalination and deionization applications, but product recovery has a major impact on the economics of pressure-driven membranes and limits process applicability. Furthermore, pressure-based membranes have several inherent technical and economical limitations to achieving high feed recoveries, the most severe of which is the osmotic pressure of the feed solution that has to be overcome by the applied hydrostatic (feed) pressure. The osmotic pressure of saline solutions such as brackish water and seawater can be significant. Moreover, since the osmotic pressure is determined by the salt concentration directly at the membrane surface, it can be affected by concentration polarization, which is the build-up of salt near the surface of the membrane due to incomplete mixing of the surface boundary layer fluid with the bulk solution, a phenomenon accentuated by high pressure fluid passing through the membrane material. Although concentration polarization can be minimized by design and operating parameters, it can never be completely excluded and must be overcome by increased applied hydrostatic (feed) pressure, particularly as feed recovery is increased. Overcoming high osmotic pressures and concentration polarization resulting from higher recoveries requires not only substantial energy to produce the necessary higher pressures and flow rates but also additional investment in capital cost for additional membrane area and pumping capacity. It can also result in shorter useful life of the membrane due to compaction effects and enhanced fouling that can occur at higher pressures and recoveries as a result of the concentration of scaling components near the surface of the membrane, particularly for membrane elements near the end of the process line where overall water recoveries are higher. Enhanced fouling increases the required frequency of membrane cleaning, increasing labor and chemical cost, and reducing throughput. For feeds with total dissolved solids (TDS) levels typical of seawater, recoveries approaching and beyond 50% are seldom feasible; for brackish water levels of TDS, recoveries beyond 80% are rarely economical, resulting in substantial waste of pretreated feed that must be returned to the source or alternately disposed.
Furthermore, membrane process equipment size is determined according to feed or concentrate flow requirements and decreases with increased recovery rate and lower feed concentration; conversely, pressure based membranes perform optimally, producing the best product quality and highest permeate flux rates, with low recoveries and low concentration feeds. Energy requirements are also directly related to feed pressures and feed water flow rates necessary to achieve a particular recovery. The design permeate flux rate predicted at a particular recovery likewise affects the number of pressure vessels, manifold connections, and size of membrane skid, as well as the size of the feed water supply systems and pretreatment equipment that are necessary.
Consequently, it is clear that a critical parameter that has the largest effect on investment and operating cost for pressure-driven membrane methods in most applications is the recovery rate ratio of permeate to feed. The feed flow is inversely proportional to the design recovery rate; therefore, the recovery rate directly affects the size and cost of all process equipment and power consumption. Higher recovery rate also contributes to reduced pretreatment capital cost and chemicals used. However, higher recoveries can increase membrane replacement cost as a result of fouling and compaction. Furthermore, pressure based membrane systems inherently perform better at lower feed concentrations and lower recoveries in which the osmotic pressure of the feed and its fouling and scaling potential are minimized.
In an electrodialysis (ED) process, separation, removal, or concentration of ionic species is accomplished by the selective transport of the ions through ion exchange membranes under the influence of an electrical field. Flowing through the series of anion and cation exchange membranes arranged in an alternating pattern between the electrodes having an electrical potential difference, the water diluate (D) feed stream (e.g., seawater for desalination), concentrate (C) stream, and electrode (E) stream are allowed to circulate in the appropriate cell compartments. Under the influence of the electrical potential difference, the negatively charged chlorides, sulfates, and other anions in the diluate (D) stream migrate toward the anode. These ions pass through the positively charged anion exchange membrane, but are rejected by the negatively charged cation exchange membrane and therefore stay in the C stream, which becomes concentrated with the ionic contaminants. The positively charged species such as sodium and other metals in the D stream migrate toward the cathode and pass through the negatively charged cation exchange membrane. These ions also stay in the C stream, being rejected by the anion exchange membrane. The E stream is the electrode stream (e.g., a sodium sulfate solution), which does not become contaminated with any ionic species from the diluate or concentrate streams, although small amounts of hydrogen are generated at the cathode and oxygen at the anode which are subsequently dissipated as the E streams are combined to maintain a neutral pH in the E stream holding tank. The overall result of the ED processing is an ion concentration increase in the concentrate stream with a depletion of ions in the diluted feed stream.
Multi-cell electrodialysis (ED) process stacks are generally built of membrane sheets separated from each other by suitably configured gaskets. For efficient separations, the distance (gap) between the sheets is as small as possible. In most designs, a spacer is introduced between the individual membrane sheets, both to assist in supporting the membrane and to help control the liquid flow distribution. The ED process stacks are typically assembled in the same fashion as a plate-and-frame filter press, the gaskets corresponding to the frames and the membrane sheets corresponding to the plates. The ED process stack configurations include flow channels for distribution of liquids to be treated to each of various layered compartments which are formed by ingenious patterns of mating holes and slots through the gaskets and the membranes prior to assembly of the ED process stack (see U.S. Pat. No. 6,537,436, Schmidt et al.).
In typical ED process stacks, the flow pattern within each compartment (i.e., between any two successive membranes) is determined by the configuration of the gasket and spacer elements used between the membranes. Two distinctively different flow arrangements are typically used. One is known as a tortuous-path design which can incorporate pressure differentials of up to about 125 pounds per square inch between inflow/outflow portions of the ED unit, while the other flow arrangement makes use of a sheet-flow principle which can incorporate pressure differentials up to about 50 pounds per square inch between inflow/outflow portions of the ED unit. ED process stacks include limitations to constant operation at high efficiencies. One design problem for both flow arrangements for multi-membrane and multi-cell stacks is that of assuring uniform fluid flow to the various compartments and effective transport of the separated ionic constituents to the membrane surfaces for removal from the ED process stack. These difficulties are obstacles to economical demineralization.
ED also has inherent limitations, working best at removing low molecular weight ionic components from a feed stream. Non-charged, higher molecular weight, and less mobile ionic species will not typically be significantly removed. This can be a disadvantage when potable water is produced from feed water sources having high suspended solids content or which are contaminated by microorganisms, which would require additional pre-treatment processes for removal prior to ED processing.
Furthermore, the concentration that can be achieved in the ED brine stream (concentrate or “C” stream) is limited by the membrane selectivity loss due to the Donnan exclusion mechanism and water transport from the dilute to the brine caused by osmosis; in particular, at very high concentrations, diffusion of ions from the concentrate stream back into the diluate stream and transport of water across the membranes can offset separation resulting from the applied electric potential, resulting in a poor (i.e., higher ion concentration than desired) product. However, in general, significantly higher brine concentration can be achieved by ED than by RO and the problem of scaling (i.e., precipitation of insoluble di- or multi-valent salts such as calcium sulfate) is less severe in ED than in RO since mono-valent ions are in general transported through the ion exchange membranes faster than multi-valent ions, resulting in a brine less concentrated in the multi-valent ions and so having less scaling potential. In contrast to RO, ED becomes less economical when extremely low salt concentrations in the product are required, as the current density becomes limited and current utilization efficiency decreases as the feed salt concentration becomes lower: with fewer ions in solution to carry current, both ion transport and energy efficiently greatly declines. Consequently, comparatively large membrane areas are required to satisfy capacity requirements for low concentration (and sparingly conductive) feed solutions.
Furthermore, at low feed concentrations, the reduction of ionic concentration polarization becomes an important design issue for ED membranes. Ionic concentration polarization is the reduction of ion concentrations near the membrane surface compared to those in the bulk solution flowing through the membrane compartment. With substantial ionic concentration polarization, electrolytic water splitting occurs due to the deficiency of solute ions adjacent to the membranes that carry the requisite electric current needed for ED membrane operation. The electrolytic water splitting is detrimental to ED process stack efficiency because of the tendency of ionic concentration polarization to occur at the membrane surface due to the hydrodynamic characteristic of channel flow providing thin viscous boundary layers adjacent to confining surfaces (i.e. adjacent membranes). The thin viscous boundary layers impose a resistance to passage of ions much greater than that of a layer of like thickness in a turbulent area of channel flow, and hence increase the likelihood of ionic concentration polarization at the membrane surfaces. Ionic concentration polarization is objectionable due to an inefficient increase in energy consumption without increasing removal of ionic constituents, requiring increased membrane area, along with pH changes in the feed and concentrate streams due to water splitting causing scale deposition in ED stacks.
In general, additional membrane area can be included in an ED process stack to counteract low separation efficiencies. However, the number of cells in an ED stack is limited by practical considerations of assembly and maintenance requirements. Since the failure of a single electrodialysis (ED) membrane can seriously impair stack performance, the necessity to be able to disassemble and reassemble a stack to replace membranes, and the necessity to be able to perform this quickly and easily, effectively limits the number of membranes that can be practically utilized in a stack. As a result, it is often desirable to use several smaller modular-size ED stacks rather than one large ED stack by using several small subassemblies having about 50 to 100 cell pairs (CP), and arranging as many as 10 of these subassemblies in series in a single clamping press. However, such a configuration increases capital costs and makes the process less economically feasible.
An alternative to utilizing modular-size ED stacks or NF or RO alone for separations is to use ED, UF, microfiltration (MF), RO, NF, distillation, evaporation, and other processes in combination with or as a pretreatment in various configurations. However, each process has drawbacks as discussed hereinabove, and prior utilized hybrid systems (e.g., RO coupled with distillation) for increased recovery have been treated as individual unit operations arranged in series sequence, with no interdependence (e.g., RO concentrate only affects operation of the distillation unit, with no reciprocal impact), with each individual process retaining its individual drawback (e.g., low recovery of RO, high operating cost of distillation.
Due to the inadequacies of each of the separate NF, RO and ED treatment systems for deionization, there exists a need for an integrated approach to deionization systems utilizing multiple types of highly efficient liquid treatment subunits including electrodialysis (ED) membrane units operated in integrated configurations with nanofiltration (NF) and/or reverse osmosis (RO) units as determined by an operator, with the feed liquids for each subunit being channeled through at least one mixing unit in order to blend numerous liquid streams into feed liquid streams having constituents optimized for removal of both TDS solids and ionized constituents by the integrated deionization system. The current invention is not a traditional hybrid process, but instead is an integral process, overcoming limitations inherent to both single processes by integrating the two individual unit processes into a single interdependent system. This integrated, interdependent system allows both the pressure-based membranes and ED membranes to operate at the optimum efficiency point of each, with both systems' operation configured to be optimally affected and enhanced by the presence of the other system.
BRIEF SUMMARY OF THE INVENTION
In accordance with the present invention, an integrated electro-pressure membrane (EPM) system is provided for treating contaminated feed liquids in order to generate decontaminated and deionized product liquids for use or for reuse in place of “virgin” liquids. The EPM system includes a pre-filtering step for the contaminated feed liquids, followed by blending the filtered liquids in a mixing unit, followed by any one of a plurality of treatment steps utilizing a NF treatment unit or a RO treatment unit operated in conjunction with an ED unit and the mixing unit.
Each disclosed embodiment of the integrated EPM system includes a central control means for an operator to control the fluid flow through respective filtering and treatment units in a parallel fluid flow configuration utilizing NF or RO units, with recirculation of reject liquid streams to at least one ED subunit. The EPM system is also readily operated in a sequential fluid flow configuration providing continuous flow through a pretreatment filtration unit, at least one ED unit, and a NF or RO unit. When operated in the sequential mode, the control means is adjustable to vary the voltage intensity supplied to the electric-driven membranes of the ED unit when a high purity decontaminated and deionized product liquid is desired.
The plurality of treatment units are maintained in fluidic interconnection and include a pretreatment unit, at least one mixing tank unit, at least one pretreatment filter unit, and one or more combinations of (a) a nanofiltration unit, or (b) a reverse osmosis unit, in combination with an electrodialysis unit disposed in fluid communication in series or parallel orientation. An operator provides input signals by control means for routing fluid flow through any one or more of the subunits (a) NF, (b) RO and/or (c) ED for generation of a product which is approximately 99% recovered relative to the input waste stream, a substantial improvement over the 70 to 96% recovery possible with conventional systems.
One embodiment of a membrane-based system for treating contaminated feed liquids includes an initial step of providing a pretreatment filtration unit through which contaminated feed liquids are filtered with a selected volume of pretreated filtrate liquid being channeled to a mixing unit for mixing with additional pretreated and recycled filtrate liquids. A step of transferring includes transferring through appropriately sized fluid conduits a selected volume of the mixed pretreated filtrate liquids to a second treatment unit consisting of an ED unit, a nanofiltration unit, or a reverse osmosis unit. If the second treatment unit is an ED unit, the pretreated filtrate liquids are electrically activated and are directed along a tortuous fluid path between a plurality of ED membranes, spacers, and gaskets whereby an ionic concentrate liquid is separated and removed from the filtrate liquids forming a decontaminated product liquid; channeling the ionic concentrate liquid for mixing with a diluate liquid stream and directing the liquid mixture through a pressure driven membrane unit providing pressure induced liquid transfer across permeable membranes while excluding passage of a specified size or ionic charge of contaminants by the pressure driven membrane unit to generate a decontaminated liquid for storage, and a concentrated reject liquid redirected to the mixing unit for blending and additional treatment in the NF or RO units, or in the ED unit, depending on constituents remaining in the blended concentrated reject liquid.
Feed rate to the surge tank and permeate flow rate out of the system can be constant, thus making it a continuous process, or feed to the tank can be batch-wise added, making the system a semi-continuous process. Feed and product salinity may be controlled as desired by adjusting ion-exchange membrane and pressure membrane areas of the ED unit and the NF or RO unit, respectively, to continuously remove and concentrate the desired mass of salt necessary to optimize performance of the EPM system. Furthermore, in addition to optimizing the respective ED and NF or RO membrane areas, the selection of membrane types for the ED, NF, or RO best suited for the particular desalting application's performance specifications, and offering the operational synergy between the ED and NF or RO units, provides the basis for optimizing the EPM system to provide the least cost and/or highest performance, integral desalting system. Consequently, this integrated apparatus and method may be used to retrofit and optimize performance of existing NF and RO treatment systems.
Furthermore, the proposed current EPM process also eliminates the need for additional staging of both NF or RO as well as the ED component, which differs from other desalting processes in the degree of desalting achieved in a single stage. NF or RO or ion exchange desalination may require more than one pass to achieve desired product quality. In ED the degree of desalting will usually be limited to 50% per pass, and some type of staging is needed for further desalting. This is normally achieved by passage through additional stacks or internal electric and/or hydraulic stages in one stack assembly. Batch recirculation is simplistic and the least capital cost intensive arrangement. Batch recirculation with ED alone however is less effective because of the lack of steady state, the high power requirements, and variable current density necessary. Variable current density leads to current efficiencies outside of the optimal range in stand alone ED processes. The novel integrated EPM process overcomes this limitation where a constant state of high current utilization efficiency may be maintained.
Another advantage of the proposed invention is that a more optimum feed concentration is maintained for both units, ED and NF or RO of the process. In the traditional continuous NF or RO system, as permeate is recovered, increased salt concentration is fed to the next membrane element in the system, resulting in decreased flux and lower product quality from that element. In a batch system in which concentrate from the NF or RO elements is returned to the feed tank, the concentration in the feed tank also increases over time, resulting in decreased water permeate flux and product quality for all membrane elements in the system. In the current invention, both in continuous and batch operation, the coupled ED unit works to decrease the concentration in the feed tank, resulting in a feed to the NF or RO unit with lower salt concentration, thus allowing higher permeate flux and product quality. In addition, as concentrate from the NF or RO unit is returned to the surge tank, it helps to maintain a constant salt concentration in the tank, allowing feed concentration to the ED unit to be maintained at a level sufficient to provide good current efficiencies for transport of ions. Consequently, both systems operate in the more optimum and energy efficient range for maximizing production and product quality.
A further benefit of the EPM process is that scaling components and subsequent NF or RO scaling is minimized. The ED unit actively transports multi-valent ions such as calcium and sulfate across the ED membranes, maintaining these at a constant or lower level than would be observed if NF or RO alone with multiple stages or concentrate recycle were employed. As a result, reduced concentrations of multi-valent ions such as calcium and sulfate which tend to scale and foul NF or RO membranes are reduced, leading to improved production rate and permeate characteristics, increasing the time required between cleaning operations, and providing longer NF or RO membrane life.
Another benefit of the current invention is that improved recoveries are possible compared to NF or RO only systems. Recoveries as high as 99+% are possible using EPM since the feed concentration is maintained at relatively constant level due to the combined separation actions of each sub-system. Since feed concentration is relatively constant, the osmotic pressure, and so productivity, of the NF or RO membranes remain constant over the entire processing time (for batch) or recovery range (for continuous systems), allowing almost complete reclamation of the feed. The resulting enhanced recovery can greatly improve the economic feasibility and cost effectiveness of a variety of desalination operations. Cost components of interest affected by improved recovery include pretreatment costs, value of recovered product, cost of disposal of concentrate, capital cost, and energy cost required to perform the additional recovery.
Another advantage of the current invention is improved product quality compared to NF or RO or ED only systems. Since the feed concentration is relatively constant over the whole range of recoveries, the rejection of the salts and productivity of the NF or RO remains constant, resulting in improved permeate product compared to NF or RO only systems in which the permeate product quality would decrease as a function of recovery.
Another advantage is lower energy requirements compared to ED only systems. While ED only systems are capable of 99+% recovery, treatment to achieve low concentrations or treatment of dilute or sparingly conductive solutions results in low energy efficiencies and the need for decreased production rate or increased membrane area and capital costs. The EPM integrated system ensures that each sub-system operates in the feed concentration range where it is most energy efficient and removal effectiveness for each subsystem is optimal, resulting in lower energy operating costs.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
The above-mentioned features of the invention will become more clearly understood from the following detailed description of the invention read together with the drawings in which:
FIG. 1 is a flow diagram of one embodiment of a typical ED only system for comparison with the present invention, illustrating pretreatment and recycling operations with an ED unit coupled with microfiltration;
FIG. 2 is a flow diagram of another embodiment of a typical ED only system of FIG. 1 , including flow through pretreatment filtration and pressurized filter treatment in conjunction with an ED unit;
FIG. 3 is a flow diagram of the current invention EPM system, including parallel operation of an ED unit, a filtration unit, and a NF or RO unit with a single mixing tank serving as feed to both units;
FIG. 4 is a flow diagram of an additional embodiment of the EPM system of FIG. 3 including sequential liquid flow through an ED unit and a NF or RO unit with a single mixing tank serving as feed to both units;
FIG. 5A is a schematic view of one embodiment of an EPM system illustrating a plurality of liquid treatment units including a NF/RO unit and an ED unit controlled by a central control means;
FIG. 5B is a flow diagram of the embodiment of FIG. 5A , including sequential liquid flow through a NF or RO unit and an ED unit controlled by a central control means;
FIG. 6 is a graphical representation of reduction in product conductivity of permeate by an integrated EPM system compared to a NF only system or an ED only system;
FIG. 7 is a graphical representation of energy use by an integrated EPM system during generation of permeate compared to a NF only system or an ED only system;
FIG. 8 is a graphical representation of relative production rate for an integrated EPM system treating feed liquids of about 50% ethylene glycol compared to a NF only system or a ED only system;
FIG. 9 is a graphical representation of total cost savings for an integrated EPM system compared to a NF only system or an ED only system; and
FIG. 10 is a graphical representation of permeate conductivity verse recovery for an integrated EPM system compared to a NF only system or an ED only system.
DETAILED DESCRIPTION OF THE INVENTION
In the embodiments illustrated in FIGS. 3 , 4 , 5 A, and 5 B of the integrated electro-pressure membrane (EPM) systems 14 , 16 , 18 , and 18 ′, provide treatment of contaminated feed liquids 22 such as glycol based thermal transfer liquids in which ionized constituents are present along with metals and other insoluble contaminants and soluble or colloidal contaminants. Typical candidates for treatment by an EPM system includes feed liquids such as industrial wastewaters, industrial-grade spent ethylene glycol, other glycol/water mixtures used in vehicular engine coolant systems, out-of-specification liquids from pharmaceutical production, and/or waste organic chemicals from petrochemical industries including certain solvent liquids deemed valuable if recovery and recycling of the solute and solvent are not cost-prohibitive. Desalination of brackish water and seawater is also a possible application. Furthermore, the EPM process should not be limited to use of ED as minor modifications through the use of bi-polar membranes to recover acids and bases from corresponding salts is possible. Similarly, the EPM process may employ non-conventional electro-deionization methods, for instance continuous deionization (CDI), in conjunction with NF or RO as well.
Membrane-based deionizing technologies may be categorized as pressure-driven membrane units, UF, NF and/or RO, and as electrical-driven ED units. Operation of a pressure-driven process utilizes a plurality of semi-permeable membranes to separate one constituent of a solution from another by means of constituent size exclusion and pressure. A filtration unit 20 having at least one filtration membrane, and/or filtration media such as layers of screens or porous material, is typically utilized with sufficient pore diameters to deny passage of insoluble particles, oils and/or organics over 1,000 molecular weight (MW), and optimally operates for selective separation of constituents in a range between about 30 Angstroms (Å) to about 1000 Å, while passing smaller ions along with water. A RO unit 50 is typically utilized for separation of constituents in the range between about 1 Å to about 20 Å. A RO unit 50 is typically operated at pressures of about 200 to about 1000 pounds per square inch maintained between inflow/outflow portions of the RO unit 50 . A NF unit 44 is typically utilized to provide separation of ions and selected organic compounds from water in a size range between UF and RO treatment. NF membranes have a wide range of performance characteristics and typically provide removal of constituents in a range between about 8 Å to about 200 Å, depending on the selectivity of the NF membranes. A pressure-driven NF unit 44 is typically operated to maintain fluid pressures between about 50 pounds per square inch to about 1,000 pounds per square inch maintained between inflow/outflow portions of the NF unit 44 . One preferred EPM system includes a NF unit 44 or a RO unit 50 capable of operations to maintain fluid pressures between about 50 pounds per square inch to about 400 pounds per square inch for low pressure fluid treatment applications. Another preferred EPM system includes a NF unit 44 or a RO unit 50 capable of operations to maintain fluid pressures between about 400 pounds per square inch to about 1,000 pounds per square inch for high pressure fluid treatment applications.
An ED system can be operated for removing low molecular weight ionic constituents of between about 1 Å to about 10 Å from a feed stream. As a contaminated and pressurized liquid is pumped through an ED membrane cell stack 68 having a plurality of interleaved with spacer layers, gaskets, and at least one anion plate and at least one cation plate, the ionic constituents are transported toward the respective anion plate and cation plate under the influence of an electric field for removal of the ionic constituents from the liquid to form a diluate liquid referred to as a decontaminated product liquid 76 . A disadvantage of an ED operation is that non-charged constituents and higher molecular weight contaminants are not typically efficiently removed by an ED unit. Conversely, NF and/or RO subunits will operate optimally to remove highly charged and some non-charged constituents and higher molecular weight contaminants, but will not typically be as efficient at removing smaller molecular weight and mono-valence charged constituents from a feed stream. The commonality of combining NF or RO subunits in series or in parallel with an ED unit, and providing for pretreatment and blending in a central mixing tank allows for optimal separation of contaminants and ionized constituents by each subunit, resulting in significant energy savings compared to thermal separation processes such as distillation or evaporation, and substantial operational cost savings compared to ion-exchange resin process units. The integrated EPM system provides a plurality of treatment units including a multi-cell electrodialysis unit 60 which removes ionic constituents and provides treatment of the NF or RO reject liquids 72 ′ after blending in a mixing unit 30 thereby allowing multiple treatment options and providing maximum recovery efficiency.
For each of the ED membrane units 60 utilized in treatment systems 10 , 12 , 14 , 16 , 18 and 18 ′, an ED membrane cell stack 68 typically includes a plurality of stacked membrane layers having interdisposed spacers, gaskets and turbulence layers. Each ED membrane stack 68 (see FIG. 5A ) includes at least one inlet and at least one fluid outlet for rapid liquid flow therethrough while an electric potential is maintained across the stacked layers by at least one positive electrode or plate 62 and at least one negative electrode or plate 62 ′. Pumps associated with each ED membrane cell stack 68 include a concentrate liquid pump 64 and an electrolytic liquid pump 66 (see FIG. 5A ). Each ED unit 60 is capable of operating with constant flow or batch fluid flow during treatment in sequence (see FIGS. 2 , 4 and 5 B), or during treatment in parallel (see FIGS. 1 and 3 ). A plurality of arrangements of ED membranes interleaved with spacers, gaskets and turbulence inducement layers are combined in stacked configuration 68 depending upon the amount of membrane surface area desired for each ED unit. In one embodiment of the integrated EPM system, ED membranes are separated by spacers composed of ethylene propylene diene terpolymer (EPDM). Those skilled in the art will recognize that a variety of materials are readily available for ED membranes and gaskets utilized in an ED stack 68 . Clamping of the ED membranes and gaskets together in an ED stack is accomplished by perimeter oriented connectors, or centrally oriented connectors extended through the ED membranes and gaskets, in order to improve the uniformity of the clamping force distribution on the ED gasket area. Threaded connector members are preferably utilized as connectors to reduce assembly labor time for each ED stack 68 used, and to facilitate change-out of ED membranes when the membranes are spent.
One embodiment of the integrated electro-pressure membrane (EPM) system 14 includes parallel treatment of contaminated feed liquids 22 utilizing pressure-driven membrane units 44 , 50 having a plurality of pressure-driven membranes through which liquids from the mixing tank 30 are channeled, and at least one electrodialysis membrane unit 60 (see FIG. 3 ). A volume of contaminated feed liquids 22 is pumped 32 through a pretreatment filtration unit 20 , for removal of micron-sized particles before transfer from at least one effluent channel of the filtrate 28 to the mixing tank 30 . Either within the mixing tank 30 or partially external of the mixing tank, a means for mixing is provided in order to rapidly mix the filtrate 28 and additional fluids returned to the mixing tank 42 ′, 58 ′, 72 , 72 ′ (discussed further herein). The means for mixing can include a mechanical mixing device having an interior rotating or pivoting member, an interior vibrating member, an interior fluid channel outlet from recirculating pumps, or a similar mixing device as known by those skilled in the art. The integrated EPM system 14 includes an operator adjusted control means 80 providing liquid transfer 58 from mixing tank 30 into an ED unit 60 for electric-driven liquid treatment. A deionized liquid 58 ′ is generated and returned to the mixing tank 30 in order to reduce the concentration of ionic constituents in feed liquids in the mixing tank 30 before mixed liquids are transferred 38 and pressurized by the second pump means 36 to the NF unit 44 , or to a RO unit 50 , for pressure-driven removal of contaminants. A polishing step is provided for liquids transferred through a micron filter unit 40 concurrent with operation of the ED unit 60 , in which an operator selects transfer 42 of mixed liquids through micron filter unit 40 or a UF unit before a filtrate 42 ′ is transferred back to a mixing tank 30 for subsequent transfer 34 , pressurization by the second pump means 36 , and transfer 38 for pressure-driven treatment in NF unit 44 , or RO unit 50 , if utilized. The maximum practical efficiency of a typical nonintegrated ED unit is typically about 90% to about 96% removal of ionic constituents. Testing results 90 , 92 have provided efficiency values for the diluate forming the decontaminated product liquid 76 recovered from integrated EPM embodiments 14 , 16 , 18 , and 18 ′ (see FIGS. 3 , 4 , 5 A, and 5 B), including treatment in a NF 44 or a RO unit 50 , and an ED unit 60 , of about 98+% efficiency 92 over a significantly short run time (see FIG. 6 ).
Additional configurations for combining the two sub-systems include providing sequential treatment of liquids (see FIGS. 4 and 5B ), or parallel treatment of liquids (see FIG. 3 ), in numerous combinations of an ED unit 60 and a NF unit 44 , or a RO unit 50 if utilized, and a liquid mixing tank 30 . For each integrated EPM system disclosed herein, when the feed rate 28 to the mixing tank and the effluent flow rate for decontaminated product liquid 76 are generally constant, the treatment system is identified as a continuous process. When the feed rate 28 to the mixing tank 30 includes sequential batch volumes, the system is classified as a semi-continuous process. For each integrated EPM system, the volume and conductivity is monitored by sampling devices such as conductivity sensors reporting to control means 80 for specific liquid transfers within the system, such as mixed liquids transfer 38 to the NF or RO units, and liquids transfer 58 to the ED unit 60 . In addition, monitoring of the filtration pressures for the NF or RO units, and the strength of electrical field(s) for each ED unit 60 are monitored and controlled by the control means 80 which includes computer circuitry for multiple analyses of liquids during transfers, of liquids blended in mixing unit 30 , and of liquids after each treatment unit. The control means 80 and includes visual readouts of the liquid conductivity and pressure parameters for each subunit, and adjustable controls 82 for operating each unit of the integrated EPM system. The visual readouts and controls 82 allow an operator to monitor performance of each unit during operation and provide a control means for an operator to increase or decrease the operating parameters of mixing tank 30 , the NF unit 44 , the RO unit 50 if utilized, and the ED unit 60 .
Each integrated EPM system utilizes a common mixing tank 30 from which feed liquids are transferred 34 , 58 to each of a plurality of treatment units 40 , 44 , 50 and 60 . Control of the liquids added to the common mixing tank 30 by an operator's adjustments of control means 80 , provides for optimized parameters of low concentrations of non-ionic contaminants and control of mixed liquids conductivity when liquids are transferred to each treatment unit 40 , 44 , 50 , 60 , thereby providing improved overall system efficiency as measured by a decrease in decontaminated product liquid 76 conductivity (i.e. removal of ionic constituents). Actual performance parameters of the integrated EPM system 90 , 92 have been tested to maintain about 98+% recovery efficiency during integrated system operations, as compared to a NF only system 110 , 112 (about 90%), or an ED only system 120 , 122 (about 90% to about 96%) over similar run times ( FIG. 6 ). Use of a common mixing tank 30 , as opposed to two or more separate filtrate and permeate storage tanks, provides a central control of feed liquid flow, and allows for rapid adjustments to the system run time for optimizing reduction in permeate conductivity during run time to maintain performance at 98+% while minimizing energy usage for the integrated EPM system 90 , 94 , compared to a NF only system 110 , 114 , or an ED only system 120 , 124 over similar run times (see FIG. 7 ).
The integrated system illustrated in FIG. 4 is a sequential process having a filtration unit 40 operating in parallel with operation in series for the ED unit 60 and NF unit 44 , or a RO unit 50 . Contaminated feed liquids 22 having ionic constituents and non-ionic constituents are pumped 32 through a pretreatment filtration unit 20 , for removal of micron-sized particles and delivery of the filtrate 28 to the mixing tank 30 . The integrated EPM system 14 includes an operator adjusted control means 80 providing control of the mixed liquid transfer 58 into the ED unit 60 for electric-driven liquid treatment. Treatment in the ED unit 60 provides for generation of a deionized product liquid 76 which is released for reuse in commerce, and concentrated brine 74 which is removed for discard. Additional effluents from the ED unit 60 can include a non-specification liquid portion 72 (see FIGS. 1 and 2 ) which is transferred by a recycle channel to the mixing tank 30 , or discarded. Alternative pathways for partially deionized fluids 58 ′ are illustrated in FIGS. 3 , 4 and 5 B, with the effluent 58 ′ from the ED unit 60 being transferred to pressure-driven filtration units 44 or 50 (see FIG. 4 ), or the partially deionized fluids 58 ′ being transferred by recycle channels for mixing in the mixing tank 30 (see FIG. 5B ), The deionized diluate liquid 58 ′ is transferred and pressurized by the second pump means 36 for pressure-driven treatment in the NF unit 44 , and/or in a RO unit 50 if utilized, to generate a pressure-driven membrane separation of non-ionized constituents to generate a permeate liquid identified as the decontaminated product liquid 76 . A second non-specification liquid portion 72 ′ is generated and transferred after NF or RO treatment to the mixing tank 30 for blending with pretreated liquid 28 and filtrate liquid 42 ′ in order to reduce the concentration of ionic constituents in feed liquids in the mixing tank 30 before mixed liquids are transferred 38 and pressurized by second pump means 36 to the NF unit 44 , or to a RO unit 50 , for pressure-driven removal of non-ionized contaminants. A deionized and decontaminated product liquid 76 is generated by the integrated system 16 which is reduced in conductivity at an overall efficiency of about 98+%, when compared to a NF only system 110 (approximately 90% efficient 112 ), or an ED only system 120 (approximately 96% efficient 122 ) over similar run times (see FIG. 6 ).
In FIG. 5A , an equipment configuration 18 is illustrated for equipment typically utilized for each of the treatment units of the integrated EPM system 16 . All of the treatment units of FIG. 5A are not required for operation of integrated EPM systems. The control means 80 provides a means for an operator's control and shut-down of treatment units not needed for treating feed liquids 22 lacking certain contaminants. The integrated system optimizes treatment options while delivering energy cost savings by selectively channeling filtered and mixed liquids 42 ′, 58 by activation of appropriately positioned valves and pumps to allow liquid flow to appropriate system units as selected by an operator having knowledge of the composition of the mixed liquids 42 ′, 58 in conjunction with knowledge of the current operational performance parameters of each system unit. The specific treatment units of FIG. 5A are discussed further herein for the embodiments illustrated in FIGS. 3 , 4 , and 5 B.
An additional embodiment for an integrated system 18 ′ is illustrated in FIG. 5B , which utilizes the equipment and control means 80 illustrated in FIG. 5A . The integrated system 18 ′ is a sequential process providing liquid treatment in a NF unit 44 or a RO unit 50 , followed in series by liquid treatment in an ED unit 60 . Contaminated feed liquids 22 having ionic constituents and non-ionic constituents are pumped 32 through a pretreatment filtration unit 20 , for removal of micron-sized particles and delivery of the filtrate 28 to the mixing tank 30 for blending of a variety of concentrated liquids. The goal is to manage separate concentrated liquid streams 58 ′, 72 ′ in order to reduce the average concentration of ionic constituents and dissolved solids in mixed liquids transferred 34 to additional treatment units 44 , 50 , 60 . The integrated system 18 ′ provides for blending in the mixing tank 30 of two or more liquids including the pretreated feed liquids 28 , deionized product liquids 58 ′ from an ED unit, and non-specification liquids 72 ′ from treatment in a NF or RO unit, in order to reduce the average concentration of ionic constituents and dissolved solids in permeate liquids in the mixing tank 30 before treatment. The mixed liquids are transferred 34 and pressurized by the second pump means 36 for transfer 38 to a NF unit 44 , or to a RO unit 50 , for pressure-driven removal of constituents such as inorganic compounds and soluble contaminants such as synthetic dyes and organic compounds. If a decontaminated product liquid 76 ′ is needed which is not deionized, then an effluent product liquid 76 ′ is separated from the NF/RO unit for use in commerce. If additional deionization treatment is preferred, the pressure treated liquid 58 ″ is transferred to an ED unit 60 for deionization and separation as decontaminated and deionized product liquid 76 . The integrated EPM system 18 ′ includes an operator adjusted control means 80 providing transfer of the reject liquid 72 ′ from the NF/RO unit to the mixing tank 30 , and transfer of a partially deionized fluid 58 ′ from the ED unit 60 to the mixing tank 30 for further mixing and additional treatment. The final product can be either the NF or RO treatment unit effluent separated as a product liquid 76 ′, or the decontaminated and deionized product liquid 76 from the ED unit 60 . Either product liquid 76 , 76 ′ is decontaminated at efficiencies of at least 98%, for production of reclaimed liquids having sufficient purity to meet “virgin” liquid specifications.
Benefits of the integrated EPM systems described herein include high production rates for decontaminating ethylene glycol with recovery rates in excess of 98%, with high gallons per hour (gph) throughput as illustrated for an integrated EPM system 96 , compared to NF only 116, or ED only 126 systems (see FIG. 8 ). Additional benefits for the integrated EPM systems include relatively low capital expenditures and operating costs, leading to significant total cost savings of about 75% for integrated EPM systems 98 having recovery efficiencies of 98+%, compared to the costs to obtain a maximum practical NF only recovery efficiency of about 90% for NF only systems 118 (see FIG. 9 ). Alternately, significant total cost savings of about 65% for integrated EPM systems 100 having recovery efficiencies of 98+% for integrated EPM systems 98 , compared to the costs to obtain a maximum practical recovery efficiency of about 96% for ED only systems 128 (see FIG. 9 ). The integrated EPM systems typically do not generate hazardous by-products, are easy to operate, control and automate, and easy to maintain. Also, studies indicate that the invention is capable of producing a product with extremely low conductivity levels (down to as low as 2.6 μMho/cm). Those skilled in the art will recognize that this represents a substantial improvement compared to traditional ED designs, which are typically limited to product with conductivities >30 μMho/cm. As a result, the invention would represent a new pretreatment option for production of ultra-pure water. The results of a plurality of production runs of varying lengths and with different configurations of treatment units are illustrated in FIGS. 6-10 . Production runs have indicated that the embodiments of the integrated EPM system are a substantial improvement over traditional designs. As illustrated in FIG. 10 , comparisons of permeate conductivity as a function of recovery for feed liquids of 50% ethylene glycol solution, indicate that the integrated EPM systems 130 readily perform at 98+% efficiency 140 , compared to RO only systems 132 providing about 96-97% efficiency 142 , or NF only systems 134 providing about 90-97% efficiency 144 . Those skilled in the art will recognize that the improved design of the integrated EPM systems result in each ED membrane cell stack requiring significantly less ED membrane area while being more energy efficient.
In addition to the described use of the method and apparatus to decontaminate and deionize used antifreeze, the system may be used to decontaminate and deionize wash water (vehicular, laundry, mop water, trailer/tank washout, textile rinses, metal, aqueous parts cleaners), oil and gas field fluids (glycol base natural gas dehydration fluids, glycol/water heat transfer fluids, amines from treatment of natural gas, produced water), other thermal transfer fluids (secondary coolants from HVAC systems and coolants from ice-skating rinks), cooling water reuse, nuclear wastewater, mixed wastewater having nuclear/radioactive and hazardous/chemical contaminates, hazardous wastewater, desalination of sea or brackish water, and drinking water production and/or provide pretreatment for ultra-pure water production.
While the present invention has been illustrated by description and while the illustrative embodiments have been described in considerable detail, it is not the intention of the applicant to restrict or in any way limit the scope of the appended claims to such detail. Additional advantages and modifications will readily appear to those skilled in the art. The invention in its broader aspects is therefore not limited to the specific details, representative apparatus and methods, and illustrative examples shown and described. Accordingly, departures may be made from such details without departing from the spirit or scope of applicant's general inventive concept.
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An integrated treatment system using electrodialysis and pressure-driven membranes for deionizing and decontaminating liquids to a near-pure quality for use or reuse in industrial or municipal operations. The integrated system includes steps of pre-filtering contaminated feed liquids blending the filtered liquids in preparation for treating the mixed liquids in parallel or sequential treatment steps utilizing nanofiltration or reverse osmosis, proceeded by or followed by an integrated electrodialysis treatment. A control means selectively directs mixed liquids to each of the treatment units for treatment in parallel or in series depending on the conductivity and residual contaminants in the mixed liquids. In comparison with nanofiltration or reverse osmosis only systems, or electrodialysis only systems, the integrated system provides improved efficiencies for treatment, requires less energy to operate, and reduces maintenance and capital costs.
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RELATED APPLICATION
This application is a division of U.S. patent application Ser. No. 10/053,182, filed Jan. 16, 2002, now U.S. Pat. No. 7,066,285.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention pertains to methods and compositions for preventing or alleviating the loss of drilling fluids into a subterranean formation during drilling of boreholes in said formation.
2. Description of Relevant Art
In the oil and gas industry, a common problem in drilling wells or boreholes in subterranean formations is the loss of circulation (of fluids, such as drilling fluids or muds) in a well or borehole during the drilling. Such lost fluids typically go into fractures induced by excessive mud pressures, into pre-existing open fractures, or into large openings with structural strength in the formation.
A large variety of materials have been used or proposed in attempts to cure lost circulation. Generally, such materials may be divided into four types or categories: fibrous materials, such as shredded automobile tires or sawdust; flaky materials, such as wood chips and mica flakes; granular materials, such as ground nutshells; and slurries, whose strength increases with time after placement, such as hydraulic cement.
Another type of slurry that thickens downhole is made, typically, by dispersing a polyacrylamide in water and then emulsifying the dispersion in a paraffinic mineral oil, typically using a polyamine as an emulsifier. Bentonite is commonly added to such a slurry where it remains in the external or oil phase of the slurry. At normal shear rates, the bentonite rarely if at all contacts the water so the slurry remains relatively thin while being pumped down the drill pipe. At higher shear rates such as prevailing at the drill bit, the emulsion breaks and the bentonite mixes with the water. Crosslinking by the polyacrylamide results in a semi-solid mass that thickens further with the bentonite as it is pumped into cracks and fractures in the formation to block the lost circulation.
Although many materials and compositions exist and have been proposed for preventing lost circulation, there continues to be a need for more versatile and better compositions and methods for preventing loss of circulation.
SUMMARY OF THE INVENTION
The present invention provides an improved composition for preventing or alleviating loss of drilling fluids or circulation in a wellbore penetrating a subterranean formation. The composition is comprised of a blend of a resilient, angular, carbon-based material and a water-swellable, but not water-soluble, crystalline synthetic polymer. Preferred carbon-based materials comprise resilient graphite carbon particles and ungraphitized carbon particles. Preferred synthetic polymers comprise polyacrylamide. The most preferred polymers comprise a dehydrated crystallized form of cross-linked polyacrylamide that will readily hydrate following exposure to water or aqueous based fluids. Such hydration may be delayed by salts in the water, such as the use of brine or addition of calcium chloride for example.
The method of the invention uses the composition of the invention in preventing or alleviating loss of drilling fluid or other fluid circulation in a wellbore penetrating a subterranean formation. In the method, the composition is preferably provided in a weighted or unweighted “pill” for introduction into the wellbore. Such “pills” typically comprise such composition blended with a small amount of drilling fluid or brine. The amount of such composition used in such pill will depend on the size of the subterranean fracture, opening, or lost circulation zone to be treated. Multiple pills or treatments may be used if needed. Preferably drilling is stopped while the pill comprising the composition of the invention is introduced into and circulated in the wellbore. The composition of the invention will enter lost circulation zones or porous or fractured portions of the formation where it will prevent or retard the entry of drilling and other wellbore fluids.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
According to the prevent invention, an unexpected synergy and improved lost circulation material may be obtained by combining two materials or compositions that have previously been known to be effective in preventing or alleviating lost circulation, but that are not individually as effective as the combination. The two components effecting such synergy are resilient, angular carbon-based material and water swellable but not water-soluble crystalline polymer.
The preferred carbon-based material preferably has a particle size that is about 95% greater than 200 mesh and about 100% less than 40 mesh. The preferred carbon-based material is preferably a dual-composition of resilient graphitic carbon particles and ungraphitized carbon particles, where preferably the quantity of resilient graphitic carbon particles exceeds the quantity of ungraphitized carbon particles or in any case where the overall composition is resilient. Carbon particles or carbon-based materials are considered resilient for purposes of the present invention if they rebound by at least about 20 volume percent when a compaction pressure of 10,000 psi is applied. A most preferred carbon-based material that is commercially available is STEELSEAL™, available from Halliburton Energy Services, Inc. in Houston, Tex., U.S.A.
The preferred synthetic polymers comprise polyacrylamide. The most preferred polymers comprise a dehydrated crystallized form of cross-linked polyacrylamide that will readily hydrate following exposure to water or aqueous based fluids. Such hydration may be delayed by salts in the water, such as with the use of brine or addition of calcium chloride for example. A most preferred crystalline polymer that is commercially available is DIAMOND SEAL™, also available from Halliburton Energy Services, Inc. in Houston, Tex., U.S.A.
STEELSEAL™ has tightly packed particles that can expand and contract under compression in pores and fractures of a subterranean formation without being dislodged or collapsing due to changes in differential pressures. STEELSEAL™ is known to be useful as a lost circulation additive for synthetic and oil-based drilling fluids to stop circulation losses in porous and fractured formations. STEELSEAL™ is also known to be effective in water-based or aqueous based fluids as a lost circulation additive and as a solid lubricant for torque and drag reduction.
DIAMOND SEAL™ is 100% crystalline synthetic polymer having the ability to absorb hundreds of times its own weight in water. For example, in fresh water, DIAMOND SEAL™ can swell 3.5 cubic feet per pound. DIAMOND SEAL™ particles are sized such that about 96% pass through 5 mesh (4.0 ml). DIAMOND SEAL™ is known to be effective at mitigating lost circulation, particularly in horizontal or directional drilling, and it can stabilize boreholes in unconsolidated formations.
The composition of the present invention comprises combinations of STEELSEAL™ and DIAMOND SEAL™ that are more effective at alleviating or preventing lost circulation than either of these components are individually, as demonstrated by the test data below. Further, the composition of the invention is effective without addition of reinforcing materials or other fibers. Moreover, the composition of the invention can provide effective bridges across even large, problematic fractures.
Various concentrations of STEELSEAL™ and DIAMOND SEAL™ were tested as shown in Table I. These two components were blended together and then added to a 14 pounds per barrel (ppb) freshwater mud and mixed for five minutes in a multimixer. The mud was then tested in a HPHT at 200 degrees Fahrenheit with a one hour heat lamp and 500 psi differential pressure using a 190 micron disc. The relative filtrate was then collected and measured.
TABLE I
Spurt
Total Relative Filtrate
Treatment
1 min., mls.
(30 × 2), mls.
80 ppb STEELSEAL ™
6
50
0 ppm DIAMOND SEAL ™
70 ppb STEELSEAL ™
5
12
10 ppb DIAMOND SEAL ™
(treated with 2000 ppm glyoxal)
in a dispersed mud
70 ppb STEELSEAL ™
5
10
10 ppb DIAMOND SEAL ™
(treated with 2000 ppm glyoxal)
78 ppb STEELSEAL ™
5
39
2 ppb DIAMOND SEAL ™
(treated with 5000 ppm glyoxal)
78 ppb STEELSEAL ™ FINE
6
25
2 ppb DIAMOND SEAL ™
0 ppb STEELSEAL ™
12
59
10 ppb DIAMOND SEAL ™
As used herein, ppb = pounds per barrel and ppm = parts per million.
As the data in Table I shows, enhanced reduction in filtrate (indicating good performance as a lost circulation material) is seen with the combination over and above the performance of either material alone. The performance reflects a surprising synergy in the combination that is not suggested by or apparent from just combining the performance of either material used alone.
Also as shown in the experimental data above, other materials or components may be added to the combination of the components of the invention. For example, glyoxal may be added to facilitate the combination of the components. Moreover, the data shows the composition of the invention is effective at high temperatures, particularly temperatures typically encountered at intermediate wellbore depths of less than about 15,000 feet. Such intermediate depths are where most lost circulation typically occurs, if at all, during drilling for the recovery of hydrocarbons.
In the composition of the invention, the most preferred quantity of STEELSEAL™ to DIAMOND SEAL™ is about 90:10 although ranges of STEELSEAL™ of about 70 pounds per barrel (ppb) to about 90 ppb and of DIAMOND SEAL™ of about 2 ppb to about 10 ppb are also preferred. The composition of the invention may be used in, added to, or blended in any water or aqueous based drilling fluid or mud, including for example brines and aqueous fluids comprising salts as well as fresh water.
According to the method of the invention, the composition of the invention is used as a lost circulation material. That is, a pill or plug comprising the composition of the invention is introduced into the wellbore and allowed to circulate through the wellbore at least to the zone needing lost circulation treatment or to the zone where lost circulation is believed to likely occur. The composition of the invention is then allowed to enter such zone. Such zone may be or may comprise or include, without limitation, fractures and porous formations. In such zone, the composition of the invention reduces, eliminates or prevents the entry of drilling fluid and/or other well fluids into said zone.
The foregoing description of the invention is intended to be a description of preferred embodiments. Various changes in the details of the described composition and method can be made without departing from the intended scope of this invention as defined by the appended claims.
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An improved composition and method is provided for preventing or alleviating lost circulation during the drilling of wellbores in subterranean formations, and particularly during the drilling of oil and gas wells. The method is suited for horizontal and directional wells as well as more vertical wells. The composition of the invention comprises a synergistic blend of resilient, angular, carbon-based material and a water-swellable, crystalline synthetic polymer. The method employs the composition of the invention in preventing lost circulation.
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BACKGROUND OF THE INVENTION
When a pot is heated on the top surface of a flat top electric heating range, it is often desirable to measure the temperature of the bottom surface of the heated pot. It is known that such heated surface emits infrared radiation. The present invention is directed toward apparatus for measuring such radiation and converting this measurement in to a corresponding temperature measurement.
The relationship between the temperature of a hot object as measured in degrees of temperature T, using the Kelvin temperature scale, and its spectral radiance L, when this relationship is measured using a wavelength of observation w, is defined by the well known Planck formula L[w]=[E][C1][w -5 ][exp{C2/wT}−1 -1 ] where E is the spectral emissivity of the hot surface and C 1 and C 2 are constants. Consequently, in order to determine the temperature of a hot object from its direct infrared radiation, it is necessary to know its emissivity as well as its radiance.
The infrared radiation emitted directly by the heated pot usually does not approach that of a black body at the temperature of the pot and its emissivity value does not approach that of a black body and hence has an emissivity value much less than E=1. However, as explained in more detail hereinafter, the radiation emitted directly by the heated pot can be enhanced so that the effective emissivity of the enhanced radiation approaches that of a black body. Moreover, the ratio of the enhanced radiance to the direct radiance is a unique function of the physical emissivity of the pot. Thus, applicant had determined that using the value of the direct radiation of the pot and the emissivity of the pot as computed from this ratio, the temperature of the heated bottom surface of the pot could be computed using the Planck formula.
However, applicant discovered that the electric range itself produced sufficient radiation to interfere with any measurement of the direct and enhanced radiation of the pot. In addition, unless great care was employed in making radiation measurements, the measurement equipment would be heated and produce self emission, which of course produced further interference.
This invention is directed toward a new type of measuring apparatus for measuring the temperature of such a heated pot in such manner that the radiation from the range could not interfere with the desired measurement and further that the apparatus could not be heated to a level at which significant self emission was produced. Moreover, this apparatus provides a means for determining the emissivity of the heated pot. Consequently, an accurate measurement of the temperature could be obtained using the Planck formula.
SUMMARY OF THE INVENTION
Apparatus in accordance with the principles of this invention is directed toward determining the temperature of a heated pot disposed over an opening in a top flat surface of a cooking range. For this purpose, the bottom surface of the pot is larger than this opening and covers it.
The apparatus employs an infrared transparent window disposed in the opening abutting said surface so that the window is flush with said surface.
An infrared reflective hemisphere is disposed below the window. The hemisphere has an open top surface in direct contact with the window and a closed bottom surface with a small opening therein. As a result, a direct infrared radiation component from the bottom of the pot and a reflected infrared radiation component from the exposed surface of the hemisphere both pass freely through the window and the mixture of these two components is essentially combined within the cavity formed by the pot and hemisphere, enhancing the direct radiation from the pot so that the combined mixture approaches that of a black body at the temperature of the pot.
The apparatus employs a first infrared wave guide coupled to the small opening in the hemisphere to receive the enhanced radiance from the pot and a second wave guide butted against the window to receive the direct pot radiance.
The apparatus also employs first means disposed below said small hemisphere opening and coupled to said first and second guides for deriving from the guides the values of the direct radiance and the enhanced radiance; and second calculating means coupled to said first means. The second means has stored therein a program for determining the emissivity of the pot from the ratio of the enhanced radiance to the direct radiance, and incorporating the direct radiance value and the emissivity in the Planck formula to compute the temperature of the pot.
In order to prevent the radiation from the cooking range from interfering with the temperature measurement, applicant utilizes in the first means infrared radiation detectors which do not respond to the wavelengths of radiation from the range but respond only to a different and non-overlapping group of wavelengths whereby range radiation cannot interfere with temperature measurements. Moreover, the apparatus incorporates additional means to prevent it from being heated to such a level that self emission can interfere with the temperature measurements.
As a result, this invention overcomes the prior art difficulties in measuring the temperatures of heated pots employing flat top cooking ranges and for the first time enables accurate temperature measurements to be obtained.
BRIEF DESCRIPTION OF THE INVENTION
FIG. 1A is a cut away side view of a preferred embodiment of the invention.
FIG. 1B is a view similar to FIG. 1A but showing a modification thereof.
FIG. 2 is a graph displaying the ratio of enhanced to direct target radiation as a function of target emissivity.
FIG. 3 is a graph displaying the spectral transmission of the range top plate made from CERAN as a function of wavelength in microns.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Referring first to FIG. 1A, an electrical cooking range has a top plate 9 made of CERAN or similar material. The range has a metal frame 19 with thermal insulation disposed on its upper surface. The range heating coil 10 rests on the insulation. The plate has a small opening 20 . A heated pot 8 has a bottom surface much larger than the opening. The pot rests on the top surface of the plate and covers the opening.
An infrared transparent window 2 is disposed in the opening flush with the top surface and is mechanically sealed thereto by a fitting ring 23 . A concave shaped infrared reflecting hollow body such as an infrared reflecting hollow hemisphere 1 has an exposed surface with a mirror finish, typically a gold coating which is highly reflective in the infrared. The hemisphere has an open top end engaging the window and an opposite closed lower end having a small opening 16 therein.
The window 2 , which typically is formed of zinc selenide, is disposed between the bottom of the pot and the open upper end of the hemisphere 1 to essentially protect the exposed surface of the concave body from contamination. At the same time, direct radiation from the bottom surface of the pot and reflected radiation from the exposed surface of the hemisphere pass freely through the plate essentially confining the mixture of the two radiation components within the cavity formed by the pot and the hemisphere. Consequently the direct radiation of the pot is enhanced and the combined radiation approaches that of a black body at the temperature of the pot.
A portion of the cavity radiation passes downward through small opening 16 in the bottom of the hemisphere. An infrared wave guide 3 , typically a hollow gold coated tube, is connected at one end to the opening 16 and is coupled at its other end through an infrared filter 18 to an infrared detector 4 such as a thermopile sensor. Detector 4 converts the cavity radiation to an electrical signal which is amplified in amplifier 15 to produce signal V 1 . Signal V 1 is proportional to the cavity radiance.
Infrared wave guide 13 has one end abutting plate 2 and is coupled at its opposite end through infrared filter 17 to an infrared detector such as a thermopile sensor 14 . Detector 14 converts the direct radiation to an electrical signal which is amplified in amplifier 22 to produce signal V 2 . Signal V 2 is proportional to the direct radiance. No reflected radiance is present in signal V 2 .
As shown in FIG. 3, the spectral transmission of CERAN or equivalent material is reduced to zero in the range of 4.5 to 13 microns. The filters 18 and 17 limit signals V 1 and V 2 to this zero range whereby the radiance from the range cannot influence the accuracy of the desired measurements.
In order to minimize heating of the hemisphere 1 and infrared wave guides 3 and 13 , thereby minimizing self emission which could otherwise adversely influence the accuracy of the desired measurements, a ceramic shroud 7 of high infrared reflectance encloses the hemisphere and the upper end of guide 3 . A metallic shroud 5 , disposed within shroud 7 , conducts heat to a thermally conductive tube 11 which in turn is connected to a beat sink 24 . The tube 11 is surrounded by a heat insulating tube 6 . The heat sink 24 is located in a relatively cool area away from the heating coils of the range. Thus this design provides for thermal insulation, radiation reflection and heat removable by conduction.
To provide additional protection of the reflective surfaces, the wave guide hemispherical reflector assembly may be sealed and filled with a chemically inert gas such as nitrogen or argon.
An ASIC chip 12 displays as an output the temperature in analog and digital form. This chip contains a look-up table having different values of emissivity E corresponding to different ratios of V 1 /V 2 . The chip contains algorithms which convert voltages V 1 and V 2 into digital numbers and then computes the ratio of these digital numbers, using the look-up table to obtain the corresponding value of the emissivity. The chip then inserts the values of V 2 and E in the Planck formula to calculate the temperature.
In the event that, despite the cooling mechanisms described above, guides 3 and 13 and the hemisphere 1 are heated to a temperature at which they emit self radiance, and this radiation can change the values of signals V 1 and V 2 , a correction can be made.
In order to correct these values, a thermocouple 25 measures the temperature of the hemisphere. A wire pair 26 connected to this thermocouple yields its output voltage Vp. A second and a third look-up table in the chip correct the values of V 1 and V 2 , respectively, in accordance with the value of Vp. The temperature is then calculated as above.
The structure shown in FIG. 1B differs only from that shown in FIG. 1A in that the guide 13 in FIG. 1A passes through the hemisphere while the guide in FIG. 1B passes along but not through the hemisphere.
While the invention has been described with particular reference to the detailed description and the drawings, the protection sought is to be limited only by the terms of the claims which follow.
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Apparatus for measuring the temperature of an electrically heated pot which uses the Planck formula and employs an infrared reflective hemisphere; first and second infrared wave guides, and first and second infrared filters and infrared detectors as well as a calculating device.
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BACKGROUND OF THE INVENTION
This invention relates to a semiconductor manufacturing apparatus and in particular to a semiconductor manufacturing apparatus in which circuit patterns are etched on a semiconductor wafer by a plasma reaction.
This invention relates to TI copending U.S. patent application Ser. Nos. 663,907; 663,901; 664,448; 663,903; 663,904; 663,805; 663,905; 663,906; 663,908; and 663,909 which by reference are incorporated herein. Copending application Ser. No. 664,448 was filed on Oct. 24, 1984 while the other copending cases were all filed on Oct. 22, 1984.
The manufacturing of semiconductor devices such as a 256K RAM or even up to a 1 megabit RAM device require precision dry etching with high repeatability, low particulate levels, reliable endpoint detection, multiple process capability and reliable feedback control to a microprocessor controller for reliable systems execution. An example of a prior art plasma reactor system is described in U.S. Pat. No. 3,757,733 which is assigned to the assignee of the present invention.
In the prior art systems, the transportation of silicon wafers through a plasma reactor required an opening in the reactant chamber that is large enough for the wafer to pass through. The mechanism that are typically used create particles that potentially impact yeild of devices of the semiconductor wafers that are processed.
Chlorine and bromine gases which are typically used in the process during plasma etching are highly corrosive to the components that are used to build the plasma reactors. Over a long term operation, reactor components exposed to the plasma must be constructed of materials that are resistance to the corrosive effects of the plasma. Aluminum is an excellent material of construction for a plasma reactor, especially when it is protected by anodization. However, during etching, when a semiconductor or silicon wafer is placed on a substrate assembly that is anodized and used as an electrode, the substrate is protected from the plasma by the silicon wafer. However, each silicon wafer has a slice or flat to allow for crystallographic orientation. If the slice is placed on the substrate with random orientation of the flat, an annulus of equal width of the flat width plus the placement tolerance will in general be exposed to the plasma. Anodizing the whole substrate is impractical in that it is conductive towards the RF electrical power used in the plasma reactor. However, it is an insulator towards DC. It is known that electrically floating objects such as silicon wafers covered with oxides exposed to a plasma will acquire an electrical potential, the floating potential, above the ground of the system. It has been observed in production that an electrostatic repulsion develops between the wafer and the semiconductor substrate causing the wafer to randomly drift off its alignment position on the substrate.
Although several commercially available automatic wafer etch reactors use a confined plasma, none of the known systems provide a small gap which will not support a plasma and therefore confine the plasma within the small gap, use the same gap for both pumping the exhaust of gases from the reactors and for transporting the semiconductor wafers into the reactant chamber and thus keeping the reactant chamber simple and free of poorly controlled dead space within the reactor chamber.
Additionally, it has been determined that the gap between the collimator or electrode and substrate during process should be approximately around 0.040 inch for oxide processing. With a non-load locked system, the process chamber is vented to atmosphere which allows the electrode and collimater to move up to between 0.030 and 0.040 inch and the semiconductor wafer passes under the collimater. This is unreliable due to the fact that an inconsistent gap can now be achieved and the slice levitation varies, also, an automatic transportation system is impractical with the above operation. And in particular, the single slice dioxide and oxide etch processes have historically used the highest possible density to remove silicon dioxide. This elevated power density is far more difficult to control than any other type of etching operation. Also, highly selective etch processing often builds up deposits in the reactors. For this reason, these processes have tended to be limited in commercial applications.
SUMMARY OF THE INVENTION
A plasma etch system that processes one slice at a time is disclosed. The system is comprised of an entry loadlock, an exit loadlock, a main chamber, vacuum pumps, RF power supply, RF matching network, a heat exchanger, throttle valve and pressure control gas flow distribution and a microprocessor controller. A multiple slice cassette full of slices is housed in the entry load lock and after pumping to process pressure, a single slice at a time is moved by an articulated arm from the cassette through an isolation gate to the main process chamber. This slice is etched and removed from the main process chamber through a second isolation gate by a second articulated arm to a cassette in the exit loadlock. The process is repeated until all semiconductor wafers have been etched. The cassette loadlock system is able to evacuate a whole cassete of semiconductor wafers for processing which lowers the particulate environment for the slices and, provides a more stable environment for the slices by removal of moisture and preventing static discharges and additonally provides a safety feature that protects the operators from harsh or toxic gases that are traditionally used in semiconductor type plasma reactors.
This novel feature enables clean slice handling and eliminates the problem that traditionally occurs in the manufacturing of semiconductor devices in that there are no airtracks on the devices, no rubbing of the parts or semiconductor wafers. The semiconductor wafers are lifted off the cassette slot before movement and all belts, pulleys or drives are either external to the chamber or shielded within the main reactor chambers. The movement of the slices through the process is tracked with sensors.
The cassette loadlock apparatus according to the invention is a closed loop feedback process control system which insures that adequate pressure within the entry loadlock, the exit loadlock and the main chamber are controlled by microprocessor. The RF power during the reaction of the manufacturing process is monitored and controlled by a microprocessors. Gas flows are monitored and controlled by the microprocessor through mass flow controllers. End of etch is monitored and controlled by the microprocessor through a novel endpoint detection scheme.
The invention provides a multiple process capability by which multiple menus can be applied to a single slice in situ to achieve special etch profiles and other special processing requirements such as high selectivity of the etch films to the substrate and the etching of multiple stacked films.
These features provide a high etch rate with high resist survival through the use of a refrigerated liquid cooling on the top and bottom electrodes, thus allowing high power with good photoresist preservation during the operation.
These and other advantages and features of the invention will be more apparent from reading of the specification in conjunction with the figures in which:
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 is a front elevation of a cassette load lock plasma reactor according to the invention;
FIG. 2 is top view of the cassette load lock plasma reactor according to the invention;
FIG. 3 is a blcok diagram of the control system for the plasma reactor according to the invetinon;
FIG. 4 is a block diagram for the RF circuit;
FIG. 5 is a block diagram for the endpoint detection logic;
FIG. 6 is a flow diagram of the endpoint detection process;
FIGS. 7a and 7b are waveforms illustrating the detection of an endpoint;
FIGS. 8 and 9 are the gas and vacuum flow diagrams;
FIGS. 10 and 11 are different views of the cassette load lock plasma reactor;
FIGS. 12 through 13 illustrate the wafer transport system;
FIGS. 14 through 17 are drawings illustrating the slice transport arm;
FIG. 18 is a view of the entrance port of the plasma reactor;
FIGS. 19 and 20 are views illustrating the operation of the gate valves;
FIG. 21 is a sectional view of the reactor chamber;
FIG. 23 is a top vie of the plasma plate illustrating an anodized ring;
FIGS. 23 and 24 illustrate the electrical assembly;
FIG. 25 is a cross sectional view of an alternate embodiment of the reaction chamber;
FIGS. 26 through 28 are illustrations of the power load lock reactor;
FIGS. 29 and 30 are illustrations of the power load lock slice handler arm; and
FIGS. 31 through 34 are diagrams of the powered load lock chambers.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In FIG. 1 there is shown a front elevation of a cassette load lock plasma reactor. The cassette of semiconductor wafers having photoresist patterns printed on them is placed in an entry load lock 21. A process is entered into a microprocessor that is contained within the cassette load lock reactor 23 by a keyboard 25 and a display 27. The menu is loaded in memory of the microprocessor and the process sequence begins. The entry load lock 21 is pumped down to a predetermined pressure or process pressure by a vacuum pump 29. The process pressure is maintained by feedback control circuit via a manometer that provides information to the microprocessor within the cassette load lock reactor 23 to control a throttle valve that is used to control the pump rate of the entry load lock 21. At the time that the entry load lock 21 is being pumped down to a process pressure and maintained there, the main chamber is either pumped down to main process pressure or is maintained at process pressure by a main chamber pump 31. A cassette elevator that is contained within the entry load lock 21 positions a first semiconductor wafer or slice that is to be processed by the cassette load lock reactor 23 and in the embodiment shown in FIG. 1, a cassette that is a handling device that stores a plurality or in the case of FIG. 1, 25 semiconductor wafers. Each wafer has patterns for semiconductor circuits printed on them by a photoresist process. The first semiconductor wafer is, as shown in FIG. 2, positioned by the cassette elevators located generally at 33. The semiconductor wafer is moved by an articulating arm 41 from the entry chamber 21 through an isolation gate valve 35 into a main process chamber 37 and placed on the main chamber bottom electrode 39 for etching. The position of the semiconductor wafer 143 is controlled by a feedback system and capacitive sensors that monitor the movement of the semiconductor wafer from the load lock chamber into the main chamber. After the slice is sensed to be safe in the main chamber 37 and the articulating arm 41 is sensed to be moved back into the entry load lock 21, the isolation gate 35 is closed and appropriate gases are applied from the gas distribution system 43 of FIG. 1 through the filtering systems generally at 45 and applied to the main chamber 37 by flow controllers 845 that are contained within each gas line 45. In the embodiment of FIG. 1, up to four gases may be applied to the main chamber for the process. Additionally, in FIG. 1, a nitrogen line 47 provides nitrogen gas for purging of the system when it is necessary to open up the main chamber, the entry load lock or the exit load lock 49.
As prescribed by the memu that was entered on the keyboard 25, pressure established by a throttle valve that is connected to the main chamber vacuum pump 31 and a manometer pressure sensor and the feedback loop process control is maintained by the microprocessor within the cassette load lock reactor 23. The cassette load lock reactor 23, in the embodiment of FIG. 1, is a plasma reactor and a plasma is formed by applying RF energy between the two electrodes that are contained within the main chamber 37 which ionizes the gases to form reactant gases that include ions, free electrons and molecular fragments. The gases are provided by the gas distribution 43 and the filters 45. RF power is provided to the main chamber 37 by an RF generator 51 and is applied to an RF matching network 53 by a conductor 55. The RF matching network controls and adjusts the energy that is applied between the electrodes that are contained within the main chamber by sensing the reflected power and converting this information to the digital signal that the microprocessor within the cassette load lock 23 will respond to.
In either etching or deposition process, the processing is automatically terminated by the microprocessor within the cassette load lock reactor 23. When in the etching mode, an endpoint is detected by an endpoint detector in the cassette load lock 23 which measures change in the optical emissions at a specific wavelength. The cassette load lock reactor 23 that is shown in FIGS. 1 and 2 provide multiple menus to be run on the same slice by the proper selection during the menu entry to the keyboard 25. After the process is complete, the slices or semiconductor wafers are automatically removed from the main chamber by a second articulated arm 57 that is located within the exit load lock 49 and is passed through a second isolation gate 61 and placed in an empty cassette whose position is positioned by the elevators at 63. At the completion of the processing of each semiconductor wafer, the process is repeated until all of the semiconductor wafers have been processed by the cassette load lock reactor after which the entry load lock 21 and the exit load lock 49 are brought up to atmospheric pressure by applying nitrogen through line 47 to purge the entry 21 or the exit load lock 49. The cassette is then removed and a new cassette is loaded for processing.
Heat transfer from the slice during etching is accomplished through a refrigerated system that is contained within a refrigerator controller 63 that refrigerates, in the embodiment of FIG. 1, an ethylene glycol-water mixture flowing through the top and bottom electrodes that are contained within the main chamber 37. A thermocouple sensor element is used to monitor the temperature so that the process may be controlled by the microprocessor that is contained within the cassette load lock reactor 23. Additionally, the oil that is used by the main chamber vacuum pump is re-circulated and filtered by a filter system 65.
FIG. 3 is a block diagram of a microprocessor control system 10 that is used to control the operation of the cassette load lock reactor 23. In particular, a central processing unit 17, which in the embodiment of FIG. 1 is manufactured with a 9900 microprocessor that is manufactured by Texas Instruments Incorporated of Dallas, Tex. or can be any central processing unit known in the art that has similar specifications as to speed, word length and operation.
The central processing unit 17 has an EPROM and RAM memory 19 which stores data and program instructions that are used to control the I/O devices that are connected to data bus 6. A language translator 15 is provided which is used to convert SECS II protocall into internal protocall that the CPU 17 will recognize. SECS II is an industry standardized interface for semiconductor equipment communication.
The central processing unit or CPU 17 is connected to a data bus 6, which interfaces to the I/O devices. In particular, a battery memory RAM 13 stores menu data that is provided to the processor system 10 of FIG. 3 by the keyboard 25 and the display terminal 27. A digital I/O 3 provides digital controls to control the process to include the gate valves and other controllable devices that are contained within the cassette load lock reactor 23 or the power load lock reactor 523 of FIG. 26 and receives status from these devices indicating the initiation of operation or the completion of operation. The status and control signals that are used to control the operation of the devices of FIG. 1 or are listed in Table 1.
TABLE______________________________________Inputs (Status) and Outputs (controls) of the Digital I/O.Device Status Controls______________________________________Gate valve 35 opened/close open/closeGate valve 61 opened/closed open/closeValves 704 opened/closed open/closeValves 705 open/closedValves 706 opened/closed open/closedValves 707 open/closedValves 708 opened/closed open/closedValves 709 open/closedValves 771 open/closedValves 773 open/closedValves 774 open/closed Purge on/offChamber gass on/offRF on/off on/offGas valves 710through 719 on/offElevator position #1 through 4Lid interlock on/offChamber pressureinterlock on/off______________________________________
An analog I/O device 5 provides analog control signals on its output by converting digital commands that are provided to it to analog signals by digital to analog converters. It additionally receives analog signals back from the cassette load lock plasma reactor 23 and the power load lock reactor 28.
Table 2 provides a listing of the signals that are converted to either analog signals from digital commands provided to the analog I/O device 5 by the microprocessor 17 or analog signals received by the analog I/O device and converted to digital signals by the D to A's that are contained within the analog device 5.
TABLE II______________________________________Analog commands and inputs for the analog device 5Inputs analog to digital converters:1 Manometers 752 and 770 for cassette load lock, 752, 772 and 775 for power load lock for monitoring pressure.2. Mass flow control devices 721 through 724 for cassette load lock plasma reactors and 721 through 730 for power load lock reactors3. RF power control4. Endpoint detection 50, 525. TemperatureCommands digital to analog converters1. Pump rate (throttle valves 704, 706 and 708) for maintaining pressure2. Flow rate set mass flow valves 721 through 724 for the cassette load lock plasma reactor and 721 through 730 for the powered load lock reactor3. RF power set4. Endpoint detection automatic gain control 50, 525. Temperature______________________________________
It should be noted that the analog I/O is just a parallel combination of digital to analog converters or analog to digital converters that are connected to the data bus 6 and the digital I/O 3 is a plurality of line drivers and receivers. Control is provided by the analog controller 7 which is a microprocessor such as a Texas Instruments 9900 that is programmed according to the microcodes that are contained within table 3. Any microprocessor that is capable of meeting similar specifications may be used however, in lieu of the Texas Instruments 9900.
The data terminal is controlled by data terminal controller 9 which interfaces the display 27 and the keyboard 25 to the microprocessor 17 as well as displaying the voltage representation that is provided from the RF generator 51 and the analog control unit 7 by a data line 12. Table 4 provides the microcode for the data terminal controller 9. The movement of the semiconductor wafers from each cassette into the reactor chambers and from the reactor chambers into the exit chamber is controlled by a slice handler 11 through the operation of stepper motors 2 and in response to sensors 4. The slice handler 11 is a microprocessor which provides digital commands on its output and receives digital inputs from the sensors. The microprocessor is a device, again, such as the TI9900 and the microcode for which is provided in Table 5A is used by the cassette load lock reactor 23 and Table 5B is used by the slice handler, in the power load lock reactor 523. The program that is used to control the central processor unit 17 is a complex program and in the embodiment of FIG. 3 has a pascal compiler. A pascal listing of the programs that are stored within the CPU 17 is provided in Table 6 for the powered load lock reactor of FIG. 26 and Table 7 for the cassette load lock reactor of FIG. 2. Tables 3-8 are provided in U.S. pat. application No. 663,901. Table 8 is an assembly language for subroutines used by the CPU 17 and stored in EPROM 19. U.S. patent application No. 663,901 is incorporated herein by reference.
FIG. 4 to which reference should now be made, there is shown a block diagram of the control circuit that is used to control the radio frequency energy that is applied to the load lock reactors 23 and 523. As was indicated in conjunction with FIGS. 1 and 3, the microprocessor 17 provides an output command to the RF generator 51 by a control line 32. The RF generator 51 includes an RF interface 26 and a generator 28. This is a commercially available unit as manufactured by Plasma Therm Inc. or can be a device such as that manufactured by Ortec Incorporated of Oak Ridge, Tenn. Status of the operation is provided back to the digital I/O 3 by a data bus 34. The RF output is applied from the RF generator 51 and in particular, the generator section 28 of the RF generator 51 to the matching network 53 by a conductor 55. The matching network includes a Bird Watt meter 22, manufactured by Bird Electronics of Columbus, Ohio, which monitors power that is applied to the upper electrode 30 that is contained within the main chamber 37 by an impedance matching circuit 53. The output of the Bird watt meter 22 is applied by an isolation amplifier to the analog to digital converter as contained within the analog I/O 5 and to the analog control microprocessor 7. Adjustment of the RF energy that is applied to the cassette load lock reactor 23 and power load lock reactor 523 is provided by the microprocessor 17 of FIG. 3. A digital to analog converter that is a part of the analog I/O 5, an isolation amplifier 25 in the RF interface 26 will cause the RF generator 51 to adjust its energy in response to the analog signal that is applied to it. This of course, provides a feedback loop for the host microprocessor 17 to control and plasma operation according to the prescribed menu that is entered by the keyboard 25.
FIG. 5 is a block diagram of the control system that is used to detect the endpoint of the operation. In the embodiment shown in FIG. 5, there are dual channels used in the endpoint detection process. Quartz windows 58 and 60 provide and optical opening into the main chamber 37. Adjustable filters 62 and 64 can be selected to ensure that only light having the proper wavelength is applied to the endpoint detector 70. There is, as described earlier, two channels, an A channel and a B channel. The A channel has a light detector 54 which is a device such as a photo multiplier or silicon detector. The B channel detector 56 of course is a similar device. Each channel has an automatic gain control circuit 50 and 52. The gain of the automatic gain control circuits 50 and 52 is controlled by the analog controller 7 and the analog I/O 5. In particular, the output of the automatic gain control circuit 50 for channel A is applied to an analog to digital converter 40 that is contained within the analog I/O 5 and applied to the analog controller 7 where the data is processed and passed on the host microprocessor 17. Adjustment of the automatic gain control circuit 50 is provided by either the host microprocessor 17 and/or the analog controller 7 by providing a digital command to a digital to analog converter 42 that is contained within the analog 5. The digital to analog converter 42 provides an analog signal to adjust the gain on the automatic gain control circuit 50. The output of the channel B automatic gain control circuit 52 is converted to a digital signal by an analog to digital converter 44 that is contained within the analog I/O 5 and is processed by the analog controller 7 for averaging of data to be used by the central processor 17. An output to set the automatic gain control circuit 52 is provided by a digital command being provided by the analog controller 7 whether originated from the analog controller 7 or the CPU 17 and is converted to an analog signal by the digital to analog converter 46 and applied to set the automatic gain control of the channel B automatic gain control circuit 52. Additionally, the display at 27a provides display of the setting up of the automatic gain control 50 and 52. An auxiliary display is provided from the analog controller 7 and a digital to analog converter 48. These provide meter displays of the endpoint detector circuit.
The operation of the endpoint detector allows the user through the keyboard entry 25 to define parameters which can be defined as two classes, the detection mode and the detection parameters.
The detection mode parameter is selected by the users and provide the following mode of operation. No endpoint mode is when the endpoint detector does not operate. Either channel A or channel B detector outputs can be monitored and applied to a strip chart recorder via the display outputs 27a. Channel A endpoint selects a signal from channel A detector to be used to determine the endpoint. The channel B mode selects the signal to be used as the endpoint detection from channel B. The a-b endpoint detection subtracts the output of B from channel A. In this mode, the signal used for endpoint detection is formed by subtracting the detector B signal 56 from that of the A detector 54. The purpose of this mode is to allow the signal to noise ratio of the combined signals to be increased by removing correlated noise during the subtraction process. The final mode of operation is the a+b mode in which the detector outputs from channel B are added to the detector outputs from channel A. This mode is useful to increase the available amount of total signals for the detection process. FIG. 6 provides a flow diagram of the adjusting of the automatic gain control circuits 50 and 52 and the operation of the endpoint detector circuit as is programmed by the analog controller 7. The endpoint detector of FIG. 5 is designed to detect the endpoint when the following parameters are set. The window length, T(w) is the time interval during which endpoint signal after signal process must remain greater than its selected threshold value for the endpoint to be determined. The filter factor T(k) determines the time interval used to perform the digital differentiation of the endpoint signal by the microprocessor 7. The +/- threshold V(t) is the percent of voltage of an upper limit, such as eight volts in the embodiment of FIG. 5 and is said to correspond to either positive or negative slope endpoint signal. This threshold is selected as a percent of the maximum voltage. The delay to detector time T(d) is in units of seconds as the time interval from the application of RF energy to the main chamber 37 to the start of endpoint detection. For example, entering of a number 40 to the keyboard 25 means that the endpoint detector will not start looking for the endpoint until after 40 seconds has expired after the RF energy is applied to the main chamber 37 by the RF generator 55. FIG. 6 is a flow diagram of the process in which the microprocessor 7 is used to perform all the signal processing for the endpoint detectors. After the initialization of turning on RF energy at circle 100, the unit waits for the delay to detect time to expire at diamond 101. The adjustments of the AGC units 50 and 52 is performed at block 102 and in the embodiment of FIG. 5, the AGC is adjusted to provide an output of five volts. The AGC is then sampled and in the embodiment of FIG. 5, the sample rate is every one-tenth second. This is illustrated by the control loop at 103 and includes the steps of reading the signal level at block 105, converting the signal level to a digital signal by the analog digital controller of either 40 or 44 at block 106 computing the average signal over a period of time over block 107, computing the difference using the filter factor at block 108 and comparing to see if the difference or summation i.e., a-b, a+b or either a or b is greater than or equal the threshold voltage at block 109. This loop continues until the difference including at block 109 is greater than or equal to the voltage threshold in which case the rendered length is incremented to insure that the window length has expired as indicated in by control loop 110. If the window length has expired, then an endpoint detection is indicated at block 111 and the operation is complete and exited from at circle 112. It should be noted that in performance of the AGC operation, the analog controller 7 reads a data word, interprets it as a voltage, compares it to a reference such as 5 volts. It then computes a gain adjustment word and sends it to the digital to analog converter either 42 or 46 which converts a digital word into a voltage level. This voltage is applied to the automatic gain control circuit either channel A AGC 50 or channel B AGC 52, of the circuit which act as of course a multiplier. In this matter, the gain is adjusting using a successive approximation until the output of either or both the channel A AGC 50 or the channel B AGC 52 is at a predetermined voltage level which in the embodiment of 55 is five volts.
FIG. 7 illustrates the operation of the control loop of FIG. 6 graphically. In particular, FIG. 7a is a curve that illustrates the signal level output from either the A detector 54 or the B detector 52 by waveform 114. In FIG. 7b, waveoform 116 illustrates the output from the analog controller 7 as is displayed on the auxiliary 1 output of the display 27a in which at point 118 the RF power is turned on. The window T(w) is represented by dimension lines 115. At point 119, the threshold voltage V(t) is exceeded and the endpoint is detected. When an endpoint is detected, a square wave output as illustrated by waveform 116 is produced.
GAS AND VACUUM CONTROL SYSTEM
The vacuum and gas control system for the cassette load lock plasma reactor 23 is illustrated in FIG. 8 to which reference should now be made. The gas from the gas distribution 43 of FIG. 1 is applied to a manifold 750 by a mass flow controller 721 through 724. The mass flow controllers are controlled by the analog inputs from the control system 10 and additionally valves 710 through 713 are controlled by the status I/O 3 of the control system 10 and are on/off valves. The gases mixed in the manifold 750 and applied to the main chamber 37 where the temperature of the reaction within the main chamber is monitored by a thermocouple 751. The thermocouple 751 is an analog input to the analog I/O 5 of the control system 10. A vacuum pump 31 pulls a vacuum in the main chamber 37 when the block valve 709 is open. The flow rate is controlled by a throttle valve 708 which position is fed into the analog input and is set by the output from the analog input of the control system 10. Sensors 2 senses the position of the silicon wafer within the main chamber 37. The vacuum of the entry load lock 21 and the exit load lock 49 is provided by pump 29 as was discussed in conjunction with FIG. 1. Gate valves 705 and 707 are set open and the pump rates are controlled by throttle valves 704 and 706. The gate valves are interfaced in the control system 10 at the digital I/O 3 and the throttle valves 704 and 706 are controlled by the analog I/O card 5. Additionally, the positioning of the semiconductor wafers within the entry load lock 21 and the exit load lock 49 is provided by the sensors 2 and motors 4.
FIG. 9 to which reference should now be made is shown the gas and vacuum flow diagram for the power load lock 523. The difference in the powdered load lock 523 and the cassette load lock 23 is due to the fact that the entry load lock can have a plasma reaction as well as the exit load lock 49. In this case there are 2 vacuum pumps required, 29a and 29b. The entry load lock has a gas manifold 760 which mixes three gases from three mass flow control valves 725 through 727 which are controlled by the analog inputs and outputs from the control system 10 and are activated by setting of gate valves 714, 715, 716. The exit load lock 49 can have a plasma reaction based upon the mixture of up to three gases in a manifold 761 that are controlled by mass control valve 728, 729 and 730. The on/off operation of the gas flow into the manifold 761 is provided by the digital I/O 3 of the control system and controls the valves 717, 718, 719 as is the case with the gas valves into the entry load lock 21.
In FIG. 10, cassette load lock reactor to which reference should now be made, there is shown a front view of the cassette load lock reactor 23 in which the keyboard 25 provides, as discussed earlier, a data entry point that is the information of which is displayed on a display 27. The distinguishing features of FIG. 10 also illustrate a quartz window covered with plexiglass or other plastic 120 for viewing by the operator of the plasma reaction that is going on within the main chamber 37. This also enables the operator to insure that the semiconductor wafer is in the proper position between the electrodes during the reaction process. Additionally, the tuning of the RF generator 51 is illustrated by tuning meter 123 and the DC voltage that develops across electrodes is displayed by the DC voltage meter 122. This of course, in FIG. 3 is provided by the analog control 7 to the terminal controller 9 via data line 12.
FIG. 11 is a top view of the cassette lock load plasma reactor 23 in which the keyboard 25 is illustrated showing switches 133, and keypads 135. The cassette that contains the semiconductor wafers to be processed is placed within the entrance load lock 21 by lifting a vacuum tight lid 137 and rotating it around hinges 124 to place the cassette into the entrance chamber 21. Glass window 128 provides for visual inspection of the placement and the transfer of the semiconductor wafers from the entrance load lock 21 to the main chamber 39. Similarly, at the completion of the process of a cassette of semiconductor wafers, the lid 139 of the exit load lock 39 is lifted by rotating the lid 139 around the hinges 126 by removal of a cassette of processed semiconductor wafers.
SEMICONDUCTOR WAFER HANDLING INCLUDING TRANSPORT ARM
FIG. 12, to which reference should now be made, there is shown a cassette 141 containing a plurality of semiconductor wafers or slices 143. A slice transport arm 145 is placed into the cassette 141 and the cassette 141 is lowered by an elevator 156 that includes lead screw 152, stepping motor 4, and sensor 2, until the semiconductor wafers 143 rest on the slice transport arm 145 in the middle of the slice opening 147. Because the slice is not touching any part of the cassette as it leaves during the rotation of the slice transport arm, there is no friction between the semiconductor wafer 143 and the slice handling arm 145. This feature minimizes particular generation as the slice leaves the cassette 141. The position of the slice transport arm 145, the cassette 141 are controlled by the slice handler 11 of FIG. 3 and the motors 4 and sensors 2. The cassette platform 154 provides a reference position for the cassette 141 and thus the exit position of the cassette can be determined with the sensor 2 and precise control of the elevator 156. After the semiconductor wafers leaves the input cassette 141, it may be placed over a primary staging platform 149 or on the reactor substrate as is illustrated in FIG. 13. The semiconductor wafer 143 is lowered to the staging platform 149 by a lifting assemblies 151 which provide a plurality of lift pins 153 that lifts the semiconductor wafer 143 off of the slice transport arm 145. The unloaded arm is then removed from under the semiconductor wafer 143. When the unloaded slice transfer arm 145 is clear, the semiconductor wafer 143 is lowered onto the staging platform 149 which centers the semiconductor wafer 143 through the action of the centering pins 155. When the entrance slice handling arm 145 is moved under the platform 149 and the slice after being raised by the pin assembly 151 and the pins 153 are retracted the semiconductor wafer is lowered onto the slice transport arm 145. When the main chamber 37 is ready to accept a semiconductor wafer 143, the entrance load lock slice transport arm 145 moves into the main process chamber 37 through the gate valve 35. (FIG. 2) The semiconductor wafer 143 is then lifted off the slice transport arm 145 and the slice transport arm is then removed from the main process chamber. The semiconductor 143 is then lowered onto the substrate within the main process chamber for processing The semiconductor wafer 143 is removed from the main process chamber to the output chamber 49 by reversing the above discussed sequences and using the output chamber slice transport arm 147. FIGS. 14 through 17 illustrates the slice transport arm 145 as is used on the entrance chamber transport arm 41 or the exit chamber transport arm 57. A fork 151 is designed with touch pads 155 for balancing of the semiconductor wafers 143 thereon. The fork is rotatable around axis 157 which is adjustable through the setting of set screws 159. A main arm 161 rotates around axis 163 and is driven by a stepping motor to FIG. 17 which is coupled to the slice transport arm 145 via coupling means 165 and FIG. 15 feed through 180 which is a vacuum tight seal load lock walls 181. The wafer transport arms is mounted to the chamber by mounting bracket 164 and through holes 165 and 167. The arm assembly 161 contains a seal chain drive mechanism which is driven by a chain 172 of FIG. 16 which rotates causing sprocket 175 to rotate the fork 151 after being driven by sprocket 176 which is connected to the drive shaft 163 and coupling 165 of FIG. 15. As illustrated in FIG. 15, the slice transport arm is very narrow to facilitate it sliding under the semiconductor wafers 143 and entering the gate port between the load locks and reaction chamber.
GATE VALVES
FIG. 18 is a side-view showing the entrance or the exit into the main chamber 37. A gate port 184 allows the slice transport arms 145 to transfer semiconductor wafers 143 into and out of the reactor chamber 37. A gate valve 35 or 61 which are identical device is shown in FIGS. 19 and 20 and include a gate plate 183 which presses against the sides 182 of the main chamber 37 to to provide a seal thereto. It is important to keep particulate emissions at a minimal and this is achieved through a camming action on gate valves. Guide rails 180 and 181 guide the gate valve 35 or 61 up to the gate plate 183 and comes in contact with stops 187 and 186. At this point, the camming action that is precipitated by the linkage 190 that includes a first arm 191 and second arm 193 going into place and locking as shown in FIG. 20 pressing the gate plate 183 against the gate stop 186 and 187 and transferring the gate carrier 189 into the up position. A spring bias provided by spring 195 holds the gate carrier 189 in the position shown in FIG. 19 until the bias provided by the spring 195 is overcome by the camming action through the rotation of the arms 191 and 193 via the rotation of a drive shaft 197 that is controlled by an air cylinder.
FIGS. 19 and 20 to which reference should now be made, illustrates a power load lock plasma reactor unit 522 in which a cassette 400 hundred contains a plurality of slices and is housed outside of the entry load lock 21. A process menu is entered into the microprocessor that is contained within the power load lock plasma reactor 523 and the process sequence begins. A single slice that is housed within the entry cassette 400 is moved from the entrance cassette 400 through the isolation gates 435 which are devices such as that disclosed in conjunction with FIGS. 19 and 20 and is carried to the power entry load lock with articulated arm 441. The power load lock 21 is pumped down to manometer to the microprocessor through a throttle pressure controller and the pre-etch process is begun within the entry load lock 21. The first semiconductor wafer is at the completion of the pre-etch process is moved from the entry load lock 21 through a second isolation gate 35 into the main chamber 37 and placed on a main chamber bottom electrode for etching. This is accomplished in the same manner as was discussed in conjunction with FIGS. 1-18. Feedback of the slice movement is accomplished by capacitive sensors in the load lock chambers and main chamber. After the semiconductor is sensed to be safe in the main chamber and the articulated arm is sensed to have been moved back from the main chamber into the entry load lock 21, the isolation are closed and the appropriate gases up to 4 are provided from the gas distribution 45. It should be noted that the gas distribution also provides gas to the entry load lock 21 up to 3 for the pre-etch reaction and to the exit load lock 37, additionally up to 3 gases may be applied there for post-etching and of course all of these are in addition to the purge gas which in the embodiments of these are in addition to the purge gas which is embodiments of FIGS. 1, 19 and 20 is nitrogen. As prescribed by the menu that has been entered by the keyboard 25, pressure stabilized by a throttle valve capacitor manometer feedback to the microprocessor, RF power is activated and applied from the RF generator 51 and automatically tuned by the RF matching network as was discussed in conjunction with FIG. 4, with control feedback from the reflected power to the microprocessor 7. Etching of the film is automatically terminated by the microprocessor 7 via the feedback from the endpoint detector as was discussed in conjunction with FIG. 6, seeing a major change in the optical emission at a given wavelength. Of course, multiple menus can be run on the same slice by the proper selection during menu entry.
At the completion of the process, the semiconductor wafer is automatically removed from the main chamber 37 by an articulated arm 57 in the exit load lock 59 and placed in the exit load lock for the post-etching process. After processing in the post-etching load lock, the semiconductor wafer is moved to the exit elevator cassette 401 by articulated arm 541. Additionally, cooling is provided to the main chamber as well as the post-chamber and the entry chamber via temperature controller 63. Viewing windows 461, 462 allows viewing of the post-etch and pre-etch operation, respectively. FIGS. 21 and 22 are mechanical illustrations of the articulated arm 441 and 541 in which each has a fork 555. The articulated arms are mounted to the power load lock assembly by pedestal 453 and include a central arm section 161 which rotates around axis 163 as was discussed in conjunction with FIGS. 11, 12, and 13.
ELECTRODE AND COLLIMATOR ASSEMBLY
FIG. 21 is a sectional view of the main chamber 37 as seen from section lines 23 of FIG. 19. Initial input of the semiconductor wafer 143 through the opening 145 onto a substrate or wafer plate 206. The wafer plate is in position to allow clearance for the semiconductor wafer 143 and the fork 151 to position the semiconductor wafer over the wafer plate 206. Pins 153 will lift the semiconductor wafer off of the fork 151 and after its removal, lower the semiconductor wafer onto the substrate or wafer plate 206. The embodiment shown in FIG. 26 provides a two position substrate. It is generally accepted that during processing in the powered load lock that the substrate should be at different positions for different modes of operation, such as 0.040 inch for oxide processing. In the case of the cassette load lock, the substrate position is varied only for oxide processing, in all other etching modes the substrate is stationary. To achieve this, the wafer plate 206 has two positions, a low position, which is expanded and a process position.
In the embodiment of FIG. 25, two stainless steel bellows an interbellows 220 and an outer bellows 221 form a chamber between the bellows at 224. By introducing compressed air into lines 211, pressure is built up in the chamber between the bellows and this causes the movement of the substrate 206 to be implemented. Under initial operation, air is introduced into, an air cylinder, not shown, which raises the pins 153 for removal of the semiconductor wafer 153 from the fork 151. The centering pins 155 are raised by introducing air into air cylinder, not shown, which brings the guides 155 into position to center the semiconductor wafer 143 onto the wafer plate 206. The wafer plate 206 is in position for the process which is defined by the opening as indicated by dimension lines 228 between the cathode 230 and the substrate or top of the wafer plate 206. A consistent process gap between the cathode 230 and the substrate 206 is maintained during processing. A consistent opening for movement of the semiconductor wafer 143 between the collimater 430 and the substrates 206 is also maintained during slice movement. A constant low pressure (1 TORR) is maintained in the main chamber 37 during slice handling, this eliminates the slice contamination caused by lifting of the main chamber to the atmospheric pressure and facilitates the use of the slice transport arm 141.
Line 212 FIG. 21 is connected to the gas distribution 43 via filters 45 (FIG. 1) and provides for the entrance of gas to be processed in between the cathode 230 and the substrate 206. Lines 210 allow for cooling of the process reaction by the temperature controller 63 to flow through channels 232 and 242 to cool the semiconductor wafer 143 when placed on the wafer plate 206. Ring 205 is an isolation substrate ring that is isolated from the substrate 206 via isolation assembly 207. The ring consists of the body of the ring itself, 205, a retractible slice centering lip 209, isolation mechanism 207 which is made of a metal but with small thermal contact or with an insulator such as teflon which more completely isolates the ring 205 thermally and electrically with a possible ring extension shown at 231. The ring extension 231 is of course to increase the surface area of the top of the ring which increases the area of the overlap between the ring and the collimator itself in the electrode assembly 240.
This extension has been found to improve the effectiveness of the collimator in eliminating plasma expansion beyond the outside ring. The ring 205 is used to provide isolation and to aid in the control of plasma discharge which occurs during the reactor process between the cathode 230 and the substrate 206. The electrode assembly includes an electrode or cathode 230 to which RF voltage is applied via attachment to the plate 250. The electrode or cathode 230 is surrounded by a collimator 430, which includes insulator 251, which is in turn surrounded by a grounded plate 252 to all of which have a cylindrical symmetry about an axis position through the center of the electrode as indicated by line 256. When placed a small distance above a flat grounded substrate 206, the electrode assembly creates a volume as indicated by dimension lines 228 which can effectively confine a high power density plasma, while maintaining a sufficient channel for flowing gas through the lines 212 in the direction as indicated by arrows 258 and for observing the plasma optically through the window 120. As discussed earlier, the chamber can be widened for automatic transport of the semiconductor wafers from outside of the main chamber 137. By having a confined high power density plasma, high rate uniform anisotropic etching, especially for silicon dioxide and silicon nitrides, can be achieved. The ring 208 has an annulus of a width equal to the distance between the placement pins 155 and pin 209 and is an area which is generally exposed to plasma due to the fact that most semiconductor wafers have a flat portion that is used for alignment. The reacting plasma will attack the semiconductor wafer plate 206 or substrate and create damages. In FIG. 22, by anodizing an area 208 around the substrate 206, an area in width as indicated by dimension lines 270 will prevent etching of the substrate 206 when as shown in FIG. 21, a semiconductor wafer 143 is placed on the substrate 206. In general, the substrate 206 is manufactured with aluminum which is highly corrosive if not protected by anodization.
The cathode assembly 230 of FIG. 21 is shown in FIGS. 24 and 24 and includes a top plate 269 and a bottom plate 268. The top plate 269 has a gas inlet 305 to allow the cooling gas to enter via from line 212 and a water cooled line 304 which removes heat from the plate 268. Recess gas flow channels are provided at 307 and areas 306 provide for thermal contact between the bottom plate 269 and the top plate 268. The bottom plate 269 is illustrated in FIG. 23 and the top plate 268 is illustrated in FIG. 24. The thermal contact area must be maximized without restricting the gas flow. This is illustrated in the top plate where there are many drilled holes in area 301 and the lines in 302 allow for gas flow channels for the top plate 268.
FIG. 25 is alternate embodiment of the substrate 206 which has dual positions. The alignment pins 155 and lift off pins 153 are controlled by lifting of the carriage assembly 312 which is guided into place by wheels 310. The carriage assembly 312 is lifted by the levers 311 being raised under compressed air applied to a cylinder contained within a housing at 313. The positioning of the substrate 206 is accomplished by feeding air in between an interbellows 220 and an outer bellows 220 into a chamber 212 at air ducts 211 which causes the wafer plate 206 to be raised or contracted depending upon the air pressure that is contained within the air chamber 224.
Insert E--Powered Load Lock Reaction
FIGS. 31 through 34 illustrate the load lock chambers which provide for pre-etch processing in the entrance load lock through a plasma assisted reaction, and post-etch processing in the exit load lock through a plasma assisted reaction. In FIGS. 31 and 32 the gas from the gas distribution manifold 760 is applied by line 781 through a baffling port 999. The feedthrough 886 as shown in FIG. 32 provides for movement of tubing 781 to provide for adjustable spacing of the electrode assembly 987 to control the volume of reactants area 988. This is illustrated in FIG. 32. In addition to the tubing 786, the electrode assembly 987 includes feedthrough 886 and O ring seals 981 and includes a gas distribution assembly 889, a retainer 888 that holds the electrode 890 onto the gas distribution assembly 889. The retainer 888 also seals the electrode assembly 987 to the walls of the collimator 891, which is made of insulating materials. The gas is distributed through the electrode 890 by means of plurality of distribution holes 991. The slice handling mechanism which is shown at 882 has a fork 873 which lifts a slice from outside of the load lock chamber and centers it on ring 876 and then rotates around axis 877 to position the slice over the bottom electrode 875. The spacing 871 and 872 is 1/8th of an inch so as to minimize its effect on the plasma that is contained within volume 988. The slice handler 441 was discussed in conjunction with FIGS. 29 and 31. The substrate 875 has cooling channels 879 to facilitate the cooling of its semiconductor slice that is mounted to the substrate during its reaction. Function 870 is designed and positioned so as to ensure that the gaps 871 and 872 are at a minimum.
FIG. 34 illustrates the bottom electrode in which the reactant gases are removed from via line 896 which goes to vacuum pumps 29a or 29b and includes a mechanical housing 885 and a bellows chamber 884. Within the bellows chamber 884 is a bellows assembly 878 which moves the bottom substrate 875 by the operation of an air cylinder pressing shaft 978 in the upper or lower position. The compressing of the bellows 878 positions the substrate 875 to ensure the proper reaction as was discussed in conjunction with the main chamber.
Although the embodiments of the invention have been described with some particularity, one skilled in the art would know that the substitution of elements will not depart from the scope of the invention as limited to the appended claims.
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An electrode and substrate assembly for a plasma reactor allows high power plasma processing with low frequency excitation. The electrode sub-assembly is contained in a chamber which is used for pre-treatment such as de-scumming photoresist or for post-etch resist stripping and passivation. A post-etch treatment is essential in plasma aluminum etching.
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BACKGROUND OF THE INVENTION
This invention relates to the use of tagatose to improve one or more specific blood factors in persons suffering from, or having propensities toward, diseases associated with abnormalities in key blood factors.
A variety of diseases is caused by or results in abnormalities in key blood factors. These factors include red blood cell count (RBC), prothromin time (PT), activated partial thromboplastin time (APTT), and fibrinogen (FIB).
In 13-week studies performed with normal rats, four test groups were placed on normal diets in which 5, 10, 15 or 20 percent by weight, respectively, was replaced with tagatose. Two control groups were included, one maintained on normal diet with no replacement; the other on normal diet in which 20 percent by weight was replaced with cellulose and fructose at 10 percent each.
At the end of the study, all animals were sacrificed and hematological analyses performed on each. The results of these analyses are shown in Table 1. The table demonstrates that the inclusion of tagatose in the diet proved advantageous for each of the above parameters. The RBC and FIB factors for those animals fed tagatose were each increased over the corresponding measurements in the control animals. The increased values were within, or near, the normal range. The PT and APTT values decreased over the study period, staying within the normal range.
Specifically, increases in RBC indicate improved hematopoiesis and better maintenance of the blood and its functions. The decreases in PT and APTT, and the increase in FIB are measures of quicker and better clotting of the blood.
The food additive and new drug regulations of the U.S. FDA endorse the use of rats as good models for the human systems in safety and efficacy studies.
TABLE 1______________________________________Hematological ValuesRBC, ×10.sup.6 PT,s APTT,s FIB mg/dl______________________________________0%ControlMale 10.9 ± 1.1 18.7 ± 2.2 260.7 ± 40.0Female 9.8 ± 0.6 15.1 ± 1.9 228.4 ± 77.1Cellulose/fructosecontrolMale 11.9 ± 1.6 19.9 ± 3.1 249.9 ± 37.3Female 9.8 ± 0.4 14.4 ± 1.8 187.9 ± 46.25%D-tagatoseMale 11.3 ± 1.2 19.5 ± 1.7 254.5 ± 45.2Female 10.1 ± 0.4.sup.c 15.6 ± 1.7.sup.c 216.0 ± 115.810%D-tagatoseMale 11.1 ± 0.9 18.9 ± 2.0 275.3 ± 66.2Female 9.6 ± 0.8 14.3 ± 1.4 229.9 ± 82.015%D-tagatoseMale 10.7 ± 0.9.sup.c 18.7 ± 3.0 319.4 ± 113.3.sup.a,dFemale 9.8 ± 0.7 13.7 ± 1.1.sup.c 236.0 ± 52.9.sup.c20%D-tagatoseMale 10.7 ± 0.9.sup.c.sup.a 18.6 ± 2.4 290.3 ± 49.0.sup.cFemale 9.5 ± 0.7 13.4 ± 1.3.sup.b 261.4 ± 50.3.sup.a,d______________________________________ Note. Values are means ±SD (n = 18-20 rats). Hematology abbreviations are defined in the text. Unit abbreviations; g/dl (grams/deciliter), mg/dl (milligrams/deciliter), fl (femtoliter), pg (picogram), s (seconds). Levels of statistical significance indicated by superscript letters. .sup.a Mean significantly different than 0% control (P ≦ 0.05). .sup.b Mean significantly different than 0% control (P ≦ 0.01). .sup.c Mean significantly different than cellulose/fructose control (P ≦ 0.05). .sup.d Mean significantly different than cellulose/fructose control (P ≦ 0.01).
SUMMARY OF THE INVENTION
In accordance with this invention, there is provided a method for enhancing key blood factors of a mammal, especially man, in need of such treatment which comprises administering to said mammal an efficacious amount of tagatose, i.e., D-tagatose, L-tagatose or a mixture of the two isomers.
DETAILED DESCRIPTION OF THE INVENTION
The tagatose may be administered to a subject in combination with a food, beverage or taken separately in powder, crystalline or liquid form. As diluent, if needed, one may use liquid or solid carriers such as water, starch, alcohol or other non-toxic substances. Preferably, the tagatose is administered in the weight range of 100 mg/kg body weight/day to 2000 mg/kg body weight/day. The tagatose may be administered daily, every other day or at other prescribed frequencies. It may be administered in combination with other medications known to be suitable for use in the treatment of the particular blood disorder being treated.
EXAMPLE 1
Treatment of Anemia
A human subject is diagnosed as anemic by virtue of reduced RBC levels, and confirmed by other analyses showing blood iron deficiency and the presence of excessive microcells. The patient is placed on a regimen of tagatose taken at a prescribed rate, for example, 30 g/day divided into 10 g doses at each meal for a prescribed period of time. The RBC level is monitored periodically. Within several weeks, improvement in the RBC level is shown. Upon continuing the treatment, the RBC level becomes normal. At the discretion of the patient's physician, the tagatose treatment is continued, modified or discontinued, to be re-started in event of a relapse.
EXAMPLE 2
Adjunct Treatment of Hemophilia
A human patient is diagnosed with hemophilia. The patient's PT and APTT are at dangerous levels, indicating slow clotting time. The patient's FIB level is low, also indicating dangerously slower clotting time. Should bleeding from injury or disease take place, death could result before clotting stopped the bleeding. The patient is placed on a regimen of tagatose taken at a prescribed rate, for example, 15 g/day divided into 5 g doses at each meal, and the patient's progress is followed. Within several weeks, analyses show that the PT and APTT levels have decreased and the FIB level has begun to increase. Continued treatment with tagatose, with or without other prescribed treatments, brings the PT, APTT, and FIB levels near or within normal ranges. At the discretion of the patient's physician, the tagatose treatment is continued, modified or discontinued.
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A method for enhancing the blood factors of a mammal comprising administering to a mammal in need of such enhancement an efficacious amount of tagatose.
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BACKGROUND OF THE INVENTION
[0001] 1. Field of the Invention
[0002] This invention relates to a wire rope construction with reverse jacketed IWRC (independent wire rope core). More specifically it relates to such construction where the wire rope has no more than 18 outer strands and where the jacket consists of nylon.
[0003] 2. Description of the Prior Art
[0004] Most wire ropes in the wire rope industry are designed so that outer rope strands are laid in the same direction as the strands of the core. For example, if the outer rope strands are laid to the left the same is done with the strands of the core. This is done so as to minimize contact loads between the two. In this manner the core strands do not deteriorate very quickly allowing the rope to fail first primarily from the outside. This allows users to count outer rope strands broken wires and use these as a retirement criteria for the rope. This method of making and inspecting ropes is standard in the industry and is a recognized method to use ropes in a safe manner.
[0005] Most of the ropes manufactured as described above will have a tendency to have their ends rotate under load. This is because all the strands of the rope want to straighten under load. Non-rotating ropes are a special category of ropes designed in such a way as to minimize or even prevent completely this rotation. These ropes are usually utilized in crane applications where it is not desirable to have the load rotate during lifting. The lifting end of the rope is always used unrestrained and free to rotate. If a conventional rope is used the rope will unlay, which is also undesirable.
[0006] Common designs used for these applications consist of multi strand ropes having the interior core strands laid in a direction which is opposite to the one of the outer rope strands. In these situations both the outer rope strands and the core strands want to unlay under load but they do it in opposite directions. It is a known fact in the industry that the larger the core diameter relative to the individual diameter of the outer rope strands, the better the antirotation properties of the rope. This is because the torque developed by the core can better counteract the torque developed by the outer strands of the rope.
[0007] There are three main categories of non-rotating ropes on the market: the 34-35 strand ropes with round and compacted strands; the 18 strand also with round and compacted strands; and finally there is also an eight strand, low cost and lower performance variety consisting of what is commonly known as 8 strand reverse IWRC rope.
[0008] The following list identifies these ropes from worst to better in relation to their anti-rotating properties.
[0009] Worst performance: 8 strand reverse IWRC rope
[0010] Intermediary performance: 18 strand non-rotating rope
[0011] Best performance: 34-35 strands non-rotating ropes.
[0012] The reason for this behaviour is quite simple: the core in the eight strand rope is the smallest of the three types described above so it does not counteract the torques of the outer strands as well as the larger cores of 18 strand, and particularly 34-35 strands. It should be noted that non-rotating wire ropes with 18 outer strands or less have generally unsatisfactory performance, with the worst cases being ropes of 8 strands or less.
[0013] Since the outer strands of these ropes cross-cut at approximately 90° angle, the outer strands of their respective cores, they usually exhibit a rapid, invisible core deterioration that cannot be detected from the outside. In other words the detection of outer broken wires cannot be used to assess the inner rope condition. This is particularly the case of 8 strands reverse IWRC ropes and also of 18 strands ropes, while this condition is less severe with the 34-35 strands ropes.
[0014] It is hence normal to retire ropes having 18 strands or less from operation after a fixed number of hours or cycles to avoid the “surprise” of a sudden internal failure. Another alternative is to jacket the core with plastic materials to prevent the abrasion taking place at the rope strand-core strand interface.
[0015] It is already known to provide a jacket of a thermoplastic material, such as polypropylene, around a lubricated core, as disclosed for example in U.S. Pat. No. 4,120,145.
[0016] Applicant's own U.S. Pat. No. 5,386,683 also discloses a jacketed core in which the plastic material of the jacket is identified as polyethylene, polypropylene, nylon or another suitable thermoplastic material.
[0017] However, none of the above prior art patents deal specifically with wire ropes of 18 outer strands or less that have reverse jacketed IWRC lay, since the applicant found that with such wire rope construction the commonly employed jacket of polypropylene produces essentially no improvement over the non-jacketed construction and is therefore unsatisfactory.
[0018] When reviewing the situation it became obvious that a conventional cushioned core solution and approach did not work in this case. The examination of the polypropylene jacket showed that it had perforated at all the contact points between the outer stands and the core. A conclusion was reached that when dealing, for example, with an 8 strand rope or an 18 strand rope of reverse IWRC lay, the compression load applied by the outer strands on the core would be higher than the compression load applied by the outer strands of a 34-35 strand rope. The same would apply to all such wire ropes of 18 outer strands or less, which must therefore be considered as a special category of non-rotating ropes to which the present invention applies.
SUMMARY OF THE INVENTION
[0019] The present invention resides in providing a nylon jacket in lieu of polypropylene jacket in wire ropes having at most 18 outer strands and a reverse IWRC lay. Despite the fact that nylon has been mentioned as a suitable jacket material in the past, it was always mentioned as a substitute or alternative material to polypropylene, performing essentially the same function. It is, therefore, surprising and unexpected that in the special category of wire ropes which are under consideration herein, nylon jacketing of the core acts very differently than that of polypropylene, providing essentially double the protection as will be shown later.
BRIEF DESCRIPTION OF THE DRAWINGS
[0020] The invention will now be described with reference to the appended drawings in which:
[0021] [0021]FIG. 1 shows a schematic cross-sectional view of a wire rope construction with a nylon jacket in accordance with the present invention; and
[0022] [0022]FIG. 2 is a graph showing fatigue test results comparing the wire rope of the present invention with similar ropes having no jacket or a polypropylene jacket.
DETAILED DESCRIPTION OF THE INVENTION
[0023] The figures illustrate a preferred but non-limitative embodiment of the invention.
[0024] [0024]FIG. 1 shows a ¾″ (1.875 cm) 8×31 reverse core rope construction with eight outer strands 10 , each having 31 wires. The IWRC core of the wire rope is formed of six strands 12 wound around a central strand 14 . The core strands 12 are wound in the apposite direction to the outer strands 10 as shown by arrows 11 and 13 . Arrow 11 indicates that the outer strands 10 of the rope are wound in the clockwise direction, while the outer strands 12 of the core are wound in the counter-clockwise direction. The core is also filled with an appropriate lubricant 15 . Between the core strands 12 and the outer strands 10 there is provided an nylon jacket 16 , which cushions the core against the pressure exerted by the outer stands 10 during application of the load.
[0025] The wire rope described above is produced as follows:
[0026] 1. a core is produced by winding strands 12 over the central strand 14 in a predetermined direction (in this specific case with a left lay as shown by arrow 13 );
[0027] 2. the core is then filled with a suitable lubricant 15 ;
[0028] 3. a nylon jacket 16 having in this case a thickness of 0.20″ (0.5 cm) is then extruded onto the core; and finally
[0029] 4. outer strands 10 (which are also normally lubricated) are wound onto the nylon jacket in the opposite direction to the core strands 12 (in this specific case with a right lay as shown by arrow 11 ), and compressed thereon so that the nylon from the jacket 16 penetrates between the interstices of the outer strands 10 .
[0030] The above specific construction is used as a specific example and the various modifications can be made therein and in the method of its manufacture. For example, various sizes mentioned herein may be modified and adopted to the requirements of the user. Also, steps 2 and 3 of the method of manufacture mentioned above could be combined so that the core is impregnated and jacketed at the same time.
[0031] [0031]FIG. 2 gives comparative results for the wire rope described above with reference to similar ropes produced without any jacket and with a polypropylene jacket of the same thickness.
[0032] Thus, the applicant first prepared a ¾″ 8 strand reverse IWRC wire rope such as shown in FIG. 1, but without any jacket between the outer stands and the core. Two samples of such rope were subjected to a reverse bend fatigue test using a load of 1000 lbs (450 kg). As shown in FIG. 2, such non-jacketed rope failed after just over 100,000 cycles.
[0033] Then, to improve this result, a polypropylene jacket of 0.20″ (0.5 cm) was used between the core and the outer strands. Surprisingly, this construction produced essentially no improvement, also as illustrated in FIG. 2.
[0034] Since polypropylene did not produce improved results one would normally have expected that nylon, which is often mentioned as an alternative to polypropylene in such cases, would also be inadequate. Applicant had used nylon in other circumstances where it was found to act in a manner similar to polypropylene. Applicant has, however, decided to try to use nylon in this particular case to see if it would enhance the performance. Two samples of the wire rope with a nylon jacket of 0.20″ (0.5 cm), such as shown in FIG. 1, where thus subjected to the same fatigue tests as the previous samples. To applicant's surprise the number of cycles to failure essentially doubled with the nylon jacketed construction as compared to polypropylene jacketed or un-jacketed constructions. This unexpected result shows that nylon is a selected material of choice for such reverse core rope constructions.
[0035] The nylon jacket did not get perforated before the occurrence of outer rope strand degradation and failure of the wire rope due to such degradation. This was contrary to what happened with the polypropylene jacket which perforated very rapidly under load.
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The wire rope of this invention has at most 18 outer strands and an independent wire rope core, with the strands of the core being laid in the opposite direction to the outer strands of the rope, and a nylon jacket is provided between the core and the outer strands of the wire rope.
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This is a streamlined continuation of application Ser. No. 360,646 filed May 16, 1973 now abandoned.
FIELD, BACKGROUND AND SUMMARY OF THE INVENTION
In the conventional disc brakes, a caliper having friction pads is usually guided on a fixed support. In accordance with the present invention, an arm or bracket fixed to a rigid part of a vehicle structure is inserted in an aperture provided in the head portion of a caliper to support and guide the caliper so that the disc brake can be made more compact than the conventional ones.
This invention relates to a disc brake for vehicles, and more particularly to a compact disc brake which is applicable to small vehicles such as autobicycles.
It is an object of this invention to provide a disc brake suitable for small vehicles. In accordance with this invention, the conventional 2-cylinder, 2-piston opposed type disc brake is replaced with a floating caliper type. Furthermore, the caliper, which has hitherto been guided through a fixed support, is changed into a guided, suspended caliper type by providing a slot or an aperture in the head portion of the caliper, which straddles the periphery of a disc, and by inserting in the slot or aperture a fixed arm or bracket which extends horizontally in the rotational direction of the disc.
Another object of this invention is to provide a disc brake wherein guide pins provided on the head portion of the caliper are inserted in holes provided in the fixed arm or bracket so that the caliper can be slidably mounted and guided by the fixed arm or bracket.
A further object of this invention is to provide a disc brake wherein the play of the caliper is eliminated and a smooth braking operation is ensured by the use of a wave-shaped spring or antirattle spring inserted in between the caliper and the fixed arm or bracket.
A still further object of this invention is to provide a disc wherein the sliding part is effectively sealed either by the use of a boot arranged between the fixed arm or bracket and the end of the caliper or by placing the guide pins in blind holes provided in the caliper.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects, features and advantages of the invention will be apparent from the following detailed disclosure, taken in conjunction with the accompanying sheets of drawings, wherein like reference numerals refer to like parts, in which:
FIG. 1 is a plan view, partly in section, of one form of disc brake embodying the invention;
FIG. 2 is a sectional view taken on the line A--A of FIG. 1;
FIG. 3 is a sectional view taken on the line B--B of FIG. 2;
FIG. 4 is a sectional veiw illustrating another disc brake embodying the invention;
FIG. 5 is a sectional view taken on the line A'--A' FIG. 4; and
FIG. 6 is a sectional view taken on the line B'--B' of FIG. 5.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
In the first embodiment, illustrated in FIG. 1, 2 and 3, an arm is fixed in a cylindrical part of a rigid support, a caliper having an acting member on one side of a disc and a reacting member on the opposite side is provided with a slot, extending paralled to a tangent to the disk, in its head portion, and the fixed arm is inserted horizontally in the slot.
Furthermore, in this embodiment, an annular flange is provided on the back plate of a circular inner friction pad assembly which is positioned between the disc and the cylinder part of the caliper. A ring spring is placed between this annular flange and the outer side of a piston. An annular protrusion is provided on the back plate of an outer friction pad which is positioned between the disc and the reacting member of the caliper. This annular protrusion engages within an annular aperture provided in the reacting member of the caliper, while a ring spring is provided between the annular protrusion and the reacting member of the caliper. This arrangement prevents the rattling of the inner and outer friction pads and thus enables the caliper to receive the brake torque.
Referring to FIG. 1, the reference numeral 1 indicates a rigid support; 2 an arm fixed to the rigid support 1; 3 a caliper; 6 a cylindrical recess in the rigid support 1; 7 a support pin fixing the arm 2 to the rigid support 1; and 8 a bolt. A slot 9 is provided in the head portion 3a of the caliper 3 and extends horizontally parallel to a tangent to the disc 4. The arm 2 is placed in the slot 9. Holes 10 and 11 are provided in the head portion 3a of the caliper and the arm 2 respectively. Guide pins 12 extends through these holes. The adjacent ends of the rigid support 1 and the caliper head 3a are covered by a boot 13. The reference numeral 15 indicates the cylinder part of the caliper 3 and 16 the reacting member of the caliper.
Referring to FIG. 2, reference numeral 14 indicates a wave-shaped spring provided between the slot 9 of the caliper head 3a and the arm 2, 16 is the reacting member of the caliper, and 26 is an outer friction pad provided between the reacting member 16 and the disc 4. The arm 2 stretches over the periphery of the disc 4 to hold and guide the caliper 3, one end of the arm being fixed in the cylindrical recess 6 of the rigid support 1. However, the arm 2 and the rigid support 1 may be formed integral with each other.
Referring to FIG. 3, a piston 17 is fitted in cylinder 15 while an annular aperture 18 is provided in the reacting member 16. An inner friction pad 21 is provided between the piston 17 and the disc 4. The inner friction pad assembly comprises a back plate 19 and a pad 21a. An annular flange 20 of the back plate 19 is in contact with the guiding face 22 of the cylinder 15. A ring-shaped spring 23 is fitted in between the reverse side of the annular flange 20 and the outer side of the piston 17.
A dust seal 24 is provided between the inner face of the cylinder 15 and the outer face of the piston 17, and a piston seal 25 in between the cylinder 15 and the piston 17. An outer friction pad 26 is provided between the reacting member 16 of the caliper 3 and the disc. The friction pad assembly 26 comprises a pad 26a and a back plate 27. The back plate 27 is provided with an annular protrusion 28, which is either welded to or formed integrally with the plate. The annular protrusion 28 engages with the annular aperture 18 provided in the reacting member 16 of the caliper in such a manner that the braking torque developed at the outer friction pad 26 is transmitted to the reacting member 16. Between the annular protrusion 28 and the annular aperture 18, there is provided a ring-shaped spring 29 which prevents the rattle of the outer friction pad 26. The reference numeral 30 indicates a fluid inlet and 31 a fluid chamber of the cylinder 15.
The above described embodiment operates as follows: With a fluid pressure being received at the fluid chamber 31 through the inlet 30, the pressure causes the piston 17 to press the inner friction pad 21 against the disc 4, and a reaction to this pressure causes the reacting member 16 of the caliper to press the outer friction pad 26 against the disc 4 thus performing a braking action. At the time of the braking action, the reacting member 16 of the caliper operates as the guide pins 12 slide through the holes 11 of the arm 2 in parallel with the rotation axis of the disc, and the braking torque is transmitted to the rigid support 1 through the guide pins 12.
In the second embodiment, as illustrated in FIG. 4, 5 and 6, an inner caliper member 101 which has an acting element is formed separately from an outer caliper member 102 which represents a reacting element. A caliper guide pin which extends through a hole provided in the fixed bracket is inserted in blind holes provided in the caliper assembly. Inner and outer friction pads are guided by pins fixed to the flanges of the fixed bracket. The friction pad guide pins are located outside the caliper assembly so that the braking torque in this case is directly received by the fixed bracket.
Referring to FIG. 4, the inner caliper 101 and the outer caliper 102 are connected to each other by bolts 103 and 104 to form a caliper assembly. The reference numeral 105 indicates a cylinder; 106 a piston; 107 a fluid chamber of the cylinder 105; 108 a seal; 109 a boot, 110 an inner friction pad; 111 a back plate affixed to the pad 110; 112 an outer friction pad; 113 a back plate affixed to the pad 112; 114 a disc; 115 a caliper guide pin; 116 a fixed horizontally extending bracket; 117 a guide hole provided in the fixed bracket 116; 118 a rubber bush; 119 a boot which is formed together with the rubber bush in one unified piece; 120 a rubber ring; 121 the head portion of the outer caliper 102; 121a a slot, extending horizontally and parallel to a tangent to disc 114, provided in the outer caliper head 102 and receiving horizontal bracket 116; and 128 and 132 antirattle springs. In FIG. 5, 122 and 123 are the flanges of the fixed bracket 116; 124 and 125 the ear-shaped parts of the back plates of friction pads; 126a and 127a the holes which are provided in the parts 124 and 125 of the back plates and through which the respective pad guide pins 126 and 127 extend; 128 the antirattle spring which is located between the edge of the friction pad back plate 111 and the connecting bolts 103 and 104; 129, 130 and 131 the protrusions which are provided on the outer caliper 102 and which are in contact with the inner face of the inner caliper 101; and 121 the head portion of the outer caliper 102. There is provided another antirattle spring 132 between the head portion 121 of the outer caliper 102 and the fixed bracket 116. The numeral 133 indicates a fork of an autobicycle; 134 the flange of the fork; and 135 the mounting holes for fixing the fixed bracket 116 to the fork flange 134 by means of bolts.
FIG. 6 illustrates a pad guide pin 127 as extending between and through the flanges 123 and 123' of fixed bracket 116, and held in position by a head on one end and a spigot or cotter pin 136 inserted through the opposite end.
The embodiment illustrated by FIG. 4 operates as follows: When the fluid pressure of the fluid chamber 107 presses the inner friction pad 110 against the disc 114, the reaction to this action causes the caliper assembly (consisting of parts 101 and 102) to slide along the caliper guide pin 115 in the guide hole 117 of the fixed bracket 116. Then, the outer caliper member 102 presses the outer friction pad 112 against the disc 114 to effect the braking action.
As shown in FIG. 5, the antirattle spring 132 which is located between the head portion 121 of the caliper assembly and the fixed bracket serves to retain the stability of the caliper assembly (101 and 102) in the rotational direction of the disc 114. Another antirattle spring 128 which is in contact with the edge of the friction pad plate 111 serves to prevent rattling under the non-braking condition and squeaking under the braking condition.
Referring now to FIG. 6, the friction pads 110 and 112 can be guided by the pad guide pin 127 connected to the flanges 123 and 123' of the fixed bracket 116. Thus, the braking torque applied to the friction pads 110 and 112 is transmitted to the fixed bracket 116. Since these pad guide pins 126 and 127 are located outside the caliper assembly as shown in FIG. 5, the friction pads can be readily replaced by simply removing the spigot pin 136 (FIG. 6) and by pulling out guide pins 126 and 127.
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A single-cylinder, suspended caliper type disc brake includes a caliper assembly comprising an acting member disposed on one side of a disc and a reacting member on the opposite side thereof. A slot or an aperture is provided in the head portion of the caliper which straddles the periphery of the disc. The slot extends horizontally and parallel to a tangent of the disc, being located radially outwardly of the tangent. A fixed arm or bracket extends horizontally in the rotational direction of the disc and is inserted into the slot or aperture and supports the caliper assembly for guided movement in the axial direction of the disc.
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RELATED APPLICATIONS
This application is related to U.S. application Ser. No.10/173,579, titled Light Source For Generating Output Signal Having Evenly Spaced Apart Frequencies and filed on even date herewith, invented by Israel Smilanski, Isaac Shpantzer, Jacob B. Khurgin, Nadejda Reingand, Pak Shing Cho, and Yaakov Achiam, which application is incorporated herein.
FIELD OF THE INVENTION
The present invention relates to an acoustically tuneable light source and method for acoustically tuning a light source.
BACKGROUND OF THE INVENTION
Tuneable light sources output light comprising at least one of a plurality of frequencies. One type of tuneable light source, the tuneable distributed feedback (DFB) laser, has found applications in optical communications. The tuning time for DFB lasers, however, is on the order of milliseconds, which is slower than the microsecond tuning times required for modern optical communication systems.
Another example of a tuneable light source is a diode-pumped, packaged acousto-optically tunable Ti:Er:LiNbO3 waveguide laser described by K. Schafer et al., IEEE J. Quant. Electr., v.33, , #10, pp.1636-1641. This laser provides sub-millisecond tuning capability through TE-TM mode conversion within birefringent material. It would be desirable, however, to form a tuneable laser from non-birefringent materials, such as non-crystalline materials, because birefringent materials are more complex in manufacturing and operation.
SUMMARY OF THE INVENTION
A first embodiment of the invention relates to a light source. The light source comprises first and second optical waveguides, at least one of which waveguides comprises a gain medium. Upon excitation, such as by irradiation with light from a light source, the gain medium generates, such as by emitting, light having a plurality of frequencies, at least some of which may be output by the light source. The particular frequencies of light output by the light source may be acoustically switched at more than about 100 kHz.
The first and second waveguide define a first optical coupling region, wherein light, such as the generated light, propagating along one of the waveguides may couple to the other waveguide. Preferably, only light that couples between waveguides may be output by the tuneable light source. The optical frequency that couples between waveguides may be acoustically switched by subjecting the first optical coupling region to acoustic waves having a longitudinal frequency ω AC1 . Essentially the only light that may couple is light that satisfies a matching condition of the first coupling region whereby, upon coupling, a frequency of the light is shifted by about ±ω AC1 .
A second embodiment of the present invention is related to an integrated laser cavity that may be used to generate laser light. The laser cavity comprises first and second optical waveguides, which define an offset coupling region therebetween. By offset it is meant that longitudinal axes of the first and second optical waveguides are spaced apart from one another. At least one of the optical waveguides comprises a gain medium configured to, upon excitation, generate light.
Light propagating along one of the first and second waveguides may couple to the other waveguide at the coupling region. The frequency of light that may couple is acoustically tuneable by varying a first longitudinal acoustic wave vector K AC of acoustic waves impinging upon the first coupling region. Upon coupling from one waveguide to the other, a wave vector of the coupled light is shifted by an amount K AC . Preferably, only light that couples may be output by the integrated laser cavity.
Another embodiment of the invention relates to an integrated interferometer having at least first and second different optical paths. The interferometer includes first and second coupling regions, whereby light propagating along the first and second optical paths couples interferingly to a first waveguide and propagates therealong. A first acoustic wave source subjects the first and second coupling regions to acoustic waves having a first longitudinal acoustic wave vector K AC1 , whereby a wave vector of light propagating along one of the first and second optical paths differs from a wave vector of light propagating along the first waveguide by an amount K AC1 .
Another aspect of the invention relates to a method for producing light. In one embodiment, a gain medium within a first waveguide is irradiated with pump light to obtain generated light having an generated light frequency. The generated light is coupled to a second waveguide by subjecting at least some of the generated light to acoustic waves having a first frequency ω ACi to thereby provide second light having a second light frequency, wherein the second light frequency differs from the emitted light frequency by an amount ω ACi . At least some of the second light is output.
Another aspect of the invention relates to an optical transmitter that includes an optical cavity comprising an optical coupling region between first and second waveguides. An acoustic wave source is disposed to subject the optical coupling region to acoustic waves having an acoustic frequency ω i , whereby, upon coupling from one waveguide to the other, a frequency of light oscillating within the optical cavity is shifted by an amount of about ±ω i . The optical cavity is configured to output at least some of the oscillating light. The transmitter also includes an acoustic wave source driver for changing the acoustic frequency ω i , wherein a frequency of light output by the optical cavity changes upon changing the acoustic frequency ω i .
Light transmitted by the optical transmitter may be received by a receiver that simultaneously detects the transmitted light with light output by an acousto-optically tuneable optical cavity local to the receiver.
BRIEF DESCRIPTION OF THE DRAWINGS
The present invention is discussed below in reference to the drawings in which:
FIG. 1 shows a tuneable light source according to the invention;
FIG. 2 shows a partial view of a coupling region of the light source of FIG. 1;
FIG. 3 shows an example of an output spectrum of the light source of FIG. 1;
FIG. 4 shows an example of a second embodiment of a tuneable light source according to the invention;
FIG. 5 shows a plot of available output frequencies for the tuneable light source of FIG. 4;
FIG. 6 shows spectra that contribute to the output frequencies of FIG. 5;
FIG. 7 shows a third embodiment of a light source according to the invention; and
FIG. 8 shows a fourth embodiment of a light source according to the invention.
FIG. 9 shows a time-frequency plot of light output by a secure communication source the invention;
FIG. 10 shows a secure communication source of the invention suitable for preparing he time-frequency plot of FIG. 9; and
FIG. 11 shows a receiver of the invention for receiving information transmitted by the secure communication of FIG. 10 .
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIGS. 1 and 2, a light source, which in this embodiment is a laser 20 , which preferably includes first, second, and third waveguides 24 , 26 , and 28 . Laser 20 is preferably tuneable, by which it is meant that a frequency of light output by laser 20 may be varied. The laser 20 may be integral with a substrate 22 , such as by having the waveguides formed therein by, for example, diffusive doping. In general, preferred substrate materials are non-crystalline. Silica, such as amorphous silica, is an example of a suitable substrate material.
First and second waveguides 24 , 26 define a first coupling region 38 , wherein light propagating along one of the first and second waveguides may couple to the other waveguide to provide coupled light, which propagates therealong. First and third waveguides 24 , 28 define a second coupling region 40 , wherein light propagating along one of the first and third waveguides may couple to the other waveguide to provide coupled light, which propagates therealong. Preferred coupling regions of devices in accordance with the invention are essentially free of crystalline material. First and second coupling regions 38 , 40 are preferably spaced apart from one another along a general propagation dimension of the first waveguide 24 .
Tuneable laser 20 includes an optical cavity preferably having at least two reflective elements and including the first, second, and third waveguides. By “including the first, second, and third waveguides” it is meant that light oscillating within the optical cavity propagates along at least portions of each of the first, second, and third waveguides. Preferably, only light satisfying a matching condition may oscillate within the cavity. Oscillation within the optical cavity preferably comprises propagation of the light between respective ends 60 , 61 of second and third waveguides 26 , 28 . A first reflective element 42 may be optically associated with end 60 and preferably operates as an output coupler that is only partially reflective at output wavelengths of tuneable laser 20 . A second reflective element 44 may be associated with end 61 and preferably reflects substantially all light at output wavelengths of tuneable laser 20 .
First waveguide 24 has a propagation constant different from a propagation constant of second and third waveguides 26 , 28 , which may have the same propagation constant. As understood in the art, a propagation constant of a waveguide depends upon the dimensions, such as the height and width of the waveguide. Dimensions of first waveguide 24 may be different from dimensions of second and third waveguides 26 , 28 . The propagation constant also depends upon the refractive index of the material forming the waveguide. First waveguide 24 may have a refractive index that is different from respective refractive indexes of second and third waveguides 26 , 28 .
The polarization of light is preferably substantially maintained upon coupling at coupling regions of devices in accordance with light sources of the invention. For example, an angular difference between (1) coupled light that has coupled from one of the waveguides (here termed the origin waveguide) to another waveguide and (2) the light propagating along the origin waveguide is less than about π/2, such as less than about π/8.
Portions of at least one and preferably all of the first, second, and third waveguides 24 , 26 , and 28 are doped with a gain medium. The gain medium preferably generates light, such as fluorescence with a plurality of wavelengths in at least the C-band, when irradiated with pump light. Of course, the tuneable laser 20 is not limited to gain media generating light in the infrared. For example, gain media generating light in the visible may also be used. A preferred gain medium, such as a gain medium comprising Er(Yb, Nd), exhibits population inversion and lasing under suitable pumping conditions.
At least one of the waveguides is preferably configured to receive pump light from a pump source 63 . For example, first waveguide 24 receives pump light 21 from a light source 63 , which generates light that has a wavelength suitable to generate light from the gain medium. Preferably, each waveguide comprising gain medium receives pump light from a pump source. Of course, all of the waveguides receiving pump light may receive the pump light from a single pump source. An example of a pump source suitable for irradiating Er(Yb, Nd) is a diode laser emitting light in the infrared, such as at about 1480 nm. A waveguide may receive pump light via, for example, a facet at an end of the waveguide, side coupling, or grating coupling. Pump light received by a waveguide propagates therealong to thereby irradiate gain medium associated with the waveguide. Light sources in accordance with the present invention are not limited to optical pumping so that, for example, electrically pumped gain media may also be used.
As best seen in FIG. 2, waveguide portions 50 , 52 of respective first and second waveguides 24 , 26 that are adjacent to first coupling region 38 define respective longitudinal axes 54 , 56 , which are preferably essentially parallel. Light propagating along one of waveguide portions 50 , 52 propagates generally along its respective longitudinal axis 54 , 56 , which axes are preferably offset from one another. A coupling region in accordance with the invention may be described as an “offset” coupling region where light that is propagating along one waveguide of the coupling region translates laterally upon coupling to the other waveguide of the coupling region.
Coupling regions of the invention are preferably configured to substantially prevent light that does not couple from one waveguide to another from continuing to propagate along the waveguide. First and second waveguide portions 50 , 52 preferably include attenuation regions 71 , 73 to attenuate light that has not coupled from one of the waveguides 24 , 26 to the other. Attenuation regions 71 , 73 may be shaped, such as by tapering, to attenuate light. Thus, for example, light satisfying a matching condition discussed below and propagating along first waveguide portion 50 toward attenuation region 71 couples to second waveguide portion 52 of second waveguide 26 . Preferably, however, propagating light that fails to satisfy the matching condition is substantially prevented from continued propagation by attenuation region 71 .
Tuneable laser 20 includes a first acoustic wave source 30 to facilitate variable wavelength coupling between first and second waveguides 24 , 26 . First acoustic wave source subjects first coupling region 38 to acoustic waves 46 having a variable frequency ω AC1 and propagating generally along a propagation axis 48 . A second acoustic wave source 32 subjects second coupling region 40 to acoustic waves (not shown) also having a variable frequency ω AC2 and propagating with a velocity V AC generally along a propagation axis 49 to thereby facilitate variable wavelength coupling between first and third waveguides 24 , 28 . First and second acoustic wave sources 30 , 32 may be piezo-electric transducers. Frequencies ω AC1 and ω AC2 may be the same or different.
First and second acoustic wave sources are operably associated with at least one acoustic wave source driver, which provides an acoustic frequency signal to the acoustic wave sources to vary the respective acoustic frequency output by each source.
An acoustic absorber 37 may be disposed to absorb or otherwise prevent acoustic waves 46 that have passed through first coupling region from returning therethrough, such as by reflection. A second acoustic absorber 36 may be disposed to absorb or otherwise prevent acoustic waves emitted by second acoustic wave source 32 that have passed through second coupling region 40 from returning therethrough, such as by reflection. Additional acoustic absorbers may be positioned to substantially prevent propagation of the acoustic waves lateral to propagation axes 48 , 49 .
Suitable coupling conditions for the coupling of light from one waveguide to another are discussed next using light propagating along first waveguide 24 and coupling to second waveguide 26 at first coupling region 38 as an example. It should be understood, however, the following coupling conditions also pertain coupling at coupling region 40 as well as coupling region of other light sources of the invention. A suitable condition for coupling is defined herein as a matching condition.
A wave vector K 2 of an optical wave 23 propagating along waveguide 24 is given by: K 2 = ω 23 c n 24 Eq . 1
where ω 23 is a frequency of optical wave 23 , c is the speed of light in a vacuum, and n 24 is the index of refraction of waveguide 24 for light having a frequency ω 23 . Acoustic wave source 30 subjects first coupling region 38 to acoustic waves 46 having a frequency ω AC , which waves travel with a longitudinal velocity V AC with respect to first coupling region 38 . By longitudinal frequency, it is meant the component of the acoustic waves taken along a longitudinal axis 54 of first waveguide 24 .
Acoustic waves 46 have an acoustic wave vector K AC and form an acoustic grating having a period ΔK given by: K A C = Δ K = ω A C V A C Eq . 2
The acoustic grating interacts with optical wave 23 , such as by scattering at least some of optical wave 23 , to provide an optical wave having a wave vector K 1 =K 2 +ΔK. At least some of the optical wave with wave vector K 1 couples into waveguide 26 and propagates therealong with wave vector K 1 , where the wave vector K 1 is given by: K 1 = ω 27 c n 26 = K 2 + Δ K Eq . 3
where ω 27 is a frequency of optical wave 27 and n 26 is a refractive index of waveguide 26 for light having a frequency ω 27 .
The matching condition, ΔK, is the difference between the wave vectors of optical waves 23 and 27 , is given by the period of the acoustic grating: Δ K = ω AC V AC = ω 27 c n 26 - ω 23 c n 24 = ω 27 c Δ n + Δ ω c n 24 Eq . 4
where Δn is a refractive index difference given by n 26 −n 24 and Δω is a frequency difference given by ω 27 −ω 23 .
When the matching condition is satisfied, light having a wave vector K 2 will couple from first waveguide 24 to second waveguide 26 . Likewise, light having a wave vector K 1 will couple from second waveguide 26 to first waveguide 24 . A similar matching condition must be met before light will couple in either direction between first waveguide 24 and third waveguide 28 at second coupling region 40 . Oscillation, and therefore lasing, will only occur at frequencies for which the matching condition is satisfied. Thus, acoustic sources 30 , 32 determine the frequency of light that is output by tuneable laser 20 for any given acoustic wave frequency.
Assuming that (Δω/c) n 24 is negligible compared to other terms in Eq. 4, a frequency ω out of light that may be output by tuneable laser 20 is given by ω out = c ω AC Δ nV AC Eq . 5
During use, tuneable light source 20 may operate as follows. Gain medium within at least one of first, second, and third waveguides 24 , 26 , 28 is irradiated with pump light 21 . Upon pumping, the gain medium generates light having a plurality of frequencies. At least one of first and second coupling regions are subjected to acoustic waves having a frequency ω AC so that light that is generated and propagates along, for example, first waveguide 24 may couple to, for example, the second waveguide 26 . Because only one frequency of the generated light may satisfy a given matching condition, the coupled light comprises essentially only light having the satisfying frequency. Thus, tuneable light source may be acoustically tuned by varying ω AC to output light having any one of the frequencies generated by the gain medium. The acoustic frequency ω AC is preferably varied using the acoustic wave source driver associated with the acoustic wave generators. The frequency of light output by tuneable laser 20 , like all tuneable light sources of the invention, may be varied, by changing the frequency of acoustic waves ω AC , between first and second frequencies in less than about 50 μs and preferably in less than about 10 μs.
As an example of using Eq. 5 to determine ω out , substitute c=3×10 8 m/s, Δn=1×10 −2 , V AC =3×10 4 m/s, and ω AC =2×10 8 Hz to predict an output frequency of 2×10 14 Hz, which corresponds to a wavelength of about 1.5 μm. Varying the acoustic wave frequency ω AC over a range of about 191 to 196 MHz allows the output wavelength to be tuned over the range of about 1.53 to 1.57 μm. Of course, the acoustic wave frequency may be varied over wider ranges, such as about 170 to about 220 MHz or even wider ranges, to provide output wavelengths of less than 1.53 μm or greater than 1.57 μm.
Referring to FIG. 3, the spectrum of light output by tuneable laser 20 includes a output spectrum 51 light having a range of frequencies centered at ω out . Preferably, however, the output spectrum 51 includes substantially fewer frequencies than light emitted by the gain medium of the waveguides. A width w 1 of output spectrum is preferably sufficiently narrow that the output spectrum 51 can be considered, as referred to above, to consist essentially of a single frequency of light. In terms of wavelength, for example, a line width of single frequency light output by tuneable light sources of the invention is less than about 0.5 nanometers, such as less than about 0.1 nanometers.
Referring to FIG. 4, a discretely tuneable light source, which in this embodiment is a tuneable laser 100 , is configured to output light having one of a set of discrete frequencies. Tuneable laser 100 includes a substrate 102 , which preferably includes first, second, third, and fourth wave guides 104 , 106 , 108 , and 110 . An interferometer 115 defines, at least in part, the set of discrete frequencies available to be output by tuneable laser 100 . Substrate 102 may be formed of material identical to that of substrate 22 .
At least one and preferably both of second and third waveguides 106 , 108 include a gain medium, which can be identical to the gain medium discussed above for tuneable laser 20 . At least one of the waveguides 104 , 106 , 108 , 110 is configured to receive light from a pump source 121 to irradiate gain medium of the first and second waveguides. For example, second and third waveguides 106 , 108 of tuneable laser 106 are configured to receive pump light 120 , which propagates along waveguides 106 , 108 irradiating gain medium therein. The pump source 121 may be identical to the pump source described above for tuneable laser 20 . The output from a single pump source may be split, such as by a beam splitter 171 and steered, such as by a mirror 173 to respective waveguides.
Tuneable laser 100 includes a first coupling region pair 112 . A coupling region pair preferably comprises a pair of coupling regions where light may couple between each of two waveguides and a third waveguide. For example, coupling region pair 112 includes first and second coupling regions 112 a, 112 b. A first acoustic wave source 116 subjects the first coupling region pair 112 to acoustic waves. Upon activation of acoustic wave source 116 , light satisfying a matching condition will couple between first waveguide 104 and second and third waveguides 106 , 108 .
Tuneable laser 100 includes a second coupling region pair 114 comprising third and fourth coupling regions 114 a, 114 b. A second acoustic wave source 118 subjects the second coupling region pair 114 to acoustic waves. Upon activation of the acoustic wave source 118 , light satisfying a matching condition will couple between fourth waveguide 110 and second and third waveguides 106 , 108 .
At least one of the waveguides of tuneable laser 100 is configured to output light that has propagated along the waveguide. For example, fourth waveguide 110 includes an output coupler 117 , which allows a first portion of light propagating along fourth waveguide 110 to be emitted as output light 122 . A second portion of light propagating along fourth waveguide 110 is reflected by output coupler 117 to thereby return along fourth waveguide 110 . The returning light may couple into second and third wave guides 106 , 108 , where the light propagates along until coupling into first waveguide 104 , where the light propagates therealong until reaching a reflector 119 , which preferably reflects substantially all light incident upon it. Thus, output coupler 117 , reflector 119 and the waveguides define an optical cavity, which may be a laser cavity supporting oscillation within a gain medium therein. As discussed below, oscillation only occurs when the light propagating within laser 100 satisfies both a matching condition for coupling and experiences constructive interference upon coupling.
Referring to FIGS. 5 and 6, the available output frequencies 129 of laser 100 define a “comb” of essentially equally spaced frequencies. The particular frequency that is output by tuneable laser 100 is determined by a gain spectrum 130 of the gain medium, an interferometer spectrum 132 of interferometer 115 , and an acoustic grating spectrum. For convenience of the following discussion, FIG. 6 shows two acoustic grating spectra 134 a and 134 b.
It should be understood that the optical cavity defined by just the output coupler 117 and the reflector 119 (without the waveguides) creates a comb of frequencies, which are narrowly spaced compared to the available output frequencies 129 of laser 100 . Therefore, the frequency comb defined by the optical cavity does not substantially affect the output frequencies available from laser 100 .
The gain spectrum 130 is determined by frequencies at which the gain medium of tuneable laser 100 generates light upon pumping, such as by irradiation with pump light. For a laser, such as tuneable laser 100 , a gain spectrum represents a broad envelope of frequencies at which lasing may occur, as understood in the art. A preferred gain spectrum covers at least a portion, and preferably all, of the C-band of frequencies. Interferometer 115 determines which frequencies of gain spectrum 130 are available for output by tuneable laser 100 .
Interferometer spectrum 132 is defined by interferometer 115 . Tuneable laser 100 may output light at frequencies corresponding to each maximum of interferometer spectrum 132 . Essentially no light may be output at frequencies corresponding to minima of interferometer spectrum 132 . The maxima and minima are determined by frequencies for which interferometer 115 causes constructive or destructive interference of light propagating therein.
Interference occurs because interferometer 115 includes at least two optical paths, each having a respective different length. Preferably, interferometer 115 is a Mach Zehnder interferometer having respective optical paths along second and third waveguides 106 , 108 . An optical path length along third waveguide 108 is greater than an optical path length along second waveguide 106 . As defined herein, the optical path lengths of each of the second and third waveguides 106 , 108 is the length of the respective waveguide between first and second coupling region pairs 112 , 114 . The frequency spacing, ΔF, between adjacent maxima of interferometer spectrum 132 is given by ΔF=c/(n×Δp), where n is the refractive index of the longer waveguide and Δp is the absolute path length difference. For LiNbO 3 , a 25 GHz spacing ΔF corresponds to about 5.4 mm path length distance difference. A 12.5 GHz spacing corresponds to a 10.8 mm path length difference. A 200 GHz spacing corresponds to a 1.35 mm path length difference.
As an example of interference caused by interferometer 115 , consider light, propagating along first waveguide 104 , which light couples, at first coupling region pair 112 , into both second and third waveguides 106 , 108 to propagate therealong. The light then propagating along each of the second and third waveguides 106 , 108 couples, at second coupling region pair 114 , into fourth waveguide 110 , whereupon interference occurs. The light may be said to have interferingly coupled by way of the coupling region pair. The interference is selective, either constructive or destructive, because of the path length difference along second and third waveguides 106 , 108 . Of course, interference also occurs at first coupling region pair 114 for light propagating in the opposite direction.
Maxima, such as maxima 133 , 135 , and 137 , of interferometer spectrum 132 are centered at frequencies for which constructive interference occurs. Thus, the maxima correspond to light for which the optical path length difference along second and third waveguides 106 , 108 is an integral multiple of the wavelength of the light propagating therealong. Minima, such as minima 139 , 141 , and 143 , of interferometer spectrum 132 are centered at frequencies for which destructive interference occurs. The frequency minima correspond to light for which the optical path length difference along second and third waveguides 106 , 108 is a integral multiple of ½ of the wavelength of the light propagating therealong.
The acoustic grating spectrum of tuneable laser 100 , is defined by the narrowest range of frequencies that will couple efficiently between (1) first waveguide 104 and second, third waveguides 106 , 108 , or (2) fourth waveguide 110 and second, third waveguides 106 , 108 . Light exactly satisfying a matching condition will couple efficiently from one waveguide to another. However, light that has a frequency only slightly different will also couple at least in part because of the finite size of the acoustic grating and coupling region. In practical terms, therefore, a distribution of frequencies will couple from one waveguide to the other. Of course, only a small range of frequencies (the acoustic grating spectrum) will couple efficiently enough to lase. A central frequency of the acoustic grating spectrum may be varied by varying the frequencies of acoustic waves impinging upon the first and second coupling regions.
During operation, gain medium within tuneable laser 100 may be irradiated with pump light from a pump source to thereby obtain emitted light that propagates along waveguides of tuneable laser 100 . First and second coupling region pairs are subjected to acoustic waves from first and second acoustic wave sources, respectively. The acoustic waves from the first and second acoustic wave sources may have the same frequency. Preferably, substantially all light coupling between the waveguides has a frequency corresponding to a matching condition of a respective coupling region.
To select an output frequency corresponding to a particular one of the maxima of interferometer spectrum 115 , the frequency of acoustic waves impinging upon the coupling pairs are varied so that the acoustic grating spectrum overlaps the particular maximum. For example, first acoustic grating spectrum 134 a has a central frequency 145 that coincides with a maximum 137 of interferometer spectrum 132 . Tuneable laser 100 would output light corresponding to central frequency 145 . On the other hand, second grating spectrum 134 b has a central frequency 147 that coincides with a minimum 139 of interferometer spectrum 132 . Essentially no light would be output for this condition.
Upon coupling, light having a wavelength that provides destructive interference is attenuated compared to light having a wavelength that provides constructive interference. Thus, even if the acoustic wave frequency is tuned so that light propagating within the waveguides of tuneable laser 100 satisfies a matching condition allowing the light to couple, oscillation will not occur unless the frequency of the light experiences constructive interference at first and second coupling pairs 112 , 114 .
Light is output from at least one of the waveguides, such as through output coupler 117 of fourth waveguide 110 . Preferably, substantially all of the light output from tuneable laser 100 satisfies both a matching condition of the first and second coupling regions and has a wavelength corresponding to constructive interference. Tuning the wave vector K AC of acoustic waves output by first and second acoustic wave sources allows light corresponding to a particular one of the discrete set of frequencies to be obtained. Thus, tuneable laser 100 outputs light having one of a discrete set of frequencies corresponding to maxima of interferometer spectrum 132 .
Referring to FIG. 7, a tuneable laser 200 includes first and second interferometers to thereby provide a comb of output frequencies having teeth with a narrower width than teeth of a comb of a laser having only a single interferometer. Tuneable laser 200 , which is preferably integral with a substrate 202 , includes first, second, third, and fourth, waveguides 204 , 206 , 208 , and 210 having a configuration similar to waveguides 104 , 106 , 108 , and 110 of tuneable laser 100 . Tuneable laser 200 defines an optical cavity between a first reflector 219 and a second reflector 221 .
A first interferometer of tuneable laser 200 includes a first coupling region pair 212 , including first and second coupling regions 212 a, 212 b and a second coupling region pair 214 , including third and fourth coupling regions 214 a , 214 b. An optical path along third waveguide 208 is greater than an optical path along second waveguide 206 . Thus, light propagating along second and third waveguides 206 , 208 and coupling at first or second coupling region pair 212 , 214 will experience interference, as discussed above for interferometer 115 .
A second interferometer of tuneable laser 200 includes third and fourth coupling regions 223 , 225 . Third coupling region 223 couples light between first waveguide 204 and a fifth waveguide 211 . Fourth coupling region 225 couples light between fifth waveguide 211 and fourth waveguide 210 . At each of coupling regions 223 , 225 , coupling may occur in either direction. A first optical path, between third and fourth coupling regions 223 , 225 , along fifth waveguide 211 is different than a second optical path, between third and fourth coupling regions 223 , 225 . Thus, upon coupling at either of third and fourth coupling regions 223 , 225 , interference occurs between light having traveled along the first and second optical paths. The second optical path includes first interferometer 215 .
A first acoustic wave source 216 subjects third coupling region 223 and first coupling region pair 212 to acoustic waves. A second acoustic wave source 218 subjects second coupling region pair 214 and fourth coupling region 225 to acoustic waves. The frequencies of acoustic waves impinging upon third coupling region 223 and second coupling region pair 214 can be varied to select the output frequency of tuneable laser 200 . Although FIG. 7 shows that acoustic wave sources 216 and 218 each subject more than 1 coupling region to acoustic waves, it should be understood that each coupling region may be provided with a dedicated acoustic wave source. Also, devices in accordance with the present invention may be configured with an acoustic wave source that subjects more than 2 coupling regions to acoustic waves. Light source 200 may also include acoustic wave absorbers, which may be similar to acoustic wave absorbers 36 and 37 of light source 20 .
Referring to FIG. 8, a tuneable light source, which in this embodiment is a tuneable laser 300 , outputs light having one of a set of discrete optical frequencies. The available output frequencies of tuneable laser 300 are determined by the output frequencies of a secondary light source, such as a comb generator 330 , which preferably emits light 331 having a plurality of equally spaced frequencies. The output of tuneable laser 300 can be acoustically tuned to output light at any one of the frequencies received from the external source. A comb generator suitable for use as a secondary light source is described in U.S. application Ser. No. 10/173,579, titled Light Source For Generating Output Signal Having Evenly Spaced Apart Frequencies, filed on even date herewith, invented by Israel Smilanski, Isaac Shpantzer, Jacob B. Khurgin, Nadejda Reingand, Pak Shing Cho, and Yaakov Achiam, which application is incorporated herein.
Tuneable laser 300 , includes a substrate 302 , which preferably includes first, second, and third waveguides 324 , 326 , and 328 . First and second waveguides 324 , 326 define a first coupling region 338 , wherein light propagating along one of the first and second waveguides may couple to the other waveguide to propagate therealong. First and third waveguides define a second coupling region 340 , wherein light propagating along one of the first and third waveguides may couple to the other waveguide to propagate therealong. The coupling regions 338 , 340 are identical to coupling regions 38 , 40 .
Tuneable laser 300 includes a first and second acoustic wave sources 330 , 332 , which operate identically to acoustic wave sources 30 , 32 to thereby facilitate variable wavelength coupling of light at first and second coupling regions 338 , 340 . Acoustic absorbers 334 , 336 operate identically to acoustic absorbers 36 , 37 of tuneable laser 20 .
First and second reflective elements 317 , 319 define an optical cavity including first, second, and third waveguides 324 , 326 , and 328 . First element 317 is preferably an output coupler. Second reflective element 319 is preferably sufficiently transmissive to allow at least some of the light 331 output by comb generator 330 to be received by waveguide 328 . Light having a frequency that satisfies a matching condition determined by a frequency of acoustic waves output by acoustic wave sources 330 , 332 , may couple between waveguides at first and second coupling regions 338 , 340 and, therefore, oscillate within the optical cavity.
Portions of at least one and preferably all of the first, second, and third waveguides 324 , 326 , and 328 are doped with a gain medium. At least one of the waveguides is configured to receive pump light 320 from a pump source 321 . The gain medium and pump source may be identical to those described for tuneable laser 20 .
At least one of the waveguides 324 , 326 , 328 is configured to receive light 331 from the comb generator 330 . Light 331 from comb generator 330 seeds the gain medium of tuneable laser 300 such that lasing occurs preferentially at frequencies of light 331 . Oscillation and, therefore, lasing, will only occur, however, at frequencies which also satisfy the matching condition as discussed above. Thus, by varying the frequency of acoustic waves impinging upon first and second coupling regions 338 , 340 , the output frequency of tuneable laser 300 can be varied between discrete frequencies corresponding to frequencies of light 331 .
In order to prevent the frequencies of light 331 , and, therefore the frequency of light output by tuneable laser 300 , from varying, the comb generator 330 may be locked, such as to a frequency stabilized reference laser 360 . Locking comb generator 330 substantially prevents the frequencies of light 331 from shifting from one optical frequency to another. Locking may be performed by, for example, either injection-locking or phase-locking. An example of a comb generator and method for locking a laser to a comb generator is discussed by C. F. Silva et al. in “Exact Optical Frequency Synthesis Over 1 THz Using SG-DBR Lasers,” Proceedings CLEO-Europe-IQEC 2000 conference, Nice, France, September, 2000, which proceeding is incorporated by reference herein to the extent necessary to understand the present invention.
Referring to FIG. 9, a method for secure optical communication includes varying, as a function of time, a frequency of light encoding transmitted information. This secure optical communication system uses optical spread spectrum techniques. During a first time period t 1 , information is encoded, such as by amplitude or, preferably, phase modulation of light having a frequency ω 1 . During a second time period t 2 , information is encoded by modulation of light having a frequency ω 2 , which may be the same as or different from ω 1 . In general, information is encoded, during the ith time period, by modulation of light of a frequency ω i . The encoding step is repeated for a number N t times until all the information has been transmitted. At each successive time period, information may be encoded upon light having a frequency different or the same as a frequency of light encoded upon during the previous time segment. Thus, the information is encoded upon light having a number of frequencies N ω , which number may be less than N t . The length of the time periods may be the same or may vary from period to period. The encoded information is transmitted to the receiver.
Light encoding the information upon the plurality of frequencies is transmitted, such as through free space or a fiber optic network to a receiver, where the information is decoded. Because the frequency of the transmitted light switches from frequency to frequency, one without knowledge of the transmission frequency sequence is prevented from decoding the transmitted information.
Referring to FIG. 10, a transmitter 408 having a light source 410 , which may be a light source in accordance with the present invention, is preferably used to provide the light which is modulated to encode the information. An acoustic wave source driver 414 varies an acoustic wave frequency of light source 410 to prepare an output beam 412 that switches between a plurality of frequencies as a function of time. Output beam 412 is received by a modulator 416 , which modulates output beam 412 with information from a data source 419 to prepare a modulated output beam 418 .
Modulator 416 is preferably a phase modulator, which prepares an optical signal that encodes information by, for example, phase shift keying, binary phase shift keying or quaternary phase shift keying. During the ith time period, phase modulator 416 modulates a phase of light having a frequency ω i of output beam 412 to encode information from data source 419 . During the jth time period, where j=i+1, phase modulator 416 modulates a phase of light having a frequency that may be the same as or different from ω i . Modulated output beam 418 is transmitted by transmitter 408 to be received and decoded by one having knowledge of the successive frequencies used to encode the information. The information may be decoded using, for example, homodyne or heterodyne detection.
Referring to FIG. 11, a heterodyne receiver 450 includes a local oscillator 451 providing an oscillator beam 452 having a variable frequency corresponding to the variable frequency of received output beam 418 . Local oscillator 451 preferably comprises any of the light sources of the invention. Oscillator beam 452 and output beam 418 are combined 453 and detected by an optical detector 454 . It is preferable that a frequency mismatch between beams 452 and 418 is less than about 1 GHz, such as less than about 250 MHz.
While the above invention has been described with reference to certain preferred embodiments, it should be kept in mind that the scope of the present invention is not limited to these. Thus, one skilled in the art may find variations of these preferred embodiments which, nevertheless, fall within the spirit of the present invention, whose scope is defined by the claims set forth below.
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The present invention relates to an integrated light source having first and second optical waveguides defining a first optical coupling region for coupling light therebetween. At least one of the optical waveguides includes a gain medium configured to emit light upon irradiation. The light source also includes a first acoustic wave source to subject the first optical coupling region to acoustic waves having a longitudinal frequency ω AC1 , whereby a frequency of light propagating along one of the first and second waveguides differs from a frequency of light propagating along the other waveguide by an amount by an amount ω AC1 .
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TECHNICAL FIELD
[0001] This description relates to displaying a model-based computer user interface.
BACKGROUND
[0002] Computer systems often are used to manage and process business data. To do so, a business enterprise may use various application programs running on one or more computer systems. Application programs may be used to process business transactions, such as taking and fulfilling customer orders, providing supply chain and inventory management, performing human resource management functions, and performing financial management functions. Application programs also may be used for analyzing data, including analyzing data obtained through transaction processing systems. In many cases, application programs used by a business enterprise are developed by a commercial software developer for sale to, and use by, many business enterprises.
[0003] Many user interfaces allow users to review, edit or enter data on a number of different panels displayed by a computer system. Some computer systems enable a user to navigate back and forth between panels at will to review, edit and enter data. Computer systems may require multiple users to review, edit or enter related data. Some users may perform different roles and functions within a computer system, and users having different roles may need to work together to process a transaction within the computer system.
SUMMARY
[0004] In one general aspect, a user interface is displayed on a computer display device. A model panel is displayed, on a computer display device, in a computer user interface where the model panel corresponds to one of an academic model or an industry model. The displayed model panel includes model components. User input that requests access to information related to one of the model components is received. Information related to the one of the model components in a second panel in the computer user interface is played on the computer display device. The second panel and the model panel are able to be viewed concurrently in the computer user interface.
[0005] Implementations may include one or more of the following features. For example, user input requesting access to information related to a second model component of the model components may be received. The second panel may cease to be displayed, and information related to the second model component may be displayed on the computer display device in a third panel in the computer user interface such that the third panel and the model panel are able to be viewed concurrently in the computer user interface.
[0006] Information related to each of the model components may be accessible to be displayed when the model panel is able to be viewed in the computer user interface. Each of the model components may be operable to display information related to the model component.
[0007] User input identifying a subject of information to be displayed in the computer user interface may be received. A determination may be made as to whether each model component is able to display information related to the subject of information. Based on the determination, a first presentation style may be used for model components for which information related to the subject information is able to be displayed and a second, different presentation style may be used for model components for which information related to the subject information is not able to be displayed.
[0008] A control may be displayed proximate to a model component, where the control is operable to display a subset of information related to the model component.
[0009] Implementations of any of the techniques described above may include a method or process, an apparatus or system, or computer software on a computer-accessible medium. The details of particular implementations are set forth in the accompanying drawings and description below. Other features will be apparent from the following description, including the drawings, and the claims.
DESCRIPTION OF DRAWINGS
[0010] FIG. 1 is a block diagram of a computer system capable of displaying a user interface providing a model-based navigation pattern.
[0011] FIGS. 2 and 3 are block diagrams of user interfaces providing model-based navigation patterns.
[0012] FIG. 4 is a flow chart of a process for displaying a user interface providing a model-based navigation pattern.
[0013] FIGS. 5-7 schematically show an example user interface providing a model-based navigation pattern.
[0014] Like reference symbols in the various drawings indicate like elements.
DETAILED DESCRIPTION
[0015] Techniques are described for a user interface providing a model-based navigation pattern of multiple displays in a computer system. The navigation pattern of multiple displays represents and directly relates to a generally known model. Presenting a user interface having a model-based navigation pattern may facilitate a user's comprehension of a collection of related data. The navigation pattern of multiple displays may be used in addition to, or in lie of, an application user interface that otherwise would be used to review, edit or enter data in a computer system. A model-based navigation pattern may be useful to enable a user who is not generally familiar with an application program to interact with data available through the application program.
[0016] A user interface that represents a generally known model of a business or business process may enable a user to more easily understand and navigate a large or complex collection of computer data. In one example, an executive of an organization may not commonly enter business data through an application user interface and may not be familiar with how to navigate through application user interfaces to review or edit data. The executive, however, may be familiar with an academic or industry business model that may be used to present or represent the business data entered through the application. In such a case, it may be advantageous to provide a user interface to business data using a model-based navigation pattern that represents a generally known academic or industry business model.
[0017] Referring to FIG. 1 , a computer system 10 includes a processing unit 12 , one or more input devices 14 , and a display device 16 that may present displays of a user interface to a user. The display device 16 has a screen 18 upon which the displays may appear. The system 10 is capable of presenting a user interface with enhanced navigation through displayed panels on the display device 16 as described below.
[0018] The processing unit 12 includes a processor 20 , random access memory (RAM) 22 , and read-only memory (ROM) 24 , all interconnected by a data bus 26 . Input device controllers 28 , also connected to the data bus 26 , receive command signals from input devices 14 and forward the command signals in the appropriate format for processing. A video controller 30 , connected to the data bus 26 , receives video command signals from the data bus 26 and generates the appropriate video signals that are forwarded to the display device 16 so that the desired display is provided on the screen 18 . The computer system 10 is not limited to a personal computer, but could instead include a personal digital assistant, a terminal, a workstation, or other such device.
[0019] ROM 24 , as is conventional, may provide non-volatile data storage for various application programs 32 , 34 , etc. Programs 32 and 34 have program instructions that may be loaded into RAM 22 during operation. Processor 20 may then execute the program instructions, as required, to perform particular program functions. Also stored in ROM 24 is a model-based user interface program 36 that may be designed to work in concert with each of the application programs 32 , 34 , etc. This is conceptually depicted in FIG. 1 by the user interface program 36 being shown as a layer on top of the application programs 32 , 34 , etc.
[0020] With such a design, user interface program modules common to several application programs need not be duplicated in each of the application programs. The user interface program 36 may create a display of a model-based navigation pattern of displays to be presented to a user on screen 18 of display device 16 . The user may interact with the display by providing input using an input device 14 , such as a mouse, keyboard, light pen, touchpad, joystick, etc. The user interface program 36 may use the received input to take appropriate actions, such as updating the display, creating a new display, interacting with applications programs 32 and/or 34 , accessing a database 38 , or accessing server 40 (described below), to list just a few examples. In other implementations, the user interface program 36 need not be a common program or module for more than one program application. Also, the components just described could be combined or separated in various manners, and could be stored in various manners, such as on various non-volatile storage medium.
[0021] Also shown in FIG. 1 is server 40 . The computer system 10 may access server 40 to run applications residing on the server 40 . The computer system 10 may do so by using a network interface 42 connected to its data bus 26 to access a network 44 . Network 44 may be, for example, a local area network (LAN), wide area network (WAN), or a network that allows the computer system 10 and the server 40 to be part of the Internet. As is conventional, the server 40 includes a network interface 46 , a processor 48 , RAM 50 , and ROM 52 , all interconnected by a data bus 54 . The server's network interface 46 provides the connection to network 44 so that client computer systems, such as system 10 , can access the server 40 . In similar fashion to computer system 10 , the server ROM 52 includes various different application programs 56 , 58 , etc., as well as a common user interface program 60 for the application programs 56 , 58 , etc. User interface program 60 may operate similarly to user interface program 36 . Any of the entities described above in the server ROM 52 could alternatively be located in a separate server, database, or computer system.
[0022] FIG. 2 illustrates a schematic representation 200 of displaying business data 210 in both an application user interface 220 and a user interface 230 providing a model-based navigation pattern. The business data 210 includes transaction data 210 A, such as, for example, data representing sales orders, purchase orders, delivery orders, customers, suppliers, employees and work flow data related to document processing. Some implementations may make a distinction between master data and processing data in transaction data 210 A. Transaction data that represents principal entities and documents (such as data representing sales orders, purchase orders, delivery orders, customers, suppliers, and employees) may be referred to as master data. Transaction data that includes transient processing data, such as workflow data or approval data may be referred to as processing data. The business data 210 may include analytical data 210 B, such as analytical data generated and stored in a data warehouse.
[0023] As illustrated, the business data 210 may be reviewed, edited and entered using application-based displays 220 that are generated by application programs. Application programs, for example, may include a customer relationship management application program, a supply chain management application program, an inventory management application program, a human resource management application program and a financial management application program. In some cases, application programs may have complex user interfaces that require a user to have significant experience to understand and efficiently use. For example, a user interface for an application program may be designed to enable efficient operation by users of performing a function on a routine basis.
[0024] In the example of FIG. 2 , the application-based displays 220 include a series of displays 220 A for entering, editing and reviewing sales orders, a series of displays 220 B for entering, editing and reviewing purchase orders, and a series of displays 220 C for inventory management. The application-based displays 220 A, 220 B and 220 C each present sequential displays such that, for example, a user must navigate through displays 221 A, 222 A, 223 A and 224 A before reaching display 225 A.
[0025] The business data 210 may be reviewed, edited and entered using a user interface 230 based on a model-based navigation pattern 230 A, 230 B, 230 C, 230 D and 230 E. In the example of model-based navigation displays 230 , the displays represent a generally known academic business process model. For example, the model may be a generally known business process model that represents the general relationship common among business enterprises between purchasing, inventory management, production, sales and financial management. One example of such a model is Michael Porter's value chain model.
[0026] In contrast to sequential application-based displays 220 A, 220 B and 220 C, each of the model-based navigation pattern displays 230 A- 230 F may be accessed by a user from any other model-based navigation pattern displays 230 A- 230 F, as represented by the circle 225 .
[0027] FIG. 3 illustrates another example schematic representation 300 of a user interface 310 based on a model-based navigation pattern. The user interface 310 may be displayed, for example, on a display device 16 of a computer system 10 , as previously described with respect to FIG. 1 .
[0028] The user interface display 310 includes product information (here, a product number 312 and a product description 314 ) identifying a particular product to which the display 310 applies. The display 310 also includes controls 320 that enable a user to display information related to the particular product based on a generally known model (rather than through various application user interfaces that could be used to enter, edit or review the product information). In this example model, the model, including the model components, is generally known and includes an inventory component, a sales component and a financial component. The controls 320 include controls 330 A and 330 B that correspond to the model's inventory component, controls 340 A- 330 C that correspond to the model's sales component and controls 350 A- 350 C that correspond to the model's financial component. The controls 320 of the display 310 also include a basic data control 360 operable to display basic data about the particular product, such as, for example, a catalog description or types of technical information.
[0029] The controls 330 A- 350 C are operable to display information from business data 370 . In this example, the business data 370 is stored in a relational database and includes sales order data 375 organized as a header data table 375 A and an item data table 375 B. The business data 370 also includes purchase order data 380 (organized as a header data table 380 A and an item data table 380 B) and delivery order data 385 (organized as a header data table 385 A and an item data table 385 B). The business data 370 also includes analytical data 390 generated by various analytical processes and organized as sales location data tables 390 A and product data tables 390 B.
[0030] In this simplified example, a user may be able to more easily comprehend the complex business data 370 when presented through navigation displays based on a generally well-known model (as compared with comprehension through application-based displays). More particularly, the user is able to display inventory information related to the particular product by inventory location (by activating control 330 A) and by purchase order (by activating control 330 B). The user is able to display sales information related to the particular product by product family (by activating control 340 A), by sales region (by activating control 340 B), or by sales representative (by activating control 340 C). The user is able to display financial information related to the particular product by profitability factors (by activating control 350 A), by product family (by activating control 350 B) and by division (by activating control 350 C).
[0031] In sum, the controls 330 , 340 and 350 , in this example, enable the user to view information related to the particular product based on a generally known model. The display 310 helps to orient the user quickly to information that may be displayed and provides the user with quick access to critical data. In contrast to using application-based displays, the user of display 310 may be able to retrieve data without navigating through multiple displays to locate data important to the user.
[0032] FIG. 4 depicts an example process 400 for providing a user interface having a navigation pattern based on a generally known model. The example process 400 may be implemented in computer-readable medium that is executed by, for example, a processor (or processors) of the server 40 described previously with respect to FIG. 1 .
[0033] The process 400 begins when the system implementing the process 400 receives a user-input indication of a product for which the navigation pattern is to be generated (step 410 ). This may be accomplished, for example, by a user entering a product identifier (such as a product identification number, a product name or a product description) to a computer system, or selecting a product identifier from a list of product identifiers.
[0034] The system performing the process 400 generates and displays, on a computer display device, a navigation-oriented user interface that is based on a generally known model (step 420 ). The displayed model includes model components operable to, when activated by user-input, display product information for the indicated product based on the model component. The system receives a user-input indication of a displayed model component (step 430 ). For example, a user may use a pointing-device to activate a control corresponding to a model component. The system determines product information corresponding to the indicated model component (step 440 ). This may be accomplished, for example, by accessing information that identifies data elements of a product that relate to the indicated model component. The system displays product information based on the model component (step 450 ). For example, the system generates and displays a user interface including the data elements identified in step 440 .
[0035] FIGS. 5-7 present a series of user interfaces 500 - 700 illustrating a navigation pattern based on the value chain model developed by Michael Porter. FIG. 5 represents a user interface 500 having a model panel 510 and a basic data panel 520 . The model panel 510 displays the value chain model components: purchasing 510 A, inventory management 510 B, planning 510 C, production 510 D, sales 510 E and financial 510 F. The model panel 510 also includes a basic data control 512 . As illustrated, the basic data control 512 is selected, and basic data for a particular product is displayed in the basic data panel 520 .
[0036] In the example user interface 500 , the model components 510 A- 510 F are not operable to display product information until a particular product is selected. Once a particular product is identified, the model components 510 A- 510 F for which data is available are operable to display product information that is relevant to the selected model component.
[0037] Referring to FIG. 6 , the user interface 600 illustrates model components 510 B- 510 F as being activated or available—that is, operable to display relevant product information for a selected model component. By contrast, the user interface 600 shows purchasing model component 510 A as being inactive or unavailable for use to display product information. The visual clue of whether information is available for each model component may be helpful to orient a user and help a user retrieve desired information about a product.
[0038] Each model component 510 A- 510 F includes a show control represented by a plus sign (such as shown control 612 for the financial model component 510 F). When activated, the show control displays additional controls to display product information related to the model component to which the show control applies.
[0039] As illustrated in FIG. 7 , the show control of the sales model component 510 E and the show control of the financial model component 510 F have been activated. As a result, additional controls 710 are presented that, when activated, display product information related to the sales model component 510 E—namely, “Sales Prices,” “Sales Texts,” “Foreign Trade Export,” “Picking and Delivery,” and “Taxes.” Similarly, the show control of the financial model component 510 F results in an additional control “Valuation Prices.” Once a show control is activated, a hide control represented by a minus sign is presented in place of the show control. For example, the hide control 712 is presented for the financial model component 510 F. The activation of one of the additional controls causes the display of appropriate information in detail display 520 . For example, when the “Sales Prices” control is selected, sale price information related to the producer is displayed in detail display 720 . When the “Valuation Price” control is selected, valuation price information related to the product is displayed in detail display 520 .
[0040] As illustrated in user interfaces 500 , 600 and 700 of FIGS. 5-7 , the model 510 is displayed in each display, and, as such, is visible to orient the user and provide the ability to navigate to another model component from any display. Also, as illustrated by user interface 700 , the activated model component for which data is displayed in detail panel 720 is highlighted (as shown by sales model component 510 E in FIG. 7 ). This also helps to orient the user displaying the model-based navigation pattern user interface.
[0041] A user interface based on a generally known model facilitates a user's comprehension of product data available in a computer system. The model-based navigation pattern may be familiar to a user apart from experience with the computer application from which the user is interacting, and thus, the model-based navigation pattern may be said to support the mental model of the user. In this example, Michael Porter's value chain model is used to enable a user to understand data available related to a particular product and to display the available data. In some implementations, a navigation pattern user interface may be used to review, enter and edit product data.
[0042] Although the techniques have been described with respect to displaying information related to a product, the techniques are applicable to displaying information to a service.
[0043] The techniques can be implemented in digital electronic circuitry, or in computer hardware, firmware, software, or in combinations of them. The invention can be implemented as a computer program product, i.e., a computer program tangibly embodied in an information carrier, e.g., in a machine-readable storage device, in machine-readable storage medium, in a computer-readable storage device, in computer-readable storage medium, or in a propagated signal, for execution by, or to control the operation of, data processing apparatus, e.g., a programmable processor, a computer, or multiple computers. A computer program can be written in any form of programming language, including compiled or interpreted languages, and it can be deployed in any form, including as a stand-alone program or as a module, component, subroutine, or other unit suitable for use in a computing environment. A computer program can be deployed to be executed on one computer or on multiple computers at one site or distributed across multiple sites and interconnected by a communication network.
[0044] Method steps of the techniques can be performed by one or more programmable processors executing a computer program to perform functions of the invention by operating on input data and generating output. Method steps can also be performed by, and apparatus of the invention can be implemented as, special purpose logic circuitry, e.g., a FPGA (field programmable gate array) or an ASIC (application-specific integrated circuit).
[0045] Processors suitable for the execution of a computer program include, by way of example, both general and special purpose microprocessors, and any one or more processors of any kind of digital computer. Generally, a processor will receive instructions and data from a read-only memory or a random access memory or both. The essential elements of a computer are a processor for executing instructions and one or more memory devices for storing instructions and data. Generally, a computer will also include, or be operatively coupled to receive data from or transfer data to, or both, one or more mass storage devices for storing data, such as, magnetic, magneto-optical disks, or optical disks. Information carriers suitable for embodying computer program instructions and data include all forms of non-volatile memory, including by way of example semiconductor memory devices, such as, EPROM, EEPROM, and flash memory devices, magnetic disks, such as, internal hard disks or removable disks; magneto-optical disks; and CD-ROM and DVD-ROM disks. The processor and the memory can be supplemented by, or incorporated in special purpose logic circuitry.
[0046] To provide for interaction with a user, the techniques 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 of 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.
[0047] A number of implementations of the techniques have been described. Nevertheless, it will be understood that various modifications may be made without departing from the spirit and scope of the claims. For example, useful results still could be achieved if steps of the disclosed techniques were performed in a different order and/or if components in the disclosed systems were combined in a different manner and/or replaced or supplemented by other components. Accordingly, other implementations are within the scope of the following claims.
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Techniques for displaying a user interface on a computer display device are described. The techniques include displaying, on a computer display device, a model panel in a computer user interface where the model panel corresponds to one of an academic model or an industry model. The displayed model panel includes model components. User input that requests access to information related to one of the model components is received. Information related to the one of the model components in a second panel in the computer user interface is played on the computer display device. The second panel and the model panel are able to be viewed concurrently in the computer user interface.
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BACKGROUND OF THE INVENTION
The present invention relates to an improved rack for storing elongated rod-like members or the like.
By way of background, it is extremely difficult to load and unload rod-like members into existing storage racks. In one respect, there is no known structure to assist guiding or camming rods or bundles of rods into openings in the rack. Therefore, oftentimes the bundles will get "hung up" on the structural portions of the rack. In addition, there is no known structure on existing racks for locking a bundle of rods in position in the event that it tilts due to there being a greater portion of the bundle outside of the rack than within the rack. This factor complicates the loading of racks because external provisions must be made for holding the outer ends of the rod bundle in an elevated position throughout the loading process. It is with overcoming the foregoing deficiencies of prior rod storage racks that the present invention is concerned.
SUMMARY OF THE INVENTION
It is one object of the present invention to provide an improved rack for storage of rod-like members which will hold the bundle in a tilted position in the rack in the event that the center of gravity of the bundle lies outside of the rack, thereby obviating the necessity to use more than one external supporting member, such as a sling, during loading of the rack.
Another object of the present invention is to provide an improved rack for storage of rod-like members which contains rollers for permitting easy movement of rods or a rod bundle into and out of the rack when they are in a horizontal position, but which contains structure which automatically bites into the rods or rod bundles in the event they tilt when the center of gravity is outside of the rack.
Another object of the present invention is to provide an improved rack for storage of rod-like members which includes camming surfaces on the structural portions of the rack which guide the rod-like members into openings within the rack. Other objects and attendant advantages of the present invention will readily be perceived hereafter.
The present invention relates to a rack for elongated rod-like members comprising a base, a plurality of frames mounted in aligned spaced relationship on said base, each of said frames comprising a plurality of vertical horizontally spaced columns, a plurality of horizontal vertically spaced beam-like members affixed to the columns of each of said frames to define openings in each of said frames with corresponding openings of all of said frames being in alignment, upper and lower edges on said beam-like members for selectively biting into said rod-like members, whereby said rod-like members will be bitingly engaged by the upper edge of one of said beam-like members of a frame at the end of said rack and the lower edge of another beam-like member at a higher elevation than the upper edge of said one of said beam-like members when the ends of said rod-like members outside of said rack tilt downwardly. In addition, rollers are provided behind the upper edges of the beam-like members to support the rod-like members to support the rod-like memebers in a horizontal attitude. The beam-like members are preferably angles, the upper legs of which are inclined toward their associated openings so as to provide a camming action for guiding said rod-like members into said openings. The various aspects of the present invention will be more readily understood when the following portions of the specification are read in conjunction with the accompanying drawings wherein:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a side elevational view of the improved rod storage rack of the present invention showing how bundles of rods are loaded into the rack;
FIG. 2 is an end elevational view taken substantially in the direction of arrows 2--2 of FIG. 1 and showing the frame at the end of the rack at which rods are loaded into the rack;
FIG. 3 is a fragmentary cross sectional view taken substantially along line 3--3 of FIG. 2 and showing columns of each of the frames, with the beam-like angles attached thereto and the rollers mounted thereon;
FIG. 4 is a fragmentary cross sectional view taken substantially along line 4--4 of FIG. 3 and showing in plan the rollers mounted between the columns;
FIG. 5 is an enlarged fragmentary cross sectional view of the lower portions of the columns and related structure;
FIG. 6 is a cross sectional view taken substantially along line 6--6 of FIG. 5 and showing details of the roller construction;
FIG. 7 is a fragmentary enlarged view, partially in cross section, showing the positions taken by a rod-like member when it is supported by the roller and when it is gripped by the upper edge of the beam-like member; and
FIG. 8 is a cross sectional view showing the manner in which a rod-like member is gripped by the lower edge of the beam-like member.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The improved rack 10 of the present invention essentially consists of a base 11, a plurality of frames 12 mounted on said base, and associated structure for supporting the frame 12 in spaced substantially parallel relationship. The base 11 includes a plurality of I-beams 13 which rest on floor 14' and which support each of frames 12. Each frame 12 includes a plurality of substantially vertical spaced substantially parallel column-like members in the nature of channels 14 having their lower ends affixed, as by welding, to the upper flanges 15 of I-beams 13. A plurality of substantially horizontal beam-like members in the nature of angles 16 have portions of their outer edges 17 and 19 (FIG. 7) of their legs 20 and 21, respectively, welded to the edges of channels 14 as shown. Thus, the channels 14 of each frame are joined to each other at their bottoms by I-beams 13 and along their sides by angles 16. An I-beam 22 is also welded across the tops of the channels 14 of each frame 12.
At the upper portion of the rack (FIG. 2), angles 23 and 24 have their horizontal legs 25 and 26, respectively, welded to the lower flanges 27 of I-beams 22 and their vertical legs 29 and 30, respectively, bolted to the webs of channels 14. In this respect, by way of example, leg 30 is bolted to channels 14 at 31' and leg 29 is bolted to its associated channels 14 in a like manner. At the lower portion of the rack, angles 31 and 32, which are essentially a part of base 11, are located at the junctures of the outermost channels 14 of each frame and their associated I-beams 13. By way of example, the vertical leg 32' of angle 31 is affixed to channels 14 by bolts at 33. The vertical leg 34 of angle 32 is affixed to channels 14 in a like manner. The horizontal legs 35 and 36' of angles 31 and 32, respectively, are cut away to receive the outermost channels 14 of each frame. Elongated cross plates 36 in the nature of elongated links are secured by bolts as shown in the positions of FIG. 1 on both sides of the rack. Bolts 37 are used for the attachment to the vertical legs of the angles 23, 24, 31 and 32. More specifically, certain sets of links 36 extend between vertical legs 30 and 34 on one side of the rack and other sets of links 36 extend between vertical legs 29 and 32' on the other side of the rack. The centers of each pair of links 36 are bolted to each other at 37'. The foregoing structure provides an extremely solid rack for storing a plurality of different sized rod-like members in openings 39 defined by the intersection of columns 14 and beam-like members 16.
A roller 40 is mounted for rotation behind the upper edge 17 of each beam-like member 16 in each opening 39, and the upper portion of roller 40 extends slightly above upper edge 17 (FIG. 8), the exact distance in this particular instance being about 1/8 of an inch. The aligned rollers 40 at each level of each frame 12 are supported in the following manner. A hexagonal rod 41 extends through aligned openings in the web of each channel 14. Hexagonal rod 41 is also press-fitted through the inner race 42 of bearings 43, with the outer race 44 being press-fitted into the outer portion of roller 40. Bearings 45 are located between the inner and outer races. Thus, the inner race will not be able to rotate relative to rod 41 and the outer races 43 will not be able to rotate relative to the outer portions of roller 40, so that rotation will be confined between the inner and outer races.
A plurality of rollers 46 are located at the lower ends of each frame 12. The rod 41' (FIG. 5), which is analogous to rod 41, is spacedly supported on plates 47 having their edges 49 (FIG. 5) welded in alignment with the webs of channels 14. Openings in plates 47 receive rod 41'. The ends of rods 41 and 41' are secured in position by nuts 42' and 42", respectively. The rollers 46 are mounted on rods 41' in a manner analogous to that described above relative to FIG. 6. The rack of FIG. 1 is approximately 33 feet long, 7 feet high and about 7 feet wide. These measurements are strictly by way of example and not by limitation.
In order to load a bundle of rods 50 (FIG. 1), the length of which may be greater or lesser than 33 feet, into rack 10, a sling 51, which is attached to an overhead lifting device, is used. Initially, the sling 51, as shown in in solid lines, is attached to bundle 50 to lift it from the floor and align it with any one of the openings 39. Thereafter, the sling 51 is moved in the direction of arrow 52 to cause the bundle 50 to enter the aligned openings 39 of the various frames until such time as sling 51 reaches the dotted line position. The sling 51 is then lowered until the lower edge of bundle 50 rests on the upper surfaces of rollers 40. This is depicted by solid lines in FIG. 7. Continued lowering of sling 51 will cause the bundle 50 to tilt to the dotted line positions shown in FIGS. 1 and 7 so that the lower surface of bundle 50 will contact the relatively narrow upper edge 17 of angle 16 at the entry frame and the upper surface 53 (FIG. 8) will engage the relatively narrow lower edge 19 of an angle 16 on one of the inner frames 12. Thus, edge 19 will bite into the upper surface 53 of bundle 50 and edge 17 will bite into the lower surface of bundle 50. This biting action will be sufficient to hold the bundle in the tilted dotted line position as depicted by dotted line numeral 50 in FIG. 1. Continued lowering of sling 51 will cause the sling to lose contact with bundle 50 in its dotted line position and thereafter sling 51 can be moved to the position 51' in FIG. 1 to raise the end of bundle 50 to a substantially horizontal position and thereafter when sling 51' is moved to the left, the rod bundle will roll on rollers 40 and will be moved all the way into rack 10 so that it will occupy the dotted line position 50" in the rack. If individual rods of bundle 50 are thereafter to be removed from the rack, this can be done manually. If the entire bundle is to be removed, it is to be noted that it can be moved out manually because the bundle rests on rollers 40 and the bundle can be rolled until a sufficient portion of the bundle extends outside of the rack so that the sling 51 can thereafter be used.
At this point it is to be noted that the upper leg 20 of each angle 16 is inclined in an upward direction toward its associated opening 39. Thus, the upper surface of each leg 20 acts to cam the bundle or a rod into the opening directly above it. At this time it is to be noted that a plate 53' is welded across the ends of each angle 16 at the entry frame 12 of the rack to reinforce it because it is this end frame which takes the greatest amount of shock when a bundle of rods is being loaded into the frame. The remainder of the frames 12 do not have reinforcing plates 53'. In addition, angle members 54 are welded to the legs of each channel 14 on each frame 12 of the rack to provide camming action for guiding the bundles of rods into the openings 39 toward which the inclined legs 55 and 56 are directed.
An inclined plate 57 is welded to the flange of I-beam 13 at the entry end of the rack to provide an inclined surface analogous to inclined surfaces 20 for guiding a bundle into an opening 39 immediately above plate 57.
A pair of tubular members 59 (FIG. 2) is mounted on each side of each frame 12. Each member 59 can receive a vertical rod to thereby provide a plurality of upstanding rods on each side of the frame, between which additional elongated rod-like members can be stored.
It can thus be seen that the improved rod storage rack of the present invention is manifestly capable of achieving the above enumerated objects, and while preferred embodiments of the improved rack have been disclosed, it will be appreciated that the present invention is not limited thereto but may be otherwise embodied within the scope of the following claims.
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A rack for elongated rod-like members including a plurality of spaced substantially parallel frames mounted on a base, with each frame consisting of columns and beams for providing a plurality of openings, spaced rollers extending between columns of each frame behind said beams for supporting the rod-like members, with the beams having inclined surfaces for guiding the rod-like members into associated openings, and the beams having upper and lower edge portions so that if a bundle of rod-like members tilts during loading, the upper edge of the beam on the frame at the entry portion will bite into the underside of the bundle and the lower edge of another beam at a higher elevation within the rack will bite into the upper side of the bundle to hold the bundle in position.
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FIELD OF THE INVENTION
[0001] The present invention relates to tools for exploring possibilities and more particularly to tools used for exploring and evaluating the likelihood and significance of possible events.
BACKGROUND OF THE INVENTION
[0002] People have long predicted the future. For instance, if a spouse presents flowers to their partner, they can predict that the reaction will be favorable. It is possible that the partner could not react or react negatively. Other implications are also possible. People are comfortable with predicting based upon the occurrence of an event. If “X” occurs then “Y” may be the result. From this very simplified methodology there is a very substantial room for improvement.
[0003] A tool has been developed and sold under the trademark IMPLICATIONS WHEEL® developed and sold by the current inventor, Joel A. Barker. This tool essentially follows the format of If “X” occurs then “Y” may result. The tool, identifies many of the different implications that may flow from “X.” Then additional layers may be followed out, separately treating each “Y” portion of the equation as a new “X” and looking for the next round of implications. The process may be repeated as many times as desired to reach out as far into the future as desired.
[0004] This tool has been important within corporate America due to the commercial advantage of being extremely well positioned for the future. For instance, a company may wish to understand what could result from buying out another company. Some of the immediate implications may include anti-trust problems, strategic partner benefits, combining of research and development departments and other potentially readily discernable implications. Less discernable implications are more readily uncovered with the aid of the IMPLICATIONS WHEEL® brand exploring tool. Subsequent layers of implications may also be uncovered or revealed by the tool. For instance, innovative new product may result from cross-fertilization of ideas in a combined research and development department.
[0005] The IMPLICATIONS WHEEL® brand method of predicting the future has some drawbacks until now. Previously, the tool used paper to record all the implications. The pieces of paper could become very large, covering more than an entire wall of a room. When an author desired to have arc completion groups complete the arcs, the wheel would be rolled up and mailed from location to location. There the user could engage in activities that are hurtful of the process, including editing the first order nodes, mistakes that if corrected would leave a mess on the otherwise crowded chart, chaining, e.g. completing third, fourth and higher order nodes before completing the second order nodes, failing to include both positive and negative nodes and other such problems. Charts were easily damaged and destroyed in this uncontrolled system. Arc completion groups would not always follow directions, scoring nodes when only completion was desired. This regularly resulted in complete re-writing of the work product, costing both time and money.
[0006] What is needed is an improved tool for predicting events, normally in the future, but potentially in the past. The tool should have controls to prevent errors and problems that result from failing to follow directions. For instance, the first order nodes should be protected from change. All second order nodes should be completed before third order nodes are made available for completion. Delivery should be performed electronically with confirmation. Editing and scoring of nodes should be performed with complete removal of any prior markings, avoiding the messes that otherwise clutter the work. Scoring should be allowed only when assigned and then may be required once assigned. Other features for the ease of use and comprehension should also be included to enhance the usability and understandability of the tool.
SUMMARY OF THE INVENTION
[0007] An investigative method, which may generally be provided with the steps of determining whether the stored subscription is valid on the local computer; if the subscription is valid presenting options of downloading assigned arcs, selecting to update the subscription to the status stored on the server side, and selecting a center; if the subscription is expired presenting options of selecting to update the subscription to the status stored on the server side, and selecting a center and precluding downloading of assigned arcs; and If the subscription is not logged in, presenting the option of selecting to update the subscription to the status stored on the server side until receipt of a communication of a valid subscription from the server side and precluding downloading of assigned arcs and selection of a center.
[0008] The user may select a center and assigned arcs from the selected center are then displayed.
[0009] The method may determining if the arc was assigned for completion. Then determine whether second order implication stage is complete, assuming the arc was assigned for completion. The entire arc is displayed only when the second order implication stage is complete.
[0010] The method may determine if the arc was assigned for completion and if so directing the user to a completion interface.
[0011] The method may determine whether time was assigned. If time was assigned, options may be presented at the completion interface of open another arc, complete second order nodes, complete third order nodes, scoring from one assigned point of view, timing from one assigned point of view, spell check, return completed arc, and quit. If time was not assigned, options may be presented of open another arc, complete second order nodes, complete third order nodes, scoring from one assigned point of view, spell check, return completed arc, and quit, while precluding an option of timing from one assigned point of view.
[0012] The user may select an option of completing third order nodes. The method determines whether there is at least one positive and at least one negative second order implication. Presentation of third order nodes is precluded unless at least one positive and at least one negative second order implications are present. That is, third order nodes are presented only when there is at least one positive and at least one negative second order implication.
[0013] When the user selects to complete second order nodes or complete third order nodes, a delay may occur for a period of time to allow a user to think about implications. A clock may govern the delay. A second clock may be maintained to measure a period of time delay between user input. The user is reminded to provide input if a predetermined amount of time has passed from the second clock.
[0014] The method may determine if scoring was assigned. Scoring may be permitted only when scoring is assigned. Editability of implication text may be disabled if scoring was assigned. The user is directed to a scoring interface.
[0015] When scoring, the method may display desirability buttons and likelihood buttons with or without a minority report button. A minority report interface is displayed when the user clicks the minority report button. The method verifies that the minority report interface is fully prepared prior to accepting any data contained in the report and precludes acceptance of an incomplete minority report.
[0016] At the scoring interface, the method :may determine whether time was assigned. Options are displayed of open another arc, quit, score from all assigned points of view and return completed arc. An option of time is precluded from all assigned points of view if time was not assigned. If time was assigned, options of open another arc, quit, score from all assigned points of view, time from any assigned points of view, and return completed arc are displayed.
[0017] Several advantages are provided from these methods, including allowing users to complete the work which was initiated during the subscription period and yet preclude perpetuation of the options available to valid accounts when the subscription expires.
[0018] As yet another advantage, the user can select a center for completion or scoring without allowing their own personal bias toward the particular arcs they have been assigned to steer them toward or away from working on a particular center.
[0019] As still yet another advantage, the user is required to determine implications based upon a parent node before the user can begin identifying higher order implications, since the entire arc is displayed only when the second order implication stage is complete.
[0020] Yet another advantage is that users who have been assigned to complete an arc are directed to a completion interface, revealing only those completion options available within the scope of their assignment.
[0021] As an example of the preceding advantage, a user that was assigned time may be presented options at the completion interface of open another arc, complete second order nodes, complete third order nodes, scoring from one assigned point of view, timing from one assigned point of view, spell check, return completed arc, and quit.
[0022] As still another advantage, if time was not assigned the user is presented with options of open another arc, complete second order nodes, complete third order nodes, scoring from one assigned point of view, spell check, return completed arc, and quit and precluded from an option of timing from one assigned point of view.
[0023] As an additional advantage, linear chaining of implications and rushing through thought is avoided, since presentation of third order nodes is precluded unless at least one positive and at least one negative second order implications are present. That is, third order nodes are presented only when there is at least one positive and at least one negative second order implication.
[0024] As still another advantage, progress is encouraged by maintaining a clock for a period of time measuring delay between user input and reminding the user to provide input if a predetermined amount of time has passed from the last receipt of input.
[0025] As yet another advantageous control scoring of an arc may be permitted only when scoring is assigned.
[0026] Another control advantage is that editability of implication text is disabled if scoring was assigned.
[0027] As still another advantage a user is directed to a scoring interface if scoring was assigned, permitting only options available to those who have been assigned scoring.
[0028] Yet another advantage is that desirability buttons and likelihood buttons are displayed when scoring.
[0029] A further advantageous feature is that a minority report button is displayed when scoring.
[0030] Still yet another advantage is that a minority report interface is displayed when the minority report button is clicked.
[0031] Another control advantage is that the minority report interface is required to be fully prepared prior to accepting any data contained in the report and precludes acceptance of an incomplete minority report.
[0032] As another control feature that is advantageous is that options are displayed for open another arc, quit, score from all assigned points of view and return completed arc and the user is precluded from the option of time from assigned all point of view if time was not assigned. Yet, when time is assigned that user is displayed the options of open another arc, quit, score from all assigned points of view, time from all assigned points of view, and return completed arc.
[0033] These and other advantages are further explained in the description, shown in the drawings and illustrate in the appendix.
DESCRIPTION OF THE DRAWINGS
[0034] FIG. 1 is a flowchart showing a preferred logic for launch and registration;
[0035] FIG. 2 is a flowchart for opening a file and showing the initial screens;
[0036] FIG. 3 is a flowchart showing the completion interface;
[0037] FIG. 4 is a flowchart showing editing of nodes;
[0038] FIG. 5 is a flowchart showing the process for adding currently unidentified implications;
[0039] FIG. 6 is a flowchart showing scoring in completion mode;
[0040] FIG. 7 is a flowchart showing timing;
[0041] FIG. 8 is a flowchart showing spell check;
[0042] FIG. 9 is a flowchart showing scoring interface;
[0043] FIG. 10 is a flowchart showing scoring in timing mode;
[0044] FIG. 11 is a flowchart showing timing;
[0045] FIG. 12 is a screen shot showing an introductory screen, listing the assigned arcs when the subscription is not current;
[0046] FIG. 13 is a screen shot showing an introductory screen, listing the assigned arcs when the subscription is current;
[0047] FIG. 14 is a screen shot that may appear to acquire subscription log-in data;
[0048] FIG. 15 is a screen shot that may appear to acquire subscription log-in data;
[0049] FIG. 16 is a screen shot that may appear to acquire subscription log-in data;
[0050] FIG. 17 is a screen shot that may appear to acquire subscription log-in data;
[0051] FIG. 18 is a screen shot showing an introductory screen, listing the assigned arcs when the subscription is current;
[0052] FIG. 19 is a screen shot showing the center and background with first order implication;
[0053] FIG. 20 is a screen shot providing for entry of the second order implications;
[0054] FIG. 21 is a screen shot showing the full arc and entry of a third order implication;
[0055] FIG. 22 is a screen shot showing the center, background and points of view assigned;
[0056] FIG. 23 is a screen shot showing the full arc in detailed scoring mode;
[0057] FIG. 24 is a screen shot showing the full arc in fast scoring mode;
[0058] FIG. 25 is a screen shot showing an interface window;
[0059] FIG. 26 is a screen shot showing an interface window;
[0060] FIG. 27 is a screen shot an interface window;
[0061] FIG. 28 is a screen shot showing a reminder window;
[0062] FIG. 29 is a screen shot showing the full arc in timing mode;
[0063] FIG. 30 is a screen shot showing the first and second order implications with a second order implication being entered;
[0064] FIG. 31 is a screen shot showing two timers and a rule reminder;
[0065] FIG. 32 is a screen shot showing a progress reminder;
[0066] FIG. 33 is a screen shot showing a reminder to include both positive and negative implications;
[0067] FIG. 34 is the screen shot showing first and second order implications;
[0068] FIG. 35 is a screen shot showing the minority report interface;
[0069] FIG. 36 is a screen shot showing a reminder to complete the minority report interface;
[0070] FIG. 37 is a screen shot showing the full arc in timing mode;
[0071] FIG. 38 is a screen shot showing the full arc in spell check mode;
[0072] FIG. 39 is a screen shot showing a portion of the scoring interface; and
[0073] FIG. 40 is a screen shot showing a portion of the scoring interface.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
[0000] Definitions
[0074] An applicant is entitled to be his own lexicographer. Accordingly, applicant chooses the following definitions to apply to the description, claims and abstract, except as may otherwise be augmented in the detailed description:
Ancestor—An ancestor of a first or subsequent order implication or node is the center and any implication/node between the center and the reference implication/node. Arc—An arc is a portion of a wheel, the data from which can be combined with existing data into a wheel. An arc is made up of one first order implication followed by up to preferably 10 second order implications followed by up to preferably ten third order implications off of each second order implications. In a sense it is a fractal of the complete wheel, but its presented shape may be a wedge instead of a wheel. An example of an arc is shown in FIG. 34 . Center—The main or principle issue being explored with a wheel. Possible category centers include: an innovation, an emerging trend, a new policy, a new product brought out by a competitor; or a significant event, i.e. 9 / 11 . Center node—The node in a wheel that represents the center of the wheel and the starting point of the discussion. Child (Children)—Any implication that has the reference implication as its parent is a child of the reference implication. Any implication that has the center as its parent is a child of the center. Completion mode—A mode of operating the program where new implications may be added, existing implications, except for the first order implications may edited and scoring and timing may be permitted. Diminished node—A condensed node, opposite of enlarged node. Descendent—Any implication that has the reference implication as its ancestor is a descendent of the reference implication. Any first or subsequent order implication is a descendent of the center. First (and subsequent) order implication—A direct possible implication of the center. A second order implication is an immediate possible implication resulting from the occurrence of a first order implication. Subsequent levels of implications, third order, fourth order, etc., are direct possible implications resulting from the occurrence of the immediate preceding order of implication. I.e. parent implication. First (and subsequent) order node—The graphic form that holds the text of a first order implication. Second order, third order, fourth order, etc. nodes correspond to similarly numbered implications. Implication—A possible result or consequence that is triggered by a previous event. Implications Wheel® —A brand of a team tool that help users discover possible future events in an orderly yet divergent pattern. An Implications Wheel® brand wheel is built using a disciplined methodology and a non-linear thinking process. Preferably, a wheel is displayed as a grouping of all desired orders of all identified possible implications flowing out of a single event. Lead—A portion of a line extending partially between two nodes. A lead is displayed when one of the two nodes is not displayed. A lead is shown as part 572 in FIG. 24 , e.g. four lines to a fourth order node with part of the line and the fourth order node not showing. Lines—A connector between two nodes. A line may be paired with one or more lines as described below. Magnified Node—An enlarged node, opposite of diminished node. Minority opinion—A scoring opinion or a potion of a group that constitutes less than a majority. Minority report—The scoring result as prepared by those holding a minority opinion. N (Nth)—A mathematical variable. Node—An area in which data concerning an implication may be recorded or displayed. Preferably, a node is displayed in the shape of a circle or oval, with certain very special nodes displayed in the shape of a star or other non-circular shape. A node may be displayed as diminished, normal or enlarged. Order—The number of ancestors of the reference implication. Parent—The parent of some implication is the immediate ancestor of the reference implication. That is, the ancestor that is connected to the reference implication without intervening implications. Point of View—The perspective used for scoring of a node, arc, or wheel done by one entity, person or group. Any wheel can be scored from multiple points of view, e.g., legal, engineering, marketing, staff, natural and/or other. Reference implication—The implication being discussed or chosen. Syn. Selected implication. Scoring mode—The mode of operating the program where implications may not be added or edited, but may be scored and timed. Sibling implications—Children of the same parent implication. Significant node—A node that is scored a +4 or greater score or −4 or lesser score. Strand—The chain of implications II being ancestors of the same implication, including that reference implication and reaching all the way back to include the center. Time Diamond—An area in which judgements concerning the amount of time between implications is indicated. Timing mode—A mode of operating the program where time diamonds may be entered or edited. Timing is a subset of completion mode or scoring mode. Wheel—A graphical representation of all identified implications that may directly or indirectly flow from a given center. Implications Wheel® is the preferred brand of a wheel. An example of a wheel is shown in FIG. 41 .
Launch and Registration
[0104] FIGS. 1-11 are flowcharts demonstrating a preferred methodology for making and using the present invention, arc completion and scoring. Referring to FIG. 1 , ovals, such as oval 100 , demonstrate a terminal point in the method. Oval 100 indicates the starting point for the future exploration method, which may be initiated in any manner known in the art, including those manners known in the art of computer software. This flow chart discussed in reference to FIG. 1 may connect into other parts of the overall process with the user entering through pentagon 101 . (A pentagon, such as pentagon 101 , indicates a point of connection to other parts of the flowchart having the same letter disposed within the pentagon. An upright pentagon, such as pentagon 101 indicates a point of entry and an inverted pentagon, such as pentagon 136 indicates a point of departure.)
[0105] Diamonds, such as diamond 102 , indicate a methodology decision making point. Diamond 102 determines whether the subscription for the use of the methodology is current. Remuneration models other than subscription may be used, however, the present inventor opines that subscriptions are the best manner of offering the present invention for use. The determination at diamond 102 checks the local computer to see if the subscription is current and valid. Three possible outcomes to this decision are “valid,” “expired,” and “never logged in.” “Never logged in” occurs the first time an instance of the program is executed on a given local computer and thereafter until a valid subscription is confirmed with the server.
[0106] Expired—If the subscription has expired the next step is indicated by oval-arrow 104 . Oval-arrows, such as oval-arrow 104 , indicate a display of particular information to the user. In the case of oval-arrow 104 each center 500 of each previously downloaded arc that has not been sent back to the data server is displayed in field 502 , perhaps as shown in FIG. 12 . Buttons 504 , 506 and 508 may present options available to the user as will be described shortly. At oval-arrow 106 , the user is notified that only active subscriptions can download arcs, perhaps as shown on line 510 of FIG. 12 , and the method hides the download button 512 as may be seen by comparing FIG. 12 and 13 . The encircled number touching on oval-arrow 106 encases indicia with such indicia being a referenced figure number of the drawings. (Similar circles throughout this application having different indicia refer to different figures with a corresponding number to that shown in the circle.) The user may selecting to update the subscription, button 506 of FIG. 12 and 13 and parallelogram 108 of FIG. 1 , which directs the user to the step indicated in parallelogram 110 , which will be described in a moment. A parallelogram, such as parallelogram 110 , is a point in the method seeking user input.
[0107] Parallelogram 110 is reachable from a different set of steps. For instance, if the locally stored subscription is “valid”, see diamond 102 , the center is displayed of each previously downloaded arc that has not yet been sent back to the data server, oval-arrow 114 , as shown in field 502 of FIG. 13 . At this point the user may also select to update the subscription, parallelogram 108 of FIG. 1 , which leads the user to the step indicated in parallelogram 110 .
[0108] One or more prompts for subscription login data may be presented such as that shown in FIGS. 14 and 15 , parallelogram 110 of FIG. 1 . In the prompt shown in FIG. 14 , a user may record various identifying information, perhaps as suggested in field 514 (organization name), field 516 (Group/user name), field 518 (password), field 520 (new password if a change is desired) and/ or other identifiers. A description of the group may be written in field 522 of FIG. 15 . Selecting “cancel”, button 524 , from either prompt shown in FIGS. 14 or 15 directs the method back to the step indicated and previously discussed with regard to diamond 102 . Upon completion of the fields the user may select “o.k.”, button 526 directing the method to write the data to the preferences file, cylinder 112 . A cylinder in a flowchart, such as cylinder 112 , is a point in the method where data is either written to or read from storage.
[0109] The server side computer is checked based upon stored data, an asynchronous process, wherein three potential results may occur, expired, valid, or invalid, rectangle 114 . If the account is expired, the user may be notified and directed to previously described diamond 102 , allowing the user to engage in those activities permitted to expired accounts. If the submitted subscription data is valid, the user is directed to previously described diamond 102 , allowing the user to engaged in those activities permitted to valid accounts. If the submitted data is invalid, the method moves to the step indicated by parallelogram 118 , also reachable from diamond 102 with a “never logged in” result. A prompt similar to that described in regard to parallelogram 110 is presented, see FIGS. 16 and 17 . The user has the option to enter subscription data and moving to the sequence of steps starting with the step previously described in regard to cylinder 112 or quitting. Selection of quitting, causes the methodology to terminate, oval 120 .
[0110] If the subscription is valid, diamond 102 , two other option are available to the user following the previously described display, oval-arrow 115 . The user may download additional assigned arcs, parallelogram 122 . The system logs into the data server over a secure channel with the locally stored login information and a request is made for a list of assigned arcs, rectangle 124 . This may be an asynchronous process. The system then logs into the data server over a secure channel with locally stored login information and downloads each arc, confirming each download when complete, rectangle 126 . The also may be an asynchronous process. Upon completion of the download, the method is directed to the display step previously described in regard to oval-arrow 115 . The flowchart indicator 128 is a symbol showing that the option of downloading assigned arcs is not an option available to expired subscriptions.
[0111] Valid and expired subscriptions also have the option of selecting a center, parallelogram 130 . Any visible first order implications are hidden and then any assigned first order implications from the selected center are displayed in field 528 , oval-arrow 132 , as shown in FIG. 18 . The user may then select a first order implication, parallelogram 134 and, as indicated by pentagon 136 , the method is directed to the method steps for opening the file and showing the initial screens as set forth in FIG. 2 , pentagon 138 .
[0000] Opening Files and Showing Initial Screens
[0112] Referring now to FIG. 2 and entering through pentagon 138 the file associated with the selected arc is loaded into memory, cylinder 140 . A decision is made as to whether the file is encrypted, diamond 142 . Note, that files preferably are always encrypted prior to sending through the server, but after it is loaded into the memory, each subsequent save may not be encrypted. If encrypted, the data from the file is decrypted, rectangle 144 . The decrypted data, recently or previously, is used to generate a data structure based upon data read from the file, rectangle 146 . A decision is made as to whether the arc was assigned for completion or scoring, diamond 148 .
[0113] For those assigned for completion, a process step is performed. Particularly, the implication text edit-ability is enabled, rectangle 150 . The text in the first order node is not made editable at anytime during the process shown in FIGS. 1-11 . This is a control process as this method is generally used in conjunction with a wheel method, which allows the sending out of arc assignments. Those sending out the arc assignments are allowed to control the assignment as specified in the first order nodes, which are non-editable to those receiving the assignments. A decision is made as to whether any arc from the wheel associated with the selected arc been opened during the current program session, diamond 152 . If no, the center is displayed together with the background in field 530 and assigned first order implications may be shown in field 532 , oval-arrow 154 , as shown in FIG. 19 . This allows the user to fully understand the purpose and goals of the wheel, and hence the arc the user has selected. The method then waits for user interaction with the completion interface as set forth in FIG. 3 , rectangle 156 and pentagon 158 .
[0114] Another decision is made, diamond 160 , if an arc from the wheel associated with the selected arc has been opened during the current program session. See diamond 152 . In particular a decision is made as to whether the second order implication stage is complete, diamond 160 . If no, the second order completion stage is displayed, oval-arrow 162 and FIG. 20 . Note that the first order implication 534 and second order nodes 536 together with any second order implications are displayed. A portion of the center node 538 may also be shown. If yes, the complete arc is displayed in completion mode oval-arrow 164 and FIG. 21 . The center node 538 , first order node 534 , second order nodes 536 and third order nodes 540 may all be displayed. The method then waits for user interaction with the completion interface as set forth in FIG. 3 , rectangle 156 and pentagon 158 .
[0115] If the arc was assigned for scoring, diamond 148 , implication text edit-ability is disabled, rectangle 166 . A decision is made as to whether any arc from the wheel associated with the selected arc has been opened during the current program session, diamond 168 . If no, the center and background, shown in field 542 and assigned point(s) of view, shown in field 544 are displayed, oval-arrow 170 , perhaps as shown in FIG. 22 . (Note, the text in the figures is merely offered to aid in identification of the location and is not presented as an implication or description relative to a particular issue being examined with the methodology.) If yes, the complete arc is displayed in scoring mode with un-scored implications displayed with indicia marking the nodes as un-scored, perhaps blurry lines or other indicator, oval-arrow 172 . See FIGS. 23 and 24 . Following either the step described in regard to oval-arrow 170 or oval-arrow 172 , the method waits for user interaction with the scoring interface, rectangle 174 and pentagon 176 , as described with regard to FIG. 9 starting at pentagon 376 .
[0000] Completion Interface
[0116] The completion interface may be entered either at pentagon 178 from pentagon 158 of FIG. 2 or pentagon 180 from FIG. 4 (pentagon 263 ), 5 (pentagon 298 ), 6 (pentagon 320 ), or 7 (pentagon 350 ). Assuming the completion interface is entered from pentagon 178 , a decision, diamond 182 , is made as to whether time was assigned. If no, the interface is displayed with the options to open another arc 546 , quit or exit 548 , complete second order implications 550 , complete third order implications 552 , score from all assigned points of view 554 , spell check 556 , and return the completed arcs 558 , oval-arrow 184 . FIGS. 25 and 26 are examples of what the display may show. Note, that the user is precluded from having the option of entering time as such option is not presented whether user enters from pentagons 178 or later 180 as the methodology recalls the decision at diamond 182 . If time was assigned, the interface is displayed with the options to open another arc 546 , quit or exit 548 , complete second order implications 550 , complete third order implications 552 , score from all assigned points of view 554 , time from all assigned points of view 560 , spell check 556 , and return the completed arcs 558 , oval-arrow 186 . FIGS. 25 and 27 are examples of what the display may show.
[0117] Whether reaching the present point in the method from oval-arrow 184 , oval-arrow 186 or pentagon 180 , the user is presented with several options, except as otherwise noted. At parallelogram 188 , the user may select to open another arc wherein the method follows the step previously described starting with diamond 102 on FIG. 1 . See pentagons 190 FIG. 3 and pentagon 101 of FIG. 1 .
[0118] The user may select to complete second order implications, parallelogram 192 , whereupon the second order implications are displayed, oval-arrow 194 , as shown in FIG. 20 . A portion of the center 538 , the first order node 534 and second order nodes 536 are displayed. The user is then directed, pentagon 196 , to the node editing procedure shown starting at pentagon 236 of FIG. 4 .
[0119] The user may select to complete third order implications, parallelogram 198 , which invokes a decision as to whether there is at least one positive and one negative second order implication, diamond 200 . If no, the user is notified, perhaps in window 562 , that they must have at least one positive and one negative second order implication, oval-arrow 202 , and is directed to select another option. That is, the user cannot enter implications of a new order until there is at least one positive and one negative implication of the current order. If yes, the full arc is displayed in completion mode, oval-arrow 204 as shown in FIG. 21 and has been previously described. The user is directed via pentagon 196 to the method described in reference to pentagon 236 of FIG. 5 .
[0120] The user may select to score from one assigned point of view, parallelogram 208 . The full arc is then displayed in scoring mode with un-scored implications bearing indicia, perhaps blurry or jagged lines 564 defining the node, such indicia indicating the unscored nature of such node, oval-arrow 210 such as found in FIGS. 23 and 24 . Scored nodes that are not scored as being significant may have indicia such as solid lines 266 , indicating that the nodes have been scored. Nodes scored as significant may have indicia such as stars 268 disposed about the node. Nodes scored with a high likelihood may bear indicia such as a second circle 270 . Leads 272 may indicate the presence of non-displayed higher order implications. The user is then directed, pentagon 212 , to the steps concerning scoring in completion mode at pentagon 300 of FIG. 6 .
[0121] The user may select timing from an assigned point of view, parallelogram 214 . The full arc is displayed in timing mode, oval-arrow 216 , as shown in FIG. 29 . This option may not be made available if timing has not been assigned. The user is then directed, pentagon 218 , to the method step concerning timing, pentagon 334 of FIG. 7 .
[0122] The user may select spell check, parallelogram 220 . The full arc is displayed in completion mode and spell check is started, oval-arrow 222 as shown in FIG. 21 . The user is then directed, pentagon 224 , to the steps concerning spell checking as set forth at pentagon 352 of FIG. 8 .
[0123] The user may select to return a completed arc, parallelogram 226 . A process step, rectangle 228 , of logging in to the data server over a secure channel with locally stored login information. The arc data is encrypted and returned to the server. This may be an asynchronous process. The user is then directed, pentagon 230 , to the method steps following from pentagon 101 of FIG. 1 .
[0124] Alternatively, the user may select quit or exit, parallelogram 232 . The program then terminates, oval 234 .
[0125] Note, at various points in the display if any implication has more than a predetermined number of implications, perhaps five, a “next page” button 592 will be presented for any additional implications and if any implication has a multiple of the predetermined number, perhaps five, a “new page” button 592 will be displayed for allowing additional implications to be placed on a new page.
[0000] Editing Nodes
[0126] The user may reach the editing nodes function through pentagon 236 . Thereafter, the user may click a second or third order node 536 , 540 , parallelogram 240 . Completing third order nodes 540 is precluded if there are not at least one positive and one negative second order node 536 as previously described, diamond 200 of FIG. 3 . A decision is made as to whether the selected node corresponds to an implication that has already been generated, diamond 242 . If no, the user is directed, pentagon 244 , to pentagon 264 of FIG. 5 .
[0127] If the selected node corresponds to a previously generated implication, the text entry display 574 is presented over the selected node containing the implication text, oval-arrow 248 , as shown in FIG. 30 . The user may edit the text and submit the changes, perhaps with the << enter>> key, <<tab>> key or clicking on the screen in a location unrelated to the node, rectangle 250 . Positive and negative scoring may be changed on the implication, preferably by changing the plus or minus indicator near the beginning of the text display.
[0128] A decision is made, diamond 252 , as to whether there are four or more sibling nodes, e.g. children of the current parent node. If no, the method is directed to the step described in regard to the step set forth in rectangle 254 , which will be described in a moment. If yes, a decision is made as to whether there is at least one positive child of the current parent node, diamond 256 . If no, the user is reminded to include at least one positive implication, parallelogram 258 , and directed to the step indicated in rectangle 254 . If there is at least one positive child of the current parent node, a decision is made as to whether there is at least one negative child implication of the current parent implication, diamond 260 . If no, the user is reminded to include at least one negative implication, parallelogram 262 , and is directed to the step described in regard to rectangle 254 . If there are four or more children nodes of the current parent node and at least one is positive and one is negative, the user moves directly to the process step set forth in rectangle 254 .
[0129] At rectangle 254 , the text of the selected implication is changed in the data structure representing the arc. The arc is written to permanent storage, cylinder 261 . The user has the option of repeating the afore described steps in editing another implication or returning to pentagon 180 of the completion interface described with reference to FIG. 3 , pentagon 263 .
[0000] Currently Unidentified Implications
[0130] This process has been found to inspire users to be aggressive on sharing implications and less aggressive on forethought. Accordingly, the process may include a step to relax the user and allow them time to think. After reaching pentagon 244 of FIG. 4 , the user is directed to pentagon 264 of FIG. 5 . There a decision is made as to whether the user has had the thirty second timer displayed, diamond 266 . A pause window 576 , perhaps thirty-seconds in duration may be presented together with a display of rule reminders 578 , which can vary as to which rules are presented, and the text of the parent implication of the selected node, oval-arrow 268 . This pause may include a delay override button 580 and visible countdown indicator 582 , preferably analog clock style, oval-arrow 268 .
[0131] Once the pause is initiated, previously or currently, the text entry display 574 may be presented over the selected node with positive and negative selection buttons 584 , 586 , oval-arrow 270 , as shown in FIG. 30 . A progress reminder may be used to keep progress moving, essentially another clock that determines whether the user taken more than a predetermined amount of time between entry of data. A decision is made as to whether the progress reminder delay passed, diamond 272 . If the delay passed, the user is reminded, perhaps with window 588 , that the progress should continue, oval-arrow 274 as shown in FIG. 32 . Once reminded or if the delay did not pass, the user may enter an implication and designating the implication as positive or negative with buttons 584 and 586 , parallelogram 276 . Positive or negative may be selected using the tab key to highlight the correct button followed by the <<enter>> key or via clicking with a mouse. A decision is made as to whether there are four or more children of the current parent node, diamond 278 . If not, the method is directed to the step identified in rectangle 288 , which will be discussed in a moment.
[0132] When four or more children of the selected parent node are present, a test is initiated to determine that both positive and negative implications are present. At diamond 280 , a decision is reached as to whether there is at least one positive child of the select parent node. If no, the user is reminded, perhaps with window 590 of FIG. 33 , to include at least one positive implication, oval-arrow 282 and is directed to rectangle 288 . If there is a positive implication, a decision is made as to whether there is at least one negative implication, diamond 284 . If no, the user is reminded to include at least one negative implication, perhaps in window 590 of FIG. 33 , oval-arrow 286 and is directed to rectangle 288 . The method proceeds to rectangle 288 if there is both a positive and a negative implication.
[0133] At rectangle 288 , an implication is created in the arc data structure as a child of the selected parent implication with a positive or a negative value corresponding to the selected button and text corresponding to the user entered text. The arc is then written to permanent storage, cylinder 290 .
[0134] A decision is then made as to whether there is a multiple of a predetermined number of children, perhaps five, of the selected parent implication, diamond 292 . If so, an option 592 is displayed for another page of the predetermined number of children as shown in FIGS. 21 and 34 , oval-arrow 294 . Either after such display or if there is not a multiple of the predetermined number, the user is presented with two options. The user may exit this portion of the methodology through pentagon 298 , bringing the user back to the completion interface, pentagon 180 of FIG. 3 . Alternatively, the user may have the method automatically select the next empty node, i.e. a node without a corresponding implication, rectangle 296 . After such selection, the method resumes the course previously described starting with oval-arrow 270 .
[0135] Scoring in Completion Mode Upon entering, pentagon 330 of FIG. 6 , the function for scoring in completion mode, un-scored existing implications are displayed in the scoring mode with an un-scored visual indicator, such as blurriness or jagged edges 564 defining the node together with the other previously described scoring indicators 566 , 568 and 570 as shown in FIGS. 23 and 24 , oval-arrow 302 . The user may select a node that corresponds to an existing implication, parallelogram 304 . Next, diamond 306 , a decision is made by the method as to whether the scoring is “fast” mode or “detailed” mode. The fast mode gathers less precise information then the detailed mode. An appropriate scoring interface is displayed for the particular scoring mode as described below.
[0136] The “detailed” scoring interface, such as that shown in FIG. 23 and indicated in oval-arrow 308 , shows the buttons 594 for indicating desirability, buttons 596 for indicating likelihood, and a minority report interface button 598 . Preferably, the buttons 594 for desirability include a wide range of numerical indicators such as +50, +5, +4, +3, +2, +1, 0, −1, −2, −3, −4, −5, and −50. The desirability buttons 594 are used to indicate the preference of the occurrence of the implication. Such desirability buttons 594 may be color coded, perhaps in a gradient manner, perhaps with blue positive numbers with white or pale tones representing more neutral numbers and red representing the negative numbers. Preferably, the likelihood buttons 596 include a wide range of numerical indicators such as 90%, 80%, 70%, 60%, 50%, 40%, 30%, 20%, and 10% or 9, 8, 7, 6, 5, 4, 3, 2, and 1. For instance somebody may identify world peace as an implication of a summit meeting. Desirability may be marked as +50 according to a scoring method, but likelihood may be scored as 10% or 1. The node may be displayed, perhaps as a magnified node, together with any indicators showing its existing score.
[0137] The “fast” scoring interface, such as that shown in FIG. 24 is displayed, oval-arrow 310 , showing the buttons 600 for indicating desirability, buttons 602 for indicating likelihood, and a minority report interface 604 . Preferably, the buttons 600 for desirability include a smaller number of options of numerical indicators such as +50, +5 or +4, +3 to −3, −4 or −5, and −50. The desirability buttons are used to indicate the preference of occurrence of the implication. Such desirability buttons 600 may be color coded, perhaps in a gradient manner, perhaps with blue positive numbers with white or pale tones representing more neutral numbers and red representing the negative numbers. Preferably, the likelihood buttons 602 include a smaller number of options of numerical indicators perhaps being “greater than 70%” and “less than or equal to 70%”. The node may be displayed, perhaps as a magnified node, together with any indicators showing its existing score.
[0138] From the steps described in regard to oval-arrows 308 and 310 , the method seeks input from the user, parallelogram 312 . The user assigns desirability and likelihood to the implications by clicking on the scoring buttons 595 and 596 or 600 and 602 . A response including both desirability and likelihood is required before the process can continue, except perhaps in fast scoring mode where a desirability of +3 to −3, e.g. neutral, does not require a likelihood scoring.
[0139] Next, rectangle 314 , the scored nodes are colored and shaped to visually indicate the desirability and likelihood combinations. Any prior scoring or non-scored, e.g. un-scored, indicators are removed in this process. FIGS. 23 and 24 are examples of different visual indicators that may be used to depart information about scored and un-scored nodes. For example, nodes that have not been scored remain blurry or with jagged edges 564 . Nodes that are not a child of the selected node may be presented in a small or abbreviated manner. Scored nodes may be shown with a smooth non-jagged outer perimeter such as nodes 566 . Significant nodes may be identified with stars such as nodes 568 . Nodes with a high likelihood, e.g. greater than 70% may be visually identified with a second ring 570 about the node. That is, those with a significant desirability score and significant likelihood may be made more prominent so as to draw the viewer's attention to those nodes of the greatest impact and those of less impacting and less likely implications are displayed less prominently. Any scored node that was previously visually marked as un-scored loses its visual “un-scored” indicator when it is scored.
[0140] The arc data is written to permanent storage, cylinder 316 . The method waits for either of three inputs, the user may submit a minority report, parallelogram 318 , the user may score another node, as was described starting at parallelogram 304 , or the user may go to the completion interface, pentagon 320 of FIG. 6 and pentagon 180 of FIG. 3 .
[0141] When the user clicks the minority report button 598 or 604 , parallelogram 318 , the minority report interface 605 is displayed, oval arrow 320 . The minority report interface 605 , shown in FIG. 35 preferably has fields for identification of the reporter(s) 606 , minority score 608 and reason for minority report 610 . The user may click “o.k.” on button 612 or “cancel” on button 614 (or similar indicators of action), parallelogram 322 . If “cancel” is selected, button 614 , the minority report interface 605 is hidden, oval-arrow 324 , and the method waits for user selection of one of the three choices identified with regard to cylinder 316 . If “O.k” button 612 was selected, a decision is made as to whether all required fields, perhaps 606 , 608 , and 610 of the minority report interface 605 are completely filled. Preferably all fields are required, diamond 326 . If not, the user is notified, perhaps with window 616 of FIG. 36 that only complete minority reports will be submitted, oval-arrow 328 , and the method is redirected to the point previously described with reference to parallelogram 322 . If complete, the minority report is recorded in the current implication and a visual indicator for a minority report, such as a subscript or superscript “M”, may be displayed next to the node that has a minority report, rectangle 330 . Completion of the process step in rectangle 330 , is followed with hiding of the minority report entry interface, oval-arrow 332 . The arc data is written to permanent storage as previously described in regard to cylinder 316 and resumes the method as previously described with regard to cylinder 316 .
[0000] Timing
[0142] Timing allows for users to estimate the amount of time that it may take to pass from the occurrence of one implication on through to a higher order implication directly resulting therefrom. The timing function, entered through pentagon 334 of FIG. 7 , accessible from pentagon 218 of FIG. 3 , first displays diamonds 618 between ancestral implications, oval-arrow 336 , as shown in FIGS. 29 and 37 . The user may select a diamond that corresponds to an existing implication, parallelogram 338 . A magnified time diamond 620 may be displayed with any existing time assignment along with magnified nodes 622 , 624 between which the time diamond is preferably positioned in the wheel, oval-arrow 340 , as shown in FIG. 37 .
[0143] The user may switch between days, weeks and years and any pre-existing time units automatically convert to the newly selected units of time measure, parallelogram 342 . The user may enter a number and submit the information, perhaps through clicking, using the <<enter>> key or <<tab>> key or other method, parallelogram 344 . The magnified time diamond 620 , two magnified nodes 622 , 624 , assigned time and any indicator as to time units are hidden, oval-arrow 346 , as shown in FIG. 29 . The data is written to permanent storage for later retrieval and use, cylinder 348 . The user may repeat the process, starting at parallelogram 338 or return to the completion interface, pentagon 350 of FIG. 7 and pentagon 180 of FIG. 3 .
[0000] Spell Check
[0144] FIG. 8 discloses the process whereby a user may spell check the text within the nodes, entered from pentagon 352 . A decision is made as to whether an implication has already been selected, diamond 354 . If not, then the method selects the first second order implications, rectangle 356 . Since the first order implication is not editable, it cannot be spell checked. Once an implication has been selected, either via the user or the method, the currently selected implication identification is saved in a variable for comparison, rectangle 358 . The implication is then evaluated to determine if it has a misspelled word, diamond 360 .
[0145] Implications that have a misspelled word are displayed in a magnified node 626 in an editable mode with the misspelled words marked with indicia 628 , oval-arrow 362 as shown in FIG. 38 . The user may submit the text, edited or otherwise, perhaps by pressing <<enter>>, <<tab>> or clicking, parallelogram 364 . The arc is written to permanent storage, cylinder 366 . The next implication in the data structure is selected, rectangle 368 . The step at rectangle 368 is also directly reachable from diamond 360 if the implication has not misspelled words. The process repeats the steps between diamond 360 and rectangle 368 until all implications have been spell checked, diamond 370 , or until the user selects cancel, parallelogram 372 . Upon completion or termination, the user is directed to the completion interface through pentagon 374 of FIG. 8 and pentagon 180 of FIG. 3 .
[0000] Scoring Interface
[0146] The scoring interface, entered through pentagon 376 , accessible through pentagon 176 of FIG. 2 , i.e. only if scoring was assigned, first determines whether time was assigned, diamond 378 . Note, that the flow chart diamonds and time diamonds are different in nature with flow chart diamonds indicating a decision making point and time diamonds recording an estimated time that would elapse between two implications if such implications do occur. If time was not assigned, the interface is displayed with options to open another arc 546 ( FIG. 25 ), quit/exit 548 ( FIG. 25 ), score from all assigned points of view 638 ( FIG. 39 ), and return the completed arc 640 ( FIG. 39 ), oval-arrow 380 . If time was assigned, the user has the options of open another arc 546 ( FIG. 25 ), quit/exit 548 ( FIG. 25 ), score from all assigned points of view 638 ( FIG. 39 ), time from all assigned points of view 642 ( FIG. 39 ) and return the completed arc 640 ( FIG. 39 ), oval-arrow 382 . Presentation of these options may also occur through pentagon 384 . (See pentagon 414 of FIG. 10 ).
[0147] The user has the option to open another arc, parallelogram 386 , which if selected directs the user back to diamond 102 of FIG. 1 via pentagons 388 and 101 .
[0148] The user has the option to score from all assigned points of view, parallelogram 390 . If selected, the full arc is displayed in scoring mode as shown in FIGS. 23 and 24 . Un-scored implications are marked with indicia 564 , such as blurry lines or jagged edges, to designate the nodes as un-scored, oval-arrow 392 . The user is directed to FIG. 10 via pentagon 394 ( FIG. 9 ) and pentagon 412 ( FIG. 10 ). Between the pentagons 412 and 414 on FIG. 10 , the flowchart is preferably identical to that in FIG. 6 with the difference being the entrance and exit points.
[0149] The user may select timing from one assigned point of view, parallelogram 396 . The full arc is displayed in timing mode as shown in FIG. 29 , oval-arrow 398 , and the user is directed to the steps identified on the flowchart in FIG. 11 , see pentagons 400 ( FIG. 9 ) and 416 ( FIG. 11 ).
[0150] The user may select to return the completed arc, parallelogram 402 . A process, rectangle 404 , occurs such as logging in to the data server over secure channels with locally stored login information. The content data is encrypted and the arc is returned to the server. This may be an asynchronous process. The user is directed to the step previously described in regard to diamond 102 of FIG. 1 via pentagons 406 ( FIG. 9 ) and 101 ( FIG. 1 ).
[0151] The user may select to quit/exit the process, parallelogram 408 , which terminates the methodology, oval 410 .
[0000] Scoring in Scoring Mode
[0152] The flowchart in FIG. 10 denotes that the process is preferably substantially the same as that shown in FIG. 6 . FIG. 6 is the scoring process that occurs when the user accesses scoring from the completion interface of FIG. 3 and FIG. 10 is the scoring process that occurs when the user accesses scoring from the scoring interface of FIG. 9 . While the scoring process remains substantially unchanged, the interface where the user starts is the interface to where the user should be returned upon completion of scoring. The user is returned to the interface from where they initiated the scoring process as indicated by the pentagons 180 , 212 of FIGS. 3 corresponding with pentagons 300 and 320 of FIG. 6 as compared with pentagons 384 and 394 of FIG. 9 corresponding with pentagons 412 and 414 of FIG. 10 .
[0000] Timing
[0153] A user may select to enter time from the scoring interface, FIG. 9 , wherein the user was directed from pentagon 400 of FIG. 9 to pentagon 416 of FIG. 11 . Time diamonds are made visible between implications and their parent, oval-arrow 418 as shown in FIG. 29 . The user may click a diamond that corresponds to an existing implication, parallelogram 420 . The time diamond 618 may be displayed as a magnified diamond 620 together with and existing time assignment, along with magnified versions of the two implications 622 , 624 between which the time diamond 620 appears, oval-arrow 422 , as shown in FIG. 37 .
[0154] The user may select the units of time measure, e.g. days, weeks, and years, parallelogram 424 , and any pre-existing time assignment is converted to the newly selected units of time measure. The user may enter a number of units, e.g. three days or four weeks, etc., and submit the information preferably via pressing the <<enter>> key, <<tab>> key or clicking, parallelogram 426 . Upon submission, the magnified time diamond 620 , the two implications 622 , 624 and the indicator as to units of measure are removed from display as shown in FIG. 29 , oval-arrow 428 . The arc is then written to permanent storage, cylinder 430 . The user may select another time diamond, parallelogram 420 , or return to the scoring interface, pentagon 432 ( FIG. 11 ) and pentagon 384 ( FIG. 9 ).
[0155] The appended computer program coding is offered as a further description to those skilled in the art of computer programming to more fully understand the present invention and further explain the subject matter described herein.
[0156] Although the present invention has been described with reference to preferred embodiments, workers skilled in the art will recognize changes may be made in form and detail without departing from the spirit and scope of the invention. For instance, different indica and shapes may be used to impart information concerning the nodes and scoring thereof.
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An investigative method, comprising a variety of strategic step controls to prevent user misuse including displaying the entire arc only when the second order implication stage is complete, allowing the option of timing from one assigned point of view only when timing was assigned, presenting third order nodes only when there is at least one positive and at least one negative second order implication, reminding the user to provide input if a predetermined amount of time has passed from the last receipt of input, permitting scoring of an arc only when scoring is assigned, disabling editability of implication text if scoring was assigned, directing a user to a scoring interface if only scoring was assigned, displaying desirability buttons and likelihood buttons when scoring, displaying a minority report interface when the minority report button is clicked, precluding acceptance of an incomplete minority report, precluding an option of time from all assigned points of view if time was not assigned and displaying options of open another arc, quit, score from all assigned points of view, time from all assigned points of view, and return completed arc.
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RELATED APPLICATION DATA
[0001] The present invention claims priority to and is a continuation of application Ser. No. 10/853,545 filed May 24, 2004 entitled Hybrid Semiconductor-Magnetic Device and Method of Operation, which in turn is a continuation of application Ser. No. 10/100,210 filed Mar. 18, 2002 entitled “Magnetoelectronic Memory Element With Inductively Coupled Write Wires,” now U.S. Pat. No. 6,804,146, which application Ser. No. 10/100,210 is a continuation of an application Ser. No. 09/532,706 filed Mar. 22, 2000 titled “Magnetoelectronic Memory Element With Isolation Element” (now U.S. Pat. No. 6,388,916). The latter application Ser. No. 09/532,706 is in turn a divisional application of Ser. No. 08/806,028 filed Feb. 24, 1997 entitled “Hybrid Hall Effect Memory Device & Method of Operation,” now U.S. Pat. No. 6,064,083. Ser. No. 08/806,028 is a continuation-in-part of Ser. No. 08/643,805, filed May 6, 1996 titled “Hybrid Hall Effect Device and Method of Operation,” (now U.S. Pat. No. 5,652,445), which in turn is a continuation-in-part of an application Ser. No. 08/493,815, filed Jun. 22, 1995 titled “Magnetic Spin Transistor Hybrid Circuit Element,” (now U.S. Pat. No. 5,565,695); and said Ser. No. 08/806,028 is also a continuation-in-part of an application Ser. No. 08/425,884, filed Apr. 21, 1995 titled “Magnetic Spin Transistor, Logic Gate & Method of Operation,” (now U.S. Pat. No. 5,629,549); and an application Ser. No. 08/643,804 filed May 6, 1996 titled “Magnetic Spin Injected Field Effect Transistor and Method of Operation,” (now U.S. Pat. No. 5,654,566).
[0002] The above applications and materials are expressly incorporated by reference herein.
FIELD OF THE INVENTION
[0003] This invention relates generally to hybrid electronic devices comprised of semiconductor structures in combination with ferromagnetic components. In particular, the present invention is directed to a spin polarized electron conduction device formed from ferromagnetic films. The ferromagnetic components contribute new parameters to the devices permitting new applications and improved performance in environments such as non-volatile memory storage.
BACKGROUND OF THE INVENTION
[0004] The semiconductor Field Effect Transistor (FET), fabricated typically as a metal oxide semiconductor (MOSFET) structure on a silicon substrate or as a Gallium Arsenide (GaAsFET) device on a Gallium Arsenide substrate, is the building block of modern digital electronics. For example, memory cells for the storage of binary information and logic gates for the processing of digital data streams both use FETs as the primary components.
[0005] A review of the cell structures of various prior art memory devices follows. Some of these, such as leading volatile memory technology (i.e. memory which is lost when power is not applied, such as in a dynamic random access memory (DRAM)) use conventional semiconductor FET structures and capacitors in their cell designs. A number of alternative memory technologies that are nonvolatile (i.e. memory is retained when power is not applied) use magnetostatic coupling and magnetoresistors comprised of ferromagnetic elements to effectuate a data storage function. In addition, a recent non-volatile device proposed by the present applicant (see U.S. Pat. No. 5,432,373) using a magnetic spin transistor with one or more passive elements is also reviewed.
[0006] Finally, a brief review of the operation of typical logic gates based on conventional FET technology is also provided.
[0000] Cell Structures Used In Conventional Volatile Memory Devices
[0007] In the case of memory cells used in DRAMs, the most common commercial cell consists of only two elements, a capacitor for data storage and a field effect transistor (FET) for isolation from the array. This cell is popular because the cell size can be made small, resulting in a high packing density and a relatively low production cost. The storage element is a capacitor, and the two stable states representing the binary data “1” or “0” can be, for example, the states with stored charge Q or with stored charge 0. Every cell is connected to an array of write and read wires, also called “bit” and “word” lines. Since one capacitor linked together with other capacitors in an array will lose its charge to its neighbor, the capacitor of each cell is connected to a transistor within that cell so as to be isolated from the array. When the transistor is “on” there is a low resistance to a write or read wire so that an applied voltage can charge the capacitor during a write process or a sense circuit can determine the stored charge during a read process. When the transistor is “off,” a high impedance to the write or read wire isolates the capacitor electrically from any other element in the array.
[0008] Typically, a Metal Oxide Semiconductor Field Effect Transistor (MOSFET) for use in a DRAM is fabricated by standard lithographic processing techniques on a silicon substrate. The oxide that isolates the gate from the channel is highly insulating, so that the metallized gate has a capacitance to the rest of the device. In some designs the gate capacitance is used as the storage capacitance. Reading is performed with a sense circuit that compares the charge (or voltage) of C with the charge (or voltage) of a standard capacitor C′ in a dummy cell. Readout voltages are the order of 10 to 100 mV and the stored charge Q is the order of a million electrons.
[0009] The conventional DRAM memory device, however, suffers from a number of operational and physical drawbacks. For one, the memory is volatile. Unavoidable leakage currents discharge the capacitor so that each cell must be refreshed constantly, i.e. read and rewritten, approximately every few milliseconds. Furthermore, background alpha-particle radiation can induce sufficient conductance in the MOSFET to drain the capacitor spuriously, erasing the memory of that cell.
[0010] Finally, cell dimensions are not shrinking to the limit permitted by lithography because of restrictions on the capacitor and FET size. Consequently, there are limits on how dense these devices can be made using conventional techniques.
[0000] Cell Structures Used in Alternative Non-Volatile Memory Devices
[0011] Several alternative technologies can be used to make nonvolatile memory cells. Capacitive memory elements utilizing ferroelectric material as a dielectric have undergone decades of development work, but still suffer from fatigue: they cannot provide an infinite number of read/write cycles.
[0012] Several competing approaches use ferromagnetic materials. Three such technologies are reviewed below.
[0000] Magnetoresistive Random Access Memory (MRAM)
[0013] Magnetoresistive Random Access Memory was proposed a decade ago [J. M. Daughton, “Magnetoresistive Memory Technology,” Thin Solid Films 216, 162 (1992)] This device employs an array of bit and word lines. Each bit line is divided into n storage cells. Each cell is a trilayer composed of a ferromagnetic metal base layer, a nonmagnetic metal middle layer, and a ferromagnetic metal top layer. Note that the F—N—F geometry is not the same as giant magnetoresistance (GMR) structures; the layers are so thick that interfacial spin scattering at the F—N interfaces is a negligible fraction of all scattering events, and there is no exchange coupling across the N layer. The cell has length l, width w and thickness d. Looking at a cell in cross section across the width, there are two stable magnetization states determined by magnetostatic coupling, each with the magnetization of the two ferromagnetic films oriented in opposing directions: clockwise and counterclockwise.
[0014] The resistance of each cell, measured with a sense current applied along the length of the cell, is a function of the anisotropic magnetoresistance (AMR) of the F layers. It has value R 1 when the magnetizations are perpendicular to the sense current (as is the case for either stable magnetization state) and R 1 ′ if the magnetizations of the ferromagnetic layers are forced to lie parallel to the sense current. Each cell in the bit line is connected to the next cell with a conducting strip which has resistance R c .
[0015] Columns of n word lines cross the m rows of bit lines. Each nonmagnetic word line crosses the top of a cell in each bit line. The state of cell (i,j) is written by sending current pulses of appropriate amplitude through bit line i and word line j, using the magnetic fields from the currents to cause the magnetization of the cell to orient either clockwise or counterclockwise. The contents of the cell are read by first biasing word line j with a large enough current so that fields from the current cause the magnetizations of both ferromagnetic layers to be canted to an orientation that is approximately 45 degrees away from the axis of the bit line.
[0016] In this orientation the resistance of the cell (for a sense current applied along the bit line) has a value R 2 that is between R 1 and R 1 ′. Next, a sense current is applied along the bit line, and a voltage is measured across the bit line, having a value proportional to (n−1)R 1 +R 2 +nR c . Finally, a read current pulse is applied to the word line, in addition to the original bias current. The field from this current pulse changes the magnetization orientation in a direction more nearly parallel to the sense current if the initial orientation was clockwise, or in a direction more nearly perpendicular to the sense current if the initial orientation was counterclockwise. Thus, the voltage across the bit line either increases or decreases when the read pulse is applied. A sense circuit that measures changes of voltage records the positive or negative change as a “1” or a “0.”
[0017] By using a derivative sense technique, MRAM avoids the necessity of electrically isolating each cell. However, this approach for a non-volatile memory element also suffers from a number of drawbacks.
[0018] To begin with, the readout voltage is quite small and the signal to noise ratio is poor. The change in resistance that must be sensed during the read process is a small fraction of R 1 , and this small change must be distinguished from a background of approximately nR 1 +R c . In practice, two elements are fabricated for each cell, thus doubling the signal, and the read process is repeated several times so that the final readout is taken as an average of repeated samplings, thus lowering the noise. This increases the time for a read cycle. Power dissipation is relatively large during readout because relatively large currents must be applied to long, resistive lines. Finally, errors can be introduced during readout if the bias current tips the magnetization into an unstable state.
[0000] MRAM with GMR Elements
[0019] Another conventional approach uses a magnetoresistor R as the storage element, and the cell is comprised of R, a reference resistor R′, and two or three FETs to isolate the cell from the rest of the array. The magnetoresistor R is typically a thin film ferromagnetic metal (or ferromagnetic/nonmagnetic metal multilayer) resistor with length l, width w and thickness d, and has two values, R′ and R′+δR, corresponding to two stable magnetization states.
[0020] For example, in one state the magnetization of a permalloy film might be parallel to the direction of flow of the sense current, I sense , and in the other state the magnetization might be perpendicular to I scene . For GMR elements, one state corresponds to the magnetizations {circumflex over ( )}M 1 and {circumflex over ( )}M 2 of F 1 and F 2 aligned parallel (or the magnetizations M i of all ferromagnetic layers in a multilayer stack aligned parallel), and in the other state {circumflex over ( )}M 1 and {circumflex over ( )}M 2 are antiparallel (or the alternate ferromagnetic layers of the multilayer stack are antiparallel). The magnetization state is written by using the magnetic field generated by current pulses applied to an array of write lines.
[0021] The read process begins by selecting a cell. When a cell is addressed the isolating FETs are set to the “on” state by driving the appropriate word line to a high voltage. In this state the FETs conduct current with some low resistance, the order of 1000 Ω or less. A bias current I sense is then applied to both the magnetoresistor R and the reference resistor R′. A sense circuit at the end of a line of cells compares the two voltages and interprets a “1” or “0” when, for example, I Sense *(R−R′)>0 or I sense *(R−R′)=0 respectively. The voltage levels corresponding to “1 38 (or “0”) are then amplified to TTL or CMOS levels.
[0022] The voltage I sense *δR that distinguishes a “1” from a “0” must be large enough for reliable discrimination. Since the magnetoresistive ratio δR/R′ of ferromagnetic films (or GMR multilayers) is small, 10 percent or less, the magnetoresistor must be made quite large. For example, with R=100 Ω and δR/R′=0.06, a reasonable bias current of 1 mA would produce a readout voltage difference of only 6 mV, and a poor signal to noise ratio is a characteristic of GMR cells.
[0023] This approach has several other drawbacks. A resistor occupies substantial area in a cell. Continuing the above example, the 100 Ω magnetoresistor could be fabricated using ferromagnetic materials with resistivities of about 20 μΩ-cm, with a length l=5 μm, width w=1 μm, and thickness d=0.01 μm. In addition, this cell requires the fabrication of two resistors, R and R′, thus requiring additional isolation FETs and, all together, taking up considerable space. The reference resistor cannot be placed outside the cell because the resistive difference, δR, is so small that the resistance of each memory resistor must be matched to a particular reference. Since resistance is a function of temperature, R=R(T), the reference resistor must be fabricated very near the magnetoresistor so that both resistors will always be at the same temperature, and the material for the reference resistor must be carefully chosen so that the temperature dependence of its resistivity is similar to that of the magnetoresistor. Finally, the resistance of each cell is quite large. When numerous cells are placed on a single read line, as in an array, the resistance of the read line is substantial. Since the read process uses current bias, the power dissipated in each read cycle is relatively large.
[0000] Spin Transistor Nonvolatile RAM (NRAM)
[0024] Active devices using magnetic spin transport are well known in the art. The history of spin transport begins with an experiment by Meservey [R. Meservey, P. M. Tedrow and P. Fulde, Phys. Rev. Lett. 25, 1270 (1970); P. M. Tedrow and R. Meservey, Phys. Rev. Lett. 26, 192 (1971); Phys. Rev. B 7, 318 (1973)] where it was shown that the electric current tunneling from a ferromagnetic electrode across a low transmission barrier into a superconducting detector carried a net spin polarization. A later spin injection experiment [described in several journals, including Mark Johnson and R. H. Silsbee, Phys. Rev. Lett. 55, 1790 (1985); Phys. Rev. B 35, 4959 (1987); Phys. Rev. B 37, 5312 (1988); Phys. Rev. B 35, 5326 (1988)] then demonstrated that (i) current driven across any ferromagnet-nonferromagnet (F 1 -N) interface carried a net spin polarization, (ii) that a nonequilibrium population of spin polarized electrons, equivalently a nonequilibrium magnetization ˜M, diffused away from the F 1 -N interface into N with a characteristic length equal to the classic spin diffusion length δ s , and (iii) that the nonequilibrium magnetization in N affected the current flow (or the voltage developed) at the N-F 2 interface of a second ferromagnetic film.
[0025] The idea of incorporating the spin injection effects to semiconductors was mentioned in the art even before the spin injection experiment by the present applicant proved the validity of the phenomenon. Indeed, Aronov [A. G. Aronov, Sov. Phys. JETP 24, L32 (1976)] proposed that a current driven from a ferromagnet into a semiconductor would be spin polarized, and that the spin polarization of the current in the semiconductor (N) would be maintained over a length scale of a diffusion length. However, to date applicant is unaware of any known successful implementations of these proposals.
[0026] Datta and Das, citing the spin injection experiment performed by the applicant, and noting the long spin diffusion lengths measured in aluminum (δ s approximately 0.5 mm at low temperature), proposed [S. Datta and B. Das, Appl. Phys. Lett. 56, 665 (1990)] a device illustrated in FIG. 2 wherein spin injection is extended to a FET-like structure: iron contacts are employed as the source and drain and the gate voltage was to be used to modulate the source-drain current allowing the device to perform as a current modulator. According to their proposed device a nonmagnetic metal gate 174 is fabricated on a Schottky (or an insulating) barrier 176 on top of a layer of InAlAs 178 that is grown on an InGaAs substrate 180 . The InAlAs—InGaAs interface forms a high conductance Two Dimensional Electron Gas (2DEG) 182 region that acts as the conducting channel between source and drain, which are thin iron films 170 fabricated on either side of the gate 174 and in contact with the 2DEG 182 . The magnetizations, {circumflex over ( )}M s 184 and {circumflex over ( )}M d 186 , of the source and drain ferromagnetic films are always aligned in parallel and along the {circumflex over ( )}x direction. The source provides spin polarized electrons to the channel with the spin axes of the electrons oriented parallel to the magnetization of the source and drain, along {circumflex over ( )}x. Because of the spin injection effect the source—drain conductance is proportional to the projection of the spin orientation of the polarized electrons reaching the drain on the orientation of the drain magnetization. A voltage V g 172 applied to the gate 174 generates an electric field along {circumflex over ( )}z along with an associated effective magnetic field along {circumflex over ( )}y, and causes the spin axis of each electron to precess [refer to a description of the Rashba effect in the above article by Datta and Das]. Thus, the orientation of the spin axes of the current carrying electrons relative to the magnetization 186 of the drain is a function of gate voltage 172 : the source-drain conductance (and current) is modulated periodically as the gate voltage is monotonically increased, and the device proposed by Datta and Das functions as a current modulator.
[0027] The Datta and Das device, however, has not yet been sucessessfully fabricated and demonstrated, and the concept has never been adapted to be used as a conventional FET because a Schottky barrier at the semiconductor—iron interface damages device performance by introducing large resistances at the source and drain. It is also likely (though unproven) that the Schottky barrier acts to impede the flow of spin polarized electrons by randomizing the spin orientation of each electron. Neither has the Datta and Das device concept been adapted to be used as a memory element because the magnetizations {circumflex over ( )}M s and {circumflex over ( )}M d were locked in a parallel configuration. Furthermore, the polarized spins were injected with orientation along {circumflex over ( )}x so that they would precess under the influence of the effective magnetic field (associated with the gate voltage) along {circumflex over ( )}y, and the length of the 2DEG conducting channel was designed to be sufficiently long that the spin polarized electrons could accumulate large phase angles as a result of their precession. In practice, precession under the influence of a field along {circumflex over ( )}y leads to randomization of spin orientation and acts to destroy the knowledge of the initial state of the spin polarized electron; therefore the information of the memory state (of the source or drain) is lost.
[0028] A replacement for conventional semiconductor devices was proposed by the present applicant in connection with a device known as the bipolar spin transistor. This device and related modifications is described-in Mark Johnson, “The All Metal Spin Transistor,” I.E.E.E. Spectrum Magazine, Vol. 31 No. 5 p. 47 (1994); and Mark Johnson, “The Bipolar Spin Transistor,” Science 260, 320 (1993). This device is depicted in FIG. 1 , with F 1 150 and F 2 152 arranged on one side of a bulk sample of aluminum 154 . F 1 150 injects a source of diffusing spin polarized electrons 156 and F 2 152 detects their presence. This device is a novel F—N—F structure that can be used as a circuit element in a nonvolatile memory cell and has several advantages. Since the readout voltage is bipolar, positive for {circumflex over ( )}M 1 and {circumflex over ( )}M 2 parallel and negative for {circumflex over ( )}M 1 and {circumflex over ( )}M 2 antiparallel, the discrimination between a logical “1” and “0” is relatively easy; each cell needs only a single storage element whose readout is compared with ground. Furthermore, the transimpedance of the spin transistor scales inversely with size, so the readout voltage is larger (for constant current) for smaller devices, thus promoting the shrinking of cell size.
[0029] Two characteristics of the device must be taken into consideration when using the device in NRAM. First, the device can be fabricated entirely from metals, and is therefore characterized by a low electrical impedance. Thus, to fabricate an array of such elements it is necessary to electrically isolate each element from others in the array, so that the output of any element will not be shorted to ground through a neighboring element. Second, the output voltages available from the device are less than TTL or CMOS levels, and the output must therefore be amplified before it is incorporated in TTL or CMOS circuits.
[0030] Another spin transistor NRAM cell design [Mark Johnson, “Magnetic Spin Transistor,” U.S. Pat. No. 5,432,373, issued Jul. 11, 1995] is composed of a spin transistor and one or more capacitors and resistors. The passive elements provide isolation for the spin transistor of each cell, and the readout voltage was transmitted to the end of a line of elements for amplification. A drawback of this design is that resistors and capacitors take up substantial space on a chip. Thus, a substantial portion (even a majority) of cell area is occupied by passive elements, packing densities are limited, and the unique scaling feature of the spin transistor is wasted.
[0031] Furthermore, cell isolation is not very efficient and the readout voltage can be degraded during transmission to the sense circuit, resulting in higher noise and lower readout sensitivity. More recent proposals for spin transistor memory cell designs [see applications referenced above] incorporate a spin transistor with one (or more) isolating FETs. This is a practical approach, and can achieve packing densities comparable with, or higher than, DRAM.
[0032] However, until the present invention it has been impossible to integrate the functions of nonvolatile storage and cell isolation in a single element.
[0000] FET Logic Gates
[0033] Logic operations in computing devices are typically performed with digital voltage pulses and FET gates that are linked together in an appropriate way. To provide an example that permits a brief critical discussion, a standard arrangement [Paul Horowitz and Winfield Hill, “The Art of Electronics,” Cambridge Univ. Press, Cambridge U.K. (1980); see p. 328] for an AND gate operation is depicted in FIG. 3 where each element Q i is an enhancement mode FET. Q 1 10 , Q 2 12 and Q 5 18 are p-channel FETs. A p-channel FET has a high impedance, and is therefore in the “off” state, when the gate voltage is zero or positive. It has a low impedance, and is therefore in the “on” state, when the gate voltage is lower than a threshold value below zero (where the threshold value is typically 0.5 Volt or less). Q 3 14 , Q 4 16 and Q 6 20 are n-channel FETs. An n-channel FET is “off” when the gate voltage is below ground and “on” when the gate voltage is larger than a threshold value above ground. Voltage pulses of positive or zero amplitude (HIGH or “1”; or LOW or “0”) are applied simultaneously to the inputs A 22 and B 24 , and the cell operates as an AND gate in the following way.
[0034] When inputs A 22 and B 24 are HIGH (“1”+“1”), Q 3 14 and Q 4 16 are “on”, Q 1 10 and Q 2 12 are “off”, and consequently the voltage at node 26 is at LOW, i.e. at ground. Since Q 6 20 is “off” and Q 5 18 is “on” the voltage output (OUT) 28 is HIGH (“1”). When A 22 and B 24 are LOW (“0”+“0”), Q 3 14 and Q 4 16 are “off”, Q 1 10 and Q 2 12 are “on”, and consequently the voltage at node 26 is HIGH. Since Q 5 18 is “off” and Q 6 20 is “on” the voltage output (OUT) 28 is LOW, at ground (“0”). When A 22 (or B 24 ) is HIGH and B 24 (or A 22 ) is LOW (“1”+“0”), Q 3 14 and Q 2 12 are “on”, Q 1 10 and Q 4 16 are “off”, and consequently the voltage at node 26 is HIGH and the voltage output (OUT) 28 is LOW, at ground (“0”). The truth table 30 for the above operations is seen to be the same as that of an AND gate.
[0035] Although logic gates of this design are the backbone of digital electronic processing, they suffer from several disadvantages. It requires numerous FETs (six in the example of FIG. 1 ) to comprise the logic gate cell, and therefore the cell occupies a large area of the chip. Furthermore, the result of the Boolean process is not stored and must be synchronized with a clock cycle to be used in the next operating step, or must be sent to a separate storage cell for later recall. The above discussion was presented for complimentary metal oxide silicon (CMOS) logic devices. The transistor—transistor logic (TTL) family is based on bipolar transistors, but similar conclusions apply. In other words, the cell of a single TTL logic gate is comprised of several transistors and several resistors, and uses considerable space on a chip. It is apparent that it would be desirable to integrate the functions of logic operation and storage in a single element.
SUMMARY OF THE INVENTION
[0036] Accordingly, there is a significant need for improved FETs and similarly operating logic devices that can be used easily and reliably in high density memory and logic environments.
[0037] An object of the present invention therefore is to provide a novel hybrid FET structure that can be used as a memory element for the nonvolatile storage of digital information, as well as in other environments (including, for example, logic applications for performing digital combinational tasks, or a magnetic field sensor).
[0038] According to a first embodiment of the present invention, a novel FET is describing using ferromagnetic materials for the source and drain, and can be described as a “spin injected FET.” This spin injected FET has two operating stable states determined by the gate voltage, “off” and “on”. The first (e.g. source) and second (e.g. drain) ferromagnetic layers of this new FET are both fabricated to be magnetically anisotropic so as to permit the device to have two stable magnetization states, parallel and antiparallel. In the “on” state the spin injected FET has two settable resistance states determined by the relative orientation of the magnetizations of the ferromagnetic source and drain, “HIGH” (antiparallel) and “LOW” (parallel). One of the ferromagnetic films (source) can be fixed with a large magnetic coercivity and polled in one direction and the other ferromagnetic film (drain) has a smaller coercivity. An external magnetic field can change the magnetization state of the device by orienting the magnetization of the drain to be parallel or antiparallel relative to that of the source.
[0039] In a magnetic sensor embodiment of the present invention, the spin injected FET can be incorporated in a “read” head for reading digital magnetic recorded data.
[0040] In a memory storage element embodiment, the spin injected FET can be provided having a conductive write layer for carrying a write electric current and inductively coupling a write magnetic field associated with this write current to the second (drain) ferromagnetic film. An external current generator can change the magnetization state of the drain, therefore, by inductively coupling a magnetic field to the drain. Even if power is removed from the above device, the second ferromagnetic film orientation is retained in its set state, thus causing the spin injected FET to behave as a non-volatile memory element because the two states of the magnetization orientation of said second ferromagnetic layer can correspond to data values stored in said memory element. An array of spin injected FETs can be coupled together in an array to form a spin injected FET memory array.
[0041] The present spin injected FET therefore will find application as the basic storage element in integrated arrays of nonvolatile random access memories (NRAM), and may replace DRAM and direct access memory (such as magnetic disk drives) in many applications. The present spin injected FET invention is a substantial improvement over prior memory cell elements. Compared with DRAM, the spin injected FET has only a single element in the cell permitting the memory cell to be made smaller, the memory is nonvolatile and is not susceptible to errors induced by background radiation (i.e. it is radiation hard). Compared to other nonvolatile memory cells, the spin injected FET has only a single element, permitting the cell size to be smaller, the cell is automatically isolated from the array unless it is addressed, and the memory array is compatible with existing CMOS (or other semiconductor) technology.
[0042] Further according to another embodiment of the present invention, a logic gate can be fabricated using the spin injected FET. This logic gate can implement any desired combinational task (function) relating one or more inputs to the spin injected FET to an output thereof. Depending on the particular function to be implemented, the state of the logic gate (which is determined by the magnetization state of the drain) is first set using a magnetic field generated by a current pulse transmitted in a write line inductively coupled to the ferromagnetic drain. This same wire also inductively couples a magnetic field generated by the combined current of one or more input data signals to the spin injected FET. The ferromagnetic drain magnetization can be configured to change or retain its orientation, depending on a particular combination of input data signals corresponding to the boolean operation desired. In other words, the ferromagnetic drain magnetization may be read out as an output binary “1” or “0” corresponding to some Boolean process dependent on the data input signals.
[0043] In any specific logic function embodiment, therefore, the present invention can be configured to implement the function of any of the following gates: a NOR gate, a NOT gate, a NAND gate, an OR gate and an AND gate, or more generally any logic gate implementing a combinational task relating one or more combination of inputs/outputs. The present spin injected FET invention is a substantial improvement over prior logic gates using semiconductor transistors [ordinary FETs for CMOS or bipolar transistors for TTL]. The spin injected FET requires fewer elements per logic cell, so cell size can be reduced and packing density increased. The result of each processing step is stored as the nonvolatile state of the device and can be read out at any later time, without synchronization to a clock cycle. In this way, parallel processing by several logic gates is facilitated. Furthermore, although the basic ideas are presented herein for a two-state device, appropriate for binary processing, it is possible to fabricate a ferromagnetic layer with more than two stable magnetization states. Therefore, more generally an n-state device can be fabricated, and simultaneous processing of n bits by each logic gate is possible.
[0044] Furthermore, in contrast to the prior art Datta and Das spin transport device described above, the spin injected FET of the present invention employs one ferromagnetic layer (source) with fixed magnetization orientation and a second ferromagnetic layer (drain) with a magnetization whose orientation changes between two stable configurations: parallel or antiparallel with the magnetization orientation of the source. The invention then uses the memory effect associated with the hysteresis of the ferromagnetic layer at the drain in order to create a spin injected FET memory element or logic gate.
BRIEF DESCRIPTION OF THE DRAWINGS
[0045] FIG. 1 is a schematic top view of a prior art “spin injection” all metal transistor that makes use of a spin polarized electron current;
[0046] FIG. 2 is a schematic cross-sectional view of a prior art FET current modulator using ferromagnetic films
[0047] FIG. 3 is a schematic representation of a logical AND gate cell comprised of conventional semiconductor field effect transistors (FETs), and an accompanying truth table;
[0048] FIG. 4 is a schematic cross-sectional view of a spin injected FET constructed in accordance with the teachings of the present invention;
[0049] FIG. 5 includes a number of density of state diagrams to describe charge and spin transport in the limit where two ferromagnetic electrodes are separated by a length L that is of the same order as an electron mean free path 1 , and where spin accumulation ˜M is negligible;
[0050] FIG. 6A is a top view of a typical physical implementation of the spin injected FET illustrated in FIG. 4 ;
[0051] FIG. 6B is a further cross-sectional view of the spin injected FET illustrated in FIG. 4 ;
[0052] FIG. 7A is a schematic cross-sectional view of a further embodiment of the present invention including a spin injected FET which operates as a memory cell, and an inductively coupled write line used for writing a logical data value to this cell;
[0053] FIG. 7B is a schematic cross-sectional view of a further embodiment of the present invention including a memory array having spin injected FETs operating as single memory cells, and a sense circuit that is used for reading the logical data value stored in a single cell;
[0054] FIG. 7C is a schematic plan view of another embodiment of the present invention which includes an array of spin injected FET memory cells and a sense circuit that is common to a number of cells in the array;
[0055] FIG. 8 is a schematic view of a further embodiment of the present invention which includes a spin injected FET used as a logic gate and a readout circuit that can be used therewith.
DETAILED DESCRIPTION OF THE INVENTION
[0056] The present invention makes use of spin polarized electron transport at ferromagnetic—non ferromagnetic interfaces, a phenomenon which is well known in the art. Further details on this topic can be found in the above mentioned articles and journals, as well as in Johnson, Phys. Rev. Lett. 70, 2142 (1993), all of which are incorporated by reference herein. Moreover, further details on the structure and operation of the general bipolar magnetic spin transistor shown in FIG. 4 can, be found in the above reference pending applications Ser. Nos. 08/425884 and 08/493815, which are also incorporated by reference herein.
[0000] Spin Injected FET Memory Element
[0057] A preferred embodiment of the invention is illustrated in FIG. 1 . A spin injected FET 100 can be created from applying spin injection techniques to a high mobility semiconductor system (refer to FIG. 4 ). A ferromagnetic film F 1 110 at the source S provides spin polarized carriers to a high mobility channel 112 , the conductance of which is determined by a gate voltage, V G 114 . A ferromagnetic film F 2 116 at the drain D presents a spin sensitive impedance to current flow, so that the device conductance is high when the magnetizations {circumflex over ( )}M s and {circumflex over ( )}M d of source and drain are aligned parallel and low when {circumflex over ( )}M s and {circumflex over ( )}M d are antiparallel. If the magnetization 118 of one of the films, e.g. F 1 , is set in the “up” orientation [left to right in FIG. 4 , i.e., in a direction substantially perpendicular to the axis of channel 112 ], then the resistance of the device has two distinct states determined by the magnetization orientation 120 of F 2 : “up” (pointing to the right, equivalently LOW or “0”) or “down” (pointing to the left, equivalently HIGH or “1”) corresponds to LOW or HIGH channel resistance from source to drain (or vice versa). Thus, FET 100 can be used as a non-volatile memory element. Moreover, it will be apparent to skilled artisans that through use of selected materials, the magnetization orientation 120 in general can be set to any one of n distinct states, thus permitting a logical data item having n possible unique values to be stored in the memory element.
[0058] A logical data value (such as a binary bit value corresponding to a 0 or 1) can be written by using the magnetic fields from current pulses in overlaid write lines (illustrated in more detail in FIG. 7A ), to orient {circumflex over ( )}M d either up or down. The stored information is nonvolatile, and is isolated from the array because the conductance of the channel also has two states: approximately zero conductance (infinite impedance) in the “off” state when no gate voltage is applied (e.g. for an enhancement mode FET), and high conductance in the “on” state when a suitable voltage is applied to the gate.
[0059] The stored bit is read by sending a read voltage pulse 114 to gate 122 , addressing the element by raising the conductance of the channel and setting the FET to the “on” state, biasing source 190 with a read voltage V R 124 , and then sensing the source-drain conductance, discriminating between two values that differ because of the spin-dependent conductance (resistance) of the drain.
[0060] The variable (2 state) resistance of the FET can therefore be used to indicate the presence of a logical “1” or “0” data bit stored as the state of the FET. The variable resistance of the FET can be explained and modeled by the following analysis: If ferromagnetic films F 1 118 and F 2 120 are spaced (edge to edge) within a distance L of the order of a few electron mean free paths l, L˜l, and if spin accumulation effects are weak (˜M is small), then the current transport in the geometry of FIG. 4 is described by the density of state diagrams of FIG. 5 . Typical values l are the order of 0.1 micron, and the preferred value of L is the order of 1 micron. For the case of negligible spin accumulation, the difference of resistance for the cases where {circumflex over ( )}M 1 and {circumflex over ( )}M 2 are parallel, R par , and where {circumflex over ( )}M 1 and {circumflex over ( )}M 2 are antiparallel, R anti , relative to the total resistance between F 1 and F 2 , R ave , is equal to:
R anti −R par =(2η 2 *R av )/(2−η 2 )
where η is the polarization efficiency of F 1 and F 2 . This result also assumes that L is smaller than a spin-flip mean free path Λ=ν F *T 1 , where ν F is the Fermi velocity and T 1 is the mean time that an electron remains polarized within the channel.
[0061] For the case that N is the conducting channel of an FET or a 2 dimensional electron gas (2DEG), the results expressed above describe a channel resistance whose value depends on the relative orientation of the magnetizations of the ferromagnetic films, and this variable resistance is useful for implementing a spin injected FET as a memory cell or logic gate.
[0062] A more detailed look at the structure of a preferred embodiment of a spin injected FET, where spin injection is incorporated into an enhancement mode FET, is depicted in a top view in FIG. 6A and in a cross-sectional view in FIG. 6B . Two regions of high conductance material 212 having an approximate thickness of 100 nm are incorporated into the surface of a p-type silicon substrate 204 . The high conductance material can be a highly n-doped region of the Si, a metallic or polysilicon layer, an epitaxial layer of high mobility semiconducting material [such as InAs], a metallic layer diffused into a doped region of the substrate, or any other material with similar electrical properties. One function of the high conductance layer 212 is to diminish (or eliminate) the Schottky barrier that typically exists at the interface between a (ferromagnetic) metal and a semiconductor, and thereby improve the ohmic contact between the source 220 (or drain 230 ) and conducting channel 208 . By improving the Ohmic contact, spin transmission between source 220 (or drain 230 ) and channel 208 are enhanced (i.e. a the value of η is increased). Another function of the high conductance layer 212 is to shorten the length L c of the channel 208 . Thus, the source 220 and drain 230 may be separated, edge to edge, by 1 micron, and the high conductance layer may extend 0.2 micron from the edge of the source 220 and drain 230 so that the length of the channel is reduced to L c =0.6 micron. Finally, it will be understood to those skilled in the art that the high conductance layer 212 is most effective in silicon based devices. There are alternative materials systems, such as Indium Arsenide—Indium Antiminide heterostructures, where ohmic contact between the ferromagnetic source 220 (or drain 230 ) and channel ( 208 ) is intrinsically good and no highly conducting layer is required. Even in silicon based devices, the highly conducting layer is not theoretically necessary, but it is likely that its presence enhances device performance by an important measure. In other words, it is likely that a Schottky barrier randomizes the spin orientation of the polarized current so effectively that the resulting polarization values are so small as to make the device impractical.
[0063] An insulating layer 202 (silicon dioxide, polyimide, etc.), 40 nm thick coats a portion of a p-type silicon substrate 204 , overlapping a portion of the conductive material 212 . A thin film of highly conducting material 206 (metal or polysilicon) approximately 0.7 microns wide is fabricated over the insulator to a thickness of 60 nm and can operate as a gate: in this embodiment, a positive voltage applied to the gate draws charge carriers to the surface of the substrate and increases the conductivity of a channel 208 near the insulator—substrate interface, beneath the gate, allowing current flow between the two high conductance regions 212 when a bias voltage is applied between source 220 and drain 230 . Those skilled in the art will appreciate that this is essentially the same gating operation as that typically used in an enhancement mode FET, where the high conductance regions are doped, n-type silicon. Moreover, while the preferred embodiment is shown to be an enhancement mode FET, it will be apparent to those skilled in the art that the present invention can be used with any general FET geometry, including those having lightly doped source/drains, vertical topologies, etc.
[0064] A second insulating layer 210 , deposited to a thickness of approximately 50 nm covers the gate to isolate it during subsequent processing steps. A thin ferromagnetic film 220 [e.g. of permalloy, cobalt, iron a Heusler alloy or Fe 0.5 Co 0.5 ] which is 60 nm thick (film 220 may be coated by a 10 nm thick layer of nonmagnetic metal, such as Ti or Au, in order to prevent oxidation) is deposited on one side of the gate making ohmic contact with highly conductive layer 212 in the region of a via hole 222 . This film 220 can be considered as a ferromagnetic “source” of the spin injected FET. A metallic strip 224 (or similar conductor) approximately 100 nm thick overlaps the ferromagnetic film 220 and is also connected to a read or bias line. As described above, ferromagnetic source 220 is chosen [by choice of material, exchange bias, or induced magnetic anisotropy] to have a relatively large coercivity H c,1 with an easy magnetization axis parallel to {circumflex over ( )}z. During device operation, the magnetization is set initially in the up orientation [or, alternatively, down] along +{circumflex over ( )}z, and the magnetization in source 220 typically remains in that orientation during all device operations. The shape of source 220 in FIG. 6A is chosen to be a crescent so that fringe fields from magnetic poles at the ends of the film are kept far from the gate region. Those skilled in the art will appreciate that other geometries that minimize stray fields in the region of the gate work equally well.
[0065] A second thin ferromagnetic film 230 [of permalloy, cobalt, Fe 0.5 Co 0.5 , etc.] is deposited to a thickness of 70 nm on the other side of the gate making ohmic contact with the highly conductive medium in the region of a via hole 232 . This film 230 can be considered as a ferromagnetic “drain” of the spin injected FET. A metallic strip 234 (similar in composition and thickness to strip 224 ) overlaps the ferromagnetic film 230 and is also connected to a bit line. Ferromagnetic drain 230 is chosen [by choice of material or induced magnetic anisotropy] to have a small coercivity, H c,2 <H c,1 , with a relatively easy axis parallel to {circumflex over ( )}z.
[0066] During device operation, the orientation of the magnetization of the drain can be set by an overlaid set of write lines, depicted schematically in FIG. 7A . In a write procedure, sending a write current pulse 310 of positive [negative] polarity and magnitude 2 mA down write line 312 (located approximately 50 nm away from drain 116 ) generates a magnetic field 314 at the drain 116 and orients (sets) the magnetization state 120 of the drain to be up (or down), parallel (or anti-parallel) relative to the orientation 118 of the source 110 . While the write line is described as a “line” it will be understood by persons skilled in the art that any number of well-known structures capable of carrying sufficient current (including for example a conductive film, or an interconnect line) to generate the field H will be suitable in the present invention. Moreover, while not essential to the description of the present invention, additional details concerning the operation of read/write lines in connection with ferromagnetic layers can be found in the aforementioned pending application Ser. Nos. 08/425884 and 08/493815.
[0067] Under these conditions therefore, the spin injected FET has two settable and stable states, determined by whether magnetization orientation 118 of drain 116 is up or down (parallel or anti-parallel relative to the magnetization orientation 120 of source 110 ), which states can correspond to a stored “bit” of data (i.e, 0 or 1). Moreover, when no voltage is applied to gate 122 , channel 112 has a high electrical impedance [e.g. for an enhancement mode FET] and no spin polarized current can flow from source 110 to drain 116 . The stored bit of information is thus nonvolatile, and is isolated from the memory array by the high resistance of channel 112 .
[0068] In a read process, a positive voltage V G 114 is applied to gate 122 , channel 112 has a relatively high conductance and a bias voltage V R 124 causes current to flow from source 110 to drain 116 . The electric current which flows is comprised of spin polarized electrons which enter the highly conductive material 212 (refer to FIG. 6B ). Since the dimensions of the highly conducting material 212 , extending about 0.2 micron past the edge of the source 220 and to a thickness of about 0.1 micron, are much smaller than the characteristic spin diffusion length δ s,1 (estimated to be about 1 micron) in the highly conductive material, the current that enters the channel 208 retains a large fraction of its initial spin polarization. Furthermore, the preferred orientation of the magnetization of the source is along +{circumflex over ( )}z (or −{circumflex over ( )}z); the injected spins will be oriented along the {circumflex over ( )}z axis and will not precess under the influence of gate voltage V G ( 114 in FIG. 7A ). The presence or lack of precession (more accurately, enhanced versus diminished precession) is an operational difference between the Datta/Das device and the present invention. As described above, the electronic source-drain conductance will have two different values for the two different states (0 or 1) of the device, with parallel or antiparallel magnetization orientation, so the quantity of spin polarized current which flows will be a function of this conductance. The readout operation is completed by sensing the source-drain conductance and discriminating between the two possible current values. It will be apparent to those skilled in the art that a ferromagnetic drain (or source) can be fabricated with n stable magnetization states, and the operation of the 2-state device described herein can be generalized to operation of an n-state device.
[0069] An example of sensing the logical data state of a spin injected FET used as a single element memory cell, is depicted in FIG. 7B . Source 110 is connected to a common read [or bias) line at a terminal 354 , gate 122 to a common word line at a terminal 364 , and drain 116 to a common bit line at a terminal 374 . At the end of the bit line is a sense circuit 380 which compares the readout of the cell with a reference voltage [internally or externally supplied]. A word line voltage applied to gate terminal 364 selects the cell for reading. A read line voltage is simultaneously applied to source terminal 354 . As suggested above the source—drain current has one of two values, determined by the two conductance values of the spin injected FET in series with resistance R 390 at the end of the bit line. These two current values in turn can develop two different voltage values at the top 384 of resistor 390 and at an input 386 of a sense amplifier 380 . This voltage value is compared with a reference voltage thus the logical value stored in the cell is interpreted as a logical “1” or a “0.”
[0070] To form a memory array, a number of spin injected FET memory cells can be configured as depicted in FIG. 7C . Here each spin injected FET is drawn with a symbol for a conventional semiconductor FET with an additional arrow representing a variable resistance value, referring to the two resistance values when the FET is in the “on” state. Write line 312 is included for each spin injected FET, in the symbol, to the side of the drain. A single sense circuit 380 is common for all the cells in the array. Each cell is isolated from the array, and its value is sensed only when addressed. For example, cell 400 is sensed only when addressed by a pulse applied to its gate 122 . Finally, while not shown or discussed explicitly herein, it will be apparent to those skilled in the art that additional peripheral and support circuits commonly associated with semiconductor memory arrays (decoders, buffers, latches, equalization, precharge, etc) can be easily adapted for use with the present invention.
[0071] The spin injected FET is an improvement over DRAM because the memory cell has a single element so that packing densities can be greater. It also has superior signal to noise ratio, and the memory is nonvolatile so that the array draws substantially less power. The spin injected FET is an improvement over other nonvolatile technologies because the cell is simpler, packing densities are greater, signal to noise is superior, and isolation from the array is more efficient.
[0072] The device may also be used as a field sensor, e.g. in a recording head. Note that the readout voltage can be increased by varying parameters such as the type of ferromagnetic material and thickness. For example, iron films have approximately twice the saturation magnetization as permalloy, and substituting iron for permalloy would double the magnitude of the readout voltage.
[0000] Spin Injected FET as Logic Gate
[0073] Boolean logic processes can also be performed using the present spin injected FET. For example, a logic input having two logical data values can be represented by two different current levels on a data wire. This logical input (having a particular current level corresponding to a “1” or “0”) can be combined with a second logical input (also having a current level corresponding to either a “1” or “0”), and the combined sum of the current levels of these logical inputs then can be applied to a write line coupled magnetically to a ferromagnetic layer of the FET (source or drain). The sum of these logic inputs constitutes a write current pulse in the write line and a corresponding magnetic field acts inductively on the magnetization state {circumflex over ( )}M of the ferromagnetic layer. Depending on the state of the orientation {circumflex over ( )}M of the ferromagnetic layer, and the particular combination of inputs therefore, the magnetic field of the write current pulse may alter this orientation, thus “storing” the result of the logic operation in the form of a new magnetization orientation in the ferromagnetic layer. Again, while not essential to the description of the present invention, additional details concerning structures and circuits usable in connection with magnetic spin transistor boolean logic processing devices can be found in the aforementioned pending application Ser. No. 08/493815.
[0074] Those skilled in the art will appreciate that this principle can be extended to create an N input logical AND gate or similar logic processor. For example, a logic processing device can be implemented wherein the magnetization state of the drain of the FET is set so that it can only altered when all N inputs are a “high” current level, thus generating a sufficiently high magnetic field to change the orientation of the FET ferromagnetic layer. Other configurations for adapting other boolean processes will be readily apparent to skilled artisans.
[0075] The result is automatically stored as a boolean function data value and can be read out at any later time. In this way the spin injected FET can function as a logic gate with memory capability. If the readout operation enables the result (“0” or “1”, HIGH or LOW) to be transmitted to another gate for another operation, then gates can be linked together to perform combinational tasks of digital processing. An example of an appropriate readout technique is presented in FIG. 8 . Readout circuit 410 amplifies an output to an appropriate CMOS level (HIGH or LOW) so that it can be integrated with CMOS (or, for an appropriate circuit, TTL) logic. Alternatively, the output can be sent to the write line of another spin injected FET gate.
[0076] The example is presented for the case of an n-channel enhancement mode spin injected FET. Other devices (depletion mode, p-channel, etc.) can be fabricated incorporating ferromagnetic layers and constructed and operated in a similar way readily apparent to those skilled in the art. As seen in FIG. 8 , a spin injected FET 400 has two resistive values in the “on” state, R s =R′±ΔR. In a real MOSFET device, R′ may typically have a value R′=100 Ω, and the spin dependent resistance may vary by 15% so that R s =85, 115 Ω are the LOW and HIGH resistive values of the device. Typically readout resistor R 390 would be matched to the value R′, and the bias voltage would have the value V DD =15 Volts. In readout circuit 410 , FET Q 1 412 can be a p-channel enhancement mode FET whose body is biased to a relatively high value, V 1 =8.1 Volts. FET Q 2 414 is an n-channel enhancement mode FET whose body is biased to a relatively low value, V 2 =7.0 Volts. The bias can be provided by an external voltage source, appropriate doping or other methods known in the art.
[0077] When R s is LOW (85 Ω), the voltage at input node 416 to readout circuit 410 is relatively HIGH (8.1 V). In this situation, Q 1 412 is “off”, Q 2 414 is “on” and output 418 is clamped LOW (ground). When R s is HIGH (115 Ω), the voltage at input 416 to readout circuit 410 is relatively LOW (7.0 V). In this case, Q 1 412 is “on”, Q 2 414 is “off” and output 418 is clamped HIGH (V DD ). Readout circuit 410 thus functions to convert the input levels to conventional CMOS output values (GND and V DD ).
[0078] When the elements of FIG. 8 are considered as a single logic function (AND) gate, the number of constituent elements is three, only half the size of the typical CMOS gate, and therefore packing densities of logic gates can be increased. The result of the logic operation is automatically stored as a nonvolatile state. Since no additional memory cell is needed to store the result, further increases of density (and operating speed) are achieved. Furthermore, it is possible to associate a single readout driver circuit with several spin injected FETs. Each of the latter can perform a simple programmed Boolean operation and store the result in a non-volatile manner. At any desired time, the results of these operations can be called in any sequence. Thus, the spin injected FET can function as a general purpose element of a programmable logic array, or gate array. Again, typical support circuits known in the art and associated with such programmable logic arrays can be used to augment and enhance the performance of circuits embodying the present invention.
[0079] Although the present invention has been described in terms of a preferred embodiment, it will be apparent to those skilled in the art that many alterations and modifications may be made to such embodiments without departing from the teachings of the present invention. For example, while not shown or discussed explicitly herein, it will be apparent to those skilled in the art that additional peripheral and support circuits commonly associated with semiconductor memory arrays (decoders, buffers, latches, equalization, precharge, etc) can be easily adapted for use with the present invention. Moreover, while the preferred embodiment is shown to be an enhancement mode FET, other active devices (depletion mode, p-channel, etc.) can be fabricated using well known techniques to include the teachings of the present invention.
[0080] Furthermore, other suitable FET orientations and geometries, including those having lightly doped source/drains, vertical topologies, etc. can be used with the present invention.
[0081] In addition, it will be apparent to those skilled in the art that a device can be constructed in a stacked fashion, i.e., having multiple levels of the memory cells or logic gates of the present invention. This can be accomplished merely by adding a passivating layer or similar insulating layer between such levels, along with appropriate conventional interconnect and peripheral support circuits. Thus, a device constructed in this manner can have even greater integration advantages over prior art.
[0082] Accordingly, it is intended that the all such alterations and modifications be included within the scope and spirit of the invention as defined by the appended claims.
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Ferromagnetic elements for use with spin memories, logic devices and processing circuits include a geometry incorporating an asymmetry about one axis and in some instances one or more curved sections. Magnetic memory elements can be set out in an array such that convex and concave portions are also optimally arranged about magnetization axes.
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BACKGROUND OF THE INVENTION
The present invention relates to thin film electroluminescent phosphor material.
Thin films of rare earth doped alkaline earth sulfides such as cerium doped strontium sulfide have been extensively investigated for applications in full color alternating current thin film electroluminescent (ACTFEL) display devices. Such a device is disclosed by Barrow et al., U.S. Pat. No. 4,751,427, incorporated by reference herein. The emission spectrum of SrS:Ce is very broad covering both blue and green portions of the visible spectrum, i.e., 440 to 660 nm with a peak at around 500 nm. A full color ACTFEL display device can be obtained by adding a red emitting phosphor, for example CaS:Eu or one that has a red component in its emission spectrum. With such a combination of films, one can build a white light emitting phosphor stack. White phosphor structures can then be laminated with primary color filters to build a color display which is very cost effective in terms of production.
With white light emitting phosphor stacks, however, the blue portion of the emission spectrum can be rather weak, particularly strontium sulfide phosphor doped with cerium which in the past has been one of the most promising of the blue emitting phosphors. Only about 10% of the original luminance can be obtained after filtering if a nearly blue color is to be achieved. For blue coloration in the CIE range of x=0.10, y=0.13 the transmission ratio is further reduced to only about 4%. Therefore, to produced a color display with acceptable luminance, it is necessary to use a lighter blue color filter but this in turn leads to a compromised blue chromaticity. Any display fabricated with such a poor blue chromaticity has a limited color gamut and is unable to produce the range of colors available with CRT or LCD technology.
Therefore, in order to achieve a high performance color ACTFEL display, the blue emission efficiency of the electroluminescent phosphor thin film must be greatly improved. In U.S. Pat. No. 4,725,344, Yocom et al., a method is disclosed for forming alkaline earth sulfide luminescent films by chemical reaction between alkaline earth metal halide and hydrogen sulfide on heated substrates. Yocom et al. does show a strontium sulfide thin film phosphor which has a more bluish color (CIE x=0.17, y=0.25) than an unfiltered SrS:Ce device. However, the luminance performance of the Yocom et al. device is not high enough for practical application. Experimentation has also been reported regarding SrS:Cu devices which are prepared by sputtering, for example in Ohnishi et al., proceedings of the SID 31/1, 31 (1992). The Ohnishi et al. device, however, is even dimmer than the Yocum et al. device (and no color data is available).
Higton et al., U.S. Pat. No. 4,365,184, disclose what is generally known in the art as a powder electroluminescent device. The construction of a powder electroluminescent includes a pair of electrodes with a phosphor layer interposed therebetween. The phosphor layer is a thick film, generally having a thickness of 25 microns or more, which is normally applied in a manner similar to paste. Powder electroluminescent devices are illuminated using a direct current. The use of a direct current between the electrodes is necessary because the powder phosphor layer, as taught by Higton et al., is a semi-insulative material and a large net direct current flow is required for illumination. The core of each phosphor particle is coated, or otherwise formed, with a resistive layer injects carriers into the powder and a much lower average electric field strength than tunneling fields required for the operation of thin film alternating current electroluminescent devices, as previously described. This resistive current then excites the activator atoms in the powder phosphor to emit light. Unfortunately, the characteristics of the resistive layer changes during extended usage which raises its threshold voltage. The increase in the threshold voltage thereby decreases the brightness of the display. If the resistive layer surrounding the particles were removed then the phosphor layer would act as a short circuit rendering the device ineffective. In contrast to ACTFEL devices, the use of an AC signal on a direct current powder device, as taught by Higton et al., would not impose a sufficient voltage on the particles for illumination. Further, if an AC voltage was applied to the powder electroluminescent device disclosed by Higton et al. the efficiency of the device would be extremely low because of the resistance layer. Because of the different operating principles between powder devices and ACTFEL devices, together with different phosphor material characteristics (resistive layer and thickness), one would not consider powder phosphors suitable for thick-film powder devices disclosed by Higton et al. suitable for an ACTFEL device.
Lehmann, in a paper titled “Alkaline Earth Sulfide Phosphorous Activated by Copper, Sulfur, and Gold,” reported that strontium sulfides doped with monovalent ions with a d 10 configuration, e.g., Cu + and Ag + , emit green and blue light, respectively, when excited by an electron bombardment. Lehmann was attempting to develop a powder cathode phosphor material suitable for cathodo ray tube devices. Such phosphor powder materials are considered unsuitable for alternating current film electroluminescent devices, such as the device disclosed by Barrow et al.
Vecht et al., in a paper entitled “DC Electroluminescence in Alkaline Earth Sulfides” disclose a powder direct current electroluminescent device using a SrS:Cu powder where the emission is a green color. Like Higton et al., such a phosphor is not suitable for alternating current thin film electroluminescent devices.
Sun et al., U.S. Pat. No. 5,309,070, disclose a (Sr,Ca)Ga 2 S 4 :Ce phosphor for an ACTFEL device. Such a phosphor offers a saturated blue color, e.g., (CIE x=0.15, y=0.10-0.20), but the luminous efficiency is poor, e.g., e40=0.02-0.03 lm/W. In addition, it is extremely difficult to fabricate such a composition as a thin film with good crystallinity at reasonable low substrate temperatures due to its complex chemistry.
A blue emitting SrS:Cu electroluminescent phosphor for alternating current thin-film electroluminescent devices was reported by Kane et al. in a paper entitled “New Electroluminescent Phosphorous Based on Strontium Sulfide.” However, the device taught by Kane et al. has a poor performance, e.g., less than 1.0 cd/m 2 at 60 Hertz.
Sun et al., in a paper entitled “A Bright and Efficient New Blue TFEL Phosphor,” developed a phosphor, namely, SrS:Cu, with an increased luminous performance over the prior known blue phosphors.
Velthaus et al., in a paper entitled “New Deposition Process for Very Blue and Bright SrS:Ce,Cl TFEL Devices,” disclose the use of silver as a co-doping 25 material for SrS:Ce,Cl thin-film electroluminescent devices. Velthaus et al. suggest that the silver co-doping improves the emission spectrum of SrS:Ce electroluminescent devices to a more bluish color. The improvement was attributed to the effect of the Ag + charge compensation for the Ce 3+ to eliminate the Sr 2+ vacancies. The mechanism can be thought of as the cerium 3+ replacing the strontium 2+ cites leaving an extra positive charge left over. The strontium vacancies, which are defects, degrade the crystallinity and cause a red shift of the emission which results in a more greenish color. Velthaus et al.'s theory is that silver which has a single positive charge added to the phosphor as a co-dopant averages out the cerium to result in a net average charge of 2+ to provide charge compensation. In this way, the emission spectrum is shifted toward blue from what it would otherwise have been without the silver. However, SrS:Ag is not recognized by those designing phosphors suitable for alternating current thin film electroluminescent devices as being an efficient phosphors since its cathodoluminescent efficiency is poor when compared to that of SrS:Cu, e.g., 1% for SrS:Ag versus 10-15% for SrS:Cu. In other words, the silver acts to fill in the holes but is not considered a light-emitting dopant.
Thus, to date producers of thin film electroluminescent devices have yet to produce a blue emitting phosphor having sufficient luminance for use in a full color ACTFEL device.
SUMMARY OF THE INVENTION
The luminance of a blue light emitting phosphor is substantially improved according to the present invention which includes an ACTFEL device having front and rear electrode sets, a pair of insulators sandwiched between the front and rear electrode sets, and a thin film electroluminescent laminar stack which includes a phosphor layer having the formula M II S:Cu,Ag where M II is taken from the group calcium, strontium, barium, and magnesium, S=sulfur, Cu=copper, and Ag=silver.
Preferably the phosphor laminate stack is annealed at between 550° and 850° centigrade prior to deposition of the top insulator layer. The M II S:Cu,Ag layer includes concentrations of dopants as follows: the primary dopant Cu should be between 0.05 and 2 mol %; and Ag should be between 0.05 and 2 mol %. Additional phosphor layers in the electroluminescent laminate stack may be of materials that produce red and green light, respectively, so that the laminate stack as a whole produces “white” light. The layers in the EL phosphor laminate stack may be deposited by sputtering, atomic layer epitaxy, evaporation, and MOCVD. The preferred formulation for the M II S:Cu,Ag layer is SrS:Cu,Ag. This device produces a blue emitting phosphor device having a broad band emission spectrum capable of producing a deep blue color and having a much greater luminance efficiency than the best available blue emitting phosphor to date.
The foregoing and other objectives, features, and advantages of the invention will be more readily understood upon consideration of the following detailed description of the invention, taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWING
FIG. 1 is a partial side cutaway view of an ACTFEL device constructed according to the invention.
FIG. 2 is a partial side cutaway view of an alternative embodiment of an ACTFEL device made according to the invention.
FIG. 3 is a graph illustrating the spectral characteristics of sample blue emitting phosphor of the invention.
FIG. 4 is a graph of the PL spectra of SrS:Cu,Ag thin film at 10 and 300K.
FIG. 5 is a graph of the thermal quenching of PL for SrS:Cu,Ag thin film.
FIG. 6 is a graph of the PLE spectra of SrS:Cu,Ag and SrS:Ag thin films at 10K.
FIG. 7 is a graph of the PL decay of the 2.87 eV (430 nm) and 2.398 eV (517 nm) emission of SrS:Cu,Ag.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring to FIG. 1, an alternating current thin-film electroluminescent device 10 includes a glass substrate 12 onto which is deposited a layer of indium tin oxide (ITO) 14 . An insulator layer 16 comprising an aluminum/titanium oxide is deposited on the ITO 14 . A phosphor layer 18 includes a thin film of SrS:Cu,Ag. The phosphor layer 18 is sandwiched by a second insulator 20 preferably made of barium tantalate (BTO). Aluminum electrodes 22 are placed atop the BTO layer 20 . The first insulator layer 16 is preferably approximately 260 nanometers thick and is deposited by atomic layer epitaxy (ALE). In an alternative embodiment, either dielectric (insulator) layer 16 or 20 could be removed. The electroluminescent phosphor layer 18 is preferably 600 nanometers to 2 micrometers thick and is deposited by sputtering from an SrS target prepared with the following doping concentration: copper, 0.05 to 2.0 mol %; and silver 0.05 to 2.0 mol %. To make a full color panel, a second phosphor layer such as ZnS:Mn or other red and green emitting phosphor (not shown in FIG. 1) may be deposited on the layer 18 . During deposition, the substrate temperature is held to between 75° and 500° C. The phosphor films are then annealed at 550° to 850° C. in nitrogen. This is followed by the deposition of the second insulator layer 20 which is preferably 300 nanometers of ATO. The top aluminum electrodes 22 complete the device fabrication. Red, blue, and green inorganic filters may be interposed between the bottom electrode layer 14 and the viewer (not shown) to provide a filtered full-color TFEL display.
FIG. 2 shows an “inverted” structure electroluminescent device 40 that is similar to FIG. 1 for making a color TFEL display. The device 40 is constructed with a substrate 44 that preferably has a black coating 46 on the lower side if the substrate 44 is transparent. On the substrate 44 are deposited rear electrodes 48 . Between the rear electrodes 48 and the rear dielectric layer 50 is a thin film absorption layer 42 . The absorption layer is either constructed of multiple graded thin film layers or is a continuous graded thin film layer made by any appropriate method. An electroluminescent layer 52 which may be a laminated structure including at least one layer having the formula M II S:Cu,Ag and layers of red and green emitting phosphor, e.g., ZnS:Mn, ZnS:Tb or SrS:Ce, is sandwiched between a rear dielectric layer 50 and a front dielectric layer 54 . In an alternative embodiment, either dielectric layer 50 or 54 could be removed. A transparent electrode layer 56 is formed on the front dielectric layer 54 and is enclosed by a transparent substrate 58 . The substrate 58 may include color filter elements 60 , 62 and 64 filtering red, blue and green light, respectively, for making a color TFEL display.
The electroluminescent phosphor layer has a chemical composition primarily consisting of SrS:Ag,Cu. To assist in forming a high quality crystal structure Ga may also be added. The phosphor layer may be deposited by any suitable method, such as one of the two methods described below. The first method is to deposit a multilayer stack of SrS:Cu,Ga and SrS:Ag,Ga sub-layers from two singly doped targets each having about 0.05 to 2.0 mol % Cu or Ag and 0.5 to 10 mol % Ga. The film stack is then post annealed at 550 to 850 C in nitrogen. During annealing, the Cu and the Ag diffuse out of the sub-layers and become intermixed uniformly throughout the stack. The second method is to deposit films from targets already doped with Cu and Ag. The targets have a typical doping concentration of Ag: 0.05 to 2.0 mol %, Cu:0.05 to 2.0 mol % and Ga:0.5 to 10 mol %. The role of Ga is to act as a flux to improve the crystalline quality of SrS films by post annealing at 550 to 850 C in nitrogen as described in U.S. Pat. No. 5,677,594.
The present inventor tested a SrS:Cu ACTFEL device which was very efficient as previously noted, e.g., luminance measured at 40 V above threshold driven at 60 Hz (L 40 @60 Hz) was close to 35 cd/m 2 with a greenish blue color, CIE x=0.16, y=0.28. The present inventor also tested a SrS:Ag ACTFEL device which as expected was inefficient, e.g., L 40 @60 Hz<0.5 cd/m 2 . On the other hand, devices with doubly doped SrS:Cu,Ag exhibited a deeper blue color and a higher radiative efficiency than singly doped SrS:Cu devices. The effect of Ag doping concentration on the electroluminescent emission spectra of SrS:Cu,Ag is shown in FIG. 3 . FIG. 3 shows the luminance intensity of the 480 nm peak was greatly increased with just a small addition of Ag. At higher Ag concentration, the emission peak actually shifted to 430-440 nm. The ACTFEL devices made with an Ag concentration of 0.6 at 3% exhibited a saturated blue color, e.g., CIE x=0.17, y=0.13, with excellent luminance and luminous efficiency, e.g., L 40 =20 cd/m 2 , and e 40 =0.15 lm/W. The latter phosphor is nearly five times of those measured in the best (Sr,Ca)Ga 2 S 4 :Ce device with the same deep blue color. It is also possible to achieve the same high luminance as singly doped SrS:Cu devices, e.g., L 40 =34 cd/m 2 , while still retaining most of the blue color, e.g., CIE y=0.20, by slightly reducing the Ag concentration in SrS:Cu,Ag devices. This represents a 30 percent improvement in the luminance efficiency of SrS:Ag,Cu over SrS:Cu devices. The following two tables summarize its performance.
TABLE 1
Blue EL Phosphor Luminance Performance
L 40
Relative
Phosphor
@60 Hz
e 40
Radiative
Materials
(cd/m 2 )
(lm/W)
Efficiency
CIEx
CIEy
SrS: Ag, Cu
20
0.15
1.15
0.15
0.13
35
0.24
1.14
0.16
0.21
SrS: Cu
35
0.24
0.89
0.16
0.27
SrS: Ce/
6
0.04
0.29
0.09
0.14
filter
SrCaGa 2 S 4 : Ce
5
0.03
0.21
0.15
0.14
TABLE 2
Ag Conc.
L 40 @60 Hz
e 40
(at %)
(cd/m 2 )
(lm/W)
CIEx
CIEy
0.0
34
0.24
0.17
0.28
0.2
32
0.24
0.18
0.26
0.3
34
0.27
0.17
0.25
0.4
35
0.24
0.16
0.21
0.5
28
0.20
0.17
0.16
0.6
20
0.15
0.17
0.13
0.7
Burn Out
Table 2 details the effect of Ag doping concentration on the EL performance of SrS:Ag,Cu devices (Cu concentration was kept roughly constant at 0.2%-0.3%).
The level of blue shift in SrS:Cu,Ag devices, e.g., >0.3 eV, is too large to be explained by the suppression of Cu + aggregate formation from Ag + co-doping. It is more likely that the Ag + centers have become EL effective in these devices and gave an emission band peaked at 430 nm, however, the exact mechanism is not clear at this moment. One possible explanation is that Cu + and Ag + ions might have formed an effectively coupled center that the excited Cu ions are able to transfer the energy to Ag + ions and allow effective Ag + emission to occur. The energy transfer channel has been identified in a photoluminescent (PL) study described in detail later. It is shown that there is a common absorption band at 4.46eV in PL excitation spectra of SrS:Cu, SrS:Ag, and SrS:Ag,Cu. The absorption band is greatly enhanced in SrS:Ag,Cu when compared to singly doped films, suggesting this band could be the pathway for energy transfer. It is understood that other activators with the same optical characteristics as Cu could also be used to activate Ag blue emission in SrS and achieve even more luminance and efficiency enhancement.
A detailed analysis of the spectroscopic investigations on SrS:Cu,Ag thin film phosphors grown by standard magnetron sputtering technique revealed the following. The PL spectra at 10K and 300K are shown in FIG. 4 . The film exhibited a deep blue color at 300K with a peak position at 2.876 eV (431 nm) and a linewidth of 390 meV, providing a blue CIE color coordinate of (x=0.165, y=0.088). As the temperature was decreased to 10K, the emission band did not show any substantial shift but the linewidth was decreased to 215 meV. At low temperatures, two additional emission bands were also observed at 3.443 eV and 2.398 eV. By comparing with the low temperature PL spectra of SrS:Cu and SrS:Ag, the present inventor has assigned the two peaks at 3.443 and 2.876 eV to Ag + emission and the 2.398 eV peak to Cu + emission. This assignment was supported by the temperature dependence of these three emission bands. The two Ag emission bands did not show any shift with temperature whereas the Cu emission exhibited a large blue shift with increasing temperature. The behaviors were consistent with those observed from singly doped SrS:Ag and SrS:Cu. The enhancement of the 2.876 eV Ag emission and the simultaneous suppression of the Cu emission suggested energy transfer from Cu to Ag. As shown in FIG. 5, the main emission band also exhibited thermal quenching as the temperature was increased. At room temperature, the PL intensity was reduced to about 45% of that at 10K, which is indicative of thermally activated non-radiative processes. The main emission band also exhibited thermal broadening from which a phonon energy of 17 meV was obtained. From this phonon energy and low temperature linewidth, the Huang-Rhys parameter was calculated to be about 19. The strong electron-phonon coupling indicated by the large value of Huang-Rhys parameter was consistent with the PL spectra which showed the absence of zero-phonon line and the broad linewidth at 10K. However, it is possible that more than one vibrational modes were involved in the broadening process which could result in an overestimation of Huang-Rhys parameter.
The low temperature PL excitation (PLE) spectra of the 3.443 and 2.398 eV emission bands were identical to those obtained from singly doped SrS:Ag and SrS:Cu samples, confirming the assignments of the 3.443 eV band being Ag + . FIG. 6 shows the PLE spectra of the main emission band at 2.876 eV along with that of SrS:Ag. The singly doped SrS:Ag exhibited two excitation bands at about 4.46 and 4.10 eV. In SrS:Ag,Cu, the 4.46 eV excitation band was significantly enhanced, exhibiting an additional shoulder feature at around 4.29 eV. These two main excitation bands around 4.46 eV suggested that the energy transfer from Cu to Ag take place through these bands.
FIG. 7 shows the PL decays of SrS:Cu,Ag. Under the resonant excitation of 4.46 eV excitation band, the 2.876 eV emission band exhibited a single exponential decay with a small non-exponential component at the beginning. The decay times for the fast component and the exponential component were determined to be 5 us an 28 us, respectively. As the excitation energy was changed to 4.00 eV, the decay of 2.876 eV (430 nm) emission changed little, indicating that the recombination process was not affected by the excitation energy. On the other hand, the 2.398 eV Cu emission band showed a very fast decay also highly non-exponential with an effective decay time of 9 us. This is in contrast to the slow decay observed in singly doped SrS:Cu, which had an effective decay time of 93 us. The observed fast decay for the Cu emission was indicative of efficient energy transfer fro Cu to Ag. When the excitation energy was changed to 4.0 eV at which energy Cu has a large excitation band, but for which Ag has no comparable feature, the decay of the 2.398 eV Cu emission band remained non-exponential with an effective decay time of about 80 us, which was much slower and close to singly doped SrS:Cu. Consistent with the PLE studies, these results clearly indicate that the energy transfer from Cu to Ag occurred through the 4.46 eV excitation bands and was not efficient when lower energy excitation band was excited.
The present inventor developed the SrS:Cu,Ag material in the following manner. The present inventor realized that SrS:Cu has a dim blue output at about 480 nm but desired a phosphor with greater luminescence. The present inventor has experienced difficulty fabricating thin films with high quality crystallinity of CaS:Cu which have a deeper blue at 430 nm than SrS:Cu. The present inventor when testing SrS:Ag noticed a good crystallinity and a blue output under ultraviolet light at about 430 nm. However, the luminescence output of SrS:Ag in an ACTFEL device is extremely low. With two unusable targets (SrS:Ag and CaS:Cu), one with a good blue output having poor crystallinity and the other with good crystallinity having good blue output under ultraviolet light, the present inventor attempted to mix the two to obtain a good blue output with good crystallinity. The shocking result of Ca,SrS:Ag,Cu was a superior blue color at 430 nm. The present inventor tried the combinations of CaS and SrS with Ag,Cu to determine which was the cause and determined that SrS:Cu,Ag was the best source of the superior blue output.
It is also understood that a broadband (white) emitting EL phosphor can be achieved by laminating SrS:Ag,Cu layer with a ZnS:Mn or other yellow or red/green emitting phosphor layer to produce white monochrome or color EL displays. The phosphor can be constructed using any suitable technique, such at sputtering, atomic layer epitaxy, and evaporation.
It is also understood that although the invention has been described primarily in terms of a conventional ACTFEL device which will be viewed with the glass substrate forming the face of a TFEL panel, the phosphor of the present invention may also be used in an inverted structure and viewed from the film side of the structure. In the latter case the first deposited electrode will be a refractive metal such as molybdenum.
The terms and expressions which have been employed in the foregoing specification are used therein as terms of description and not of limitation, and there is no intention, in the use of such terms and expressions, of excluding equivalents of the features shown and described or portions thereof, it being recognized that the scope of the invention is defined and limited only by the claims which follow.
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A light emitting phosphor having improved luminance is incorporated into an ACTFEL device which includes a phosphor layer having the formula M II S:Cu,Ag where M II is taken from the group calcium, strontium, barium and magnesium, S is sulfur, Cu is copper, and Ag is silver.
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CROSS REFERENCE TO RELATED APPLICATION
The present application is an application filed under the National Phase of and claims priority to PCT application entitled "Sinker Drive Mechanism" assigned Ser. No. GB97/00501 and filed Feb. 24, 1997, which PCT application claims priority to a patent application filed in Great Britain entitled "Sinker Drive Mechanism", assigned Ser. No. 96-03941.7 and filed Feb. 24, 1996, each of which describe inventions made by the present inventor and assigned to the present assignee.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a sinker drive mechanism, in particular but not exclusively for driving sinkers in a straight bar knitting machine.
2. Description of Related Art
In a straight bar knitting machine, sinkers are advanced after having received yarn in order to draw the yarn around the needle shanks prior to operation of the needles.
Conventionally, each sinker is advanced mechanically by a striking jack which is engaged by a slur cock which traverse across the back of the sinkers so as to advance each sinker in succession.
The mechanical action of a slur cock is noisy, relatively slow and requires continuous maintenance.
SUMMARY OF THE INVENTION
The sinker drive mechanism for a knitting machine includes a piston assembly for actuating the sinkers. The mechanism has valve means for advancing in succession each of a plurality of pistons of the piston assembly and disposed along the length of a support body to actuate the respective sinker. The valve means includes a piston head movable along a piston chamber within the support body to introduce pressure to each piston of the plurality of pistons and urge serial movement of the plurality of pistons with resulting actuation of the respective sinkers.
It is therefore a primary object of the present invention to provide an improved drive mechanism which overcomes drawbacks associated with conventional mechanical sinker drive mechanisms.
According to one aspect of the present invention there is provided a sinker drive mechanism including an elongate support body including a plurality of pistons spaced along its length, each piston being extendable to advance an individual sinker to an extended position.
According to another aspect of the present invention there is provided a knitting machine or weaving machine including a drive mechanism as defined above.
BRIEF DESCRIPTION OF THE DRAWINGS
Reference is now made to the accompanying drawings, in which:
FIG. 1 is a cross-sectional view through the knitting head of a conventional straight bar knitting machine;
FIG. 2 is a similar view to FIG. 1 showing a straight bar knitting machine modified in accordance with a first embodiment of the present invention;
FIG. 3 is a diagrammatic sectional view of a sinker drive mechanism according to the present invention;
FIG. 4 is a front view of the drive mechanism shown in FIG. 3;
FIG. 5 is a cross-sectional view taken along line V--V in FIG. 4;
FIG. 6 is a view similar to FIG. 3 of an alternative embodiment.
FIG. 7 is a schematic diagram of a multi-sectioned knitting machine;
FIG. 8 is a schematic diagram of a single sectioned knitting machine;
FIG. 9 is a similar view to FIG. 2 showing a straight bar mechanism according to a second embodiment of the present invention;
FIG. 10 is a similar view to FIG. 5 showing a modified embodiment according to the present invention;
FIG. 11 is a cross-sectional view taken along line XI--XI in FIG. 10.
DETAILED DESCRIPTION OF THE INVENTION
Referring initially to FIG. 1 there is shown a typical layout of a conventional straight bar knitting machine having knitting needles A held in a needle bar E. Sinkers B (typically one between every two needles) are slidingly received in a sinker bar K which extends along the length of the knitting head. Dividers C are usually located inbetween each pair of neighbouring sinkers.
A catch bar G extending along the length of the knitting head is provided for advancement of the dividers and the simultaneous retraction of the sinkers and dividers.
A slur cock SC is provided mounted on a guide rail extending along the knitting head. The slur cock SC moves along the guide rail and advances each sinker sequentially by engaging by a camming action, an associated striking jack J.
In accordance with a first embodiment of the present invention (FIG. 3), the slur cock SC and associated guide rail and drive mechanism is replaced by a sinker drive mechanism 10 which operates the sinkers via the striking jacks J. In accordance with a second embodiment of the present invention (FIG. 9), the striking jacks J are also replaced so that the sinker drive mechanism operates directly upon the sinkers B. In both embodiments the drive mechanism 10 basically comprises a series of independently movable striking pistons 12 housed in a support body 14 which extends along the length of the knitting head, there being one striking piston 12 for striking each jack J. The body 14 is conveniently mounted upon the machine bed which normally supports the conventional slur cock rail.
The pistons 12 are operated in sequence along the length of the support body 14 so as to operate the striking jacks J sequentially along the knitting head; retraction of the pistons 12 being achieved by the conventional motion of the catch bar G when retracting the sinkers B and dividers C.
In the embodiment shown in FIGS. 3 to 5, the body 14 is conveniently made from a machinable material such as a suitable metal, eg brass and the pistons 12 are preferably each in the form of a rod having a close tolerance fit within a cylinder bore 16. Seals between the piston 12 and associated cylinder bore 16 are preferably not provided in order to avoid lubrication, overheating and seizure problems. Instead, the cylinder bore 16 and/or the pistons 12 are coated with a hard wearing low friction material such as polytetrafluoroethylene. A conventional coating process known as the `Nyflor` process is used in order to attain a coating having a hardness in the range of 800-1000 Vickers. The tolerance between the piston 12 and associated cylinder bore 16 is chosen to give the desired pressure sealing characteristics for advancing the pistons 12 when exposed to pressurised fluid. The tolerance is preferably 0 to 1 thousandth of an inch for a piston 12 of 3/16 inch diameter.
Preferably as shown in FIGS. 5 and 9, the pistons 12 include a head 12a of reduced diameter to enable the piston to extend inbetween adjacent dividers C for operating the sinker B located therebetween.
Sequential advancement of the pistons 12 is preferably achieved as indicated in FIG. 3.
In the embodiment shown in FIG. 4, the support body 14 includes an elongate cylinder bore 18 defining a piston chamber in which a piston 20 is housed. The piston 20 includes a piston stem 21 having a piston head 22. Preferably, the piston head 22 carries one or more piston rings (not shown) made for example from cast iron for providing a seal between the piston head 22 and bore 18.
Preferably the piston 20 is rotatable about its longitudinal axis and indexing means (not shown) are preferably provided for indexing the piston 20 through a small area prior to each stroke of the piston. In this way wear on the piston rings caused by the mouths of bores 16 is evenly distributed about the circumference of the piston rings.
Located at one end of the cylinder bore 18 is a port 24 having a valve 24a and located at the opposite end of the cylinder bore 18 is a port 26 having a valve 26a. All the cylinder bores 16 communicate with the cylinder bore 18 via conduits 16a.
During one knitting cycle, the piston head 22 is driven from one end to the other end of the bore 18. At commencement of the stroke of the head 22, all pistons 12 reside at their retracted positions due to the return motion of the catch bar G during the previous knitting cycle.
Immediately prior to the advancement of piston head 22, the port 24, 26 located at the advancement side of piston head 22 is vented so as to avoid pressure build up on the upstream side of the piston head 22 as it advances and the port 24, 26 located on the downstream side of the piston head 22 is connected to a source of pressurised fluid, typically compressed air. Typically the source of pressurised air is at a pressure of 150 psi; the pressure for advancing each piston being typically 2 psi.
Accordingly, as the piston head 22 advances, it sequentially opens communication between successive cylinder bores 16 and the pressurised fluid on the downstream side of the piston head 22 and so sequentially advances neighbouring pistons 12 as it proceeds toward the upstream end of the cylinder bore 18.
Preferably the size of the conduits 16a is chosen such that the conduit opening neighbouring of neighbouring conduits 16a are sufficiently spaced from one another in the axial direction of bore 18 such that each piston 12 is fully advanced before the next succeeding piston 12.
Accordingly, the piston 20 effectively acts as a linear valve for sequentially supplying pressurised fluid to successive cylinder bores 16.
After all the pistons 12 have been advanced, cylinder bore 18 is vented to enable the catch bar G to subsequently retract all the pistons 12 during the later stages of the knitting cycle.
Preferably as shown in FIG. 4, the pistons 12 are arranged in laterally spaced rows extending along the length of the body 14, the pistons 12 in each row being staggered to thereby enable a minimum pitch distance D to be achieved. The pitch between the pistons 12 corresponds to the distance between adjacent striker jacks J so that there is one piston 12 per striker jack.
In the event that the knitting machine has sinkers only (ie. the dividers are replaced by sinkers and associated striking jacks) then additional pistons 12 would be provided.
Typically for machines of 21 to 30 gauge, the diameter of the pistons 12 would be about 3/16 inch.
An alternative arrangement is illustrated in FIG. 6 for controlling supply of pressurised fluid to the cylinder bore 16 and for venting one end of the bore 18 during advancement of the piston head 22.
In FIG. 6 the cylinder bore 18 is open ended at both ends to define large venting ports 30, 31 respectively. In this embodiment, ports 24, 26 serve to supply pressurised fluid only under the control of respective valves 24a, 26a.
A pair of valve elements 32, 33 are provided for sealingly closing respective ports 30, 32. Preferably as shown, valve elements 32, 33 are connected to a common drive mechanism 36 simultaneously closing and opening of the ports 30, 32. In FIG. 6, the drive mechanism 36 includes a piston and cylinder assembly 37 which through connecting rods 38 move the valve elements 32, 33.
Two alternative drive mechanisms are illustrated in FIGS. 7 and 8 for reciprocating the piston 20.
In FIG. 7, a drive mechanism 40 for driving pistons 20 in a multiple section straight bar knitting machine is illustrated. In FIG. 7, 3 knitting sections KS are illustrated in which each section KS includes a sinker drive means 10 according to the present invention. The pistons 20 of each sinker drive means are mechanically connected in series by connecting rods 21a.
One of the connecting rods 21a is drivingly connected to a toothed rack 42 which is reciprocated by a drive means 44. The drive means 44 preferably comprises a piston and cylinder assembly 46 which is arranged to reciprocate a toothed rack 47; a pinion gear 48 being provided to transmit drive from rack 47 to rack 42. Preferably a reduced gear ratio of about 4:1 is chosen between racks 47 and 42.
Accordingly as assembly 46 reciprocates rack 47, all the pistons 20 are simultaneously reciprocated across their respective knitting sections KS.
Although FIG. 7 only illustrates three knitting section KS, it will be appreciated that the knitting machine may include more or fewer knitting section KS.
In FIG. 8, an alternative drive means for piston 20 is illustrated which is particularly suitable for a knitting machine having a single knitting section. In FIG. 6, the piston rod 21 is connected to a linear motor 50 which is arranged to reciprocate along a rail 51. A suitable linear motor is a microstepping motor, as for example a `L-series stepping linear motor` as produced by Parker. A stepping linear motor is preferred as it can be controlled to accelerate/decelerate in a desired manner during its reciprocal driving stroke of the piston 20.
As an alternative, it is envisaged that the linear motor may be a continuously operable linear motor controlled by an encoder which responds to displacement of the motor.
A modified embodiment 100 is illustrated in FIGS. 10 and 11. In embodiment 100 the piston chamber is defined by the internal bore 118 of a hollow tube 120. The hollow tube 120 is provided with a plurality of communication bores 121 extending generally radially through the wall of the tube 120. The bores 121 are spaced along the length of the tube and are arranged such that each bore 121 is aligned with a corresponding cylinder bore 16 so as to provide fluid communication between the corresponding bore 16 and the piston chamber.
The tube 120 is conveniently made from a suitable plastics material such as a polyamide. Accordingly the tube 120 is simple to manufacture, by for example extrusion techniques to define the piston chamber. Drilling of the tube wall is conveniently performed in order to define the communication bores 121.
The support body 14 in embodiment 100 includes an elongate recess 130 which defines a seat for the tubes 120. The recess 130 is preferably part circular in cross-section having a diameter corresponding to the outer diameter of tube 120.
Terminal ends of the piston cylinders 16 open into the recess 130. Accordingly, when the tube 120 is seated in the recess 130, its outer face is in face to face contact with the recess 130 with bores 121 aligned with corresponding cylinders 16. The tube 120 is preferably secured in the seat by a suitable adhesive which also acts to provide a seal to prevent leakage of fluid between neighbouring cylinders 16. A silicon based adhesive has been found to be suitable.
Preferably in embodiment 100, the piston head 22 is provided with resilient annular seals 140 which sealingly engage the internal face of bore 118. Each seal 140 preferably includes an inclined seal lip 141 which when exposed to fluid pressure is deflected outwardly to increase sealing contact with the internal face of bore 118.
Preferably in embodiment 100, the support body 14 is formed from a suitable plastics material, such as for example a polyamide.
Preferably in embodiment 100, each piston 12 includes a piston stem 150 formed from a small diameter rod, preferably made of steel, and a piston head 151 having a resilient seal 152 for sealingly contacting the internal face of the associated cylinder 16. The seal 152 preferably includes an inclined seal lip 153 which deflects outwardly when exposed to fluid pressure to thereby increase sealing contact with the internal face of the associated cylinder 16.
Preferably a second annular seal 160 is provided on the piston head 151 at a spaced located along the axis of the piston. The second seal 160 may be of any conventional formed. Conveniently the piston head 151 is formed from a suitable plastics material, such as for example a polyamide.
Operation of the embodiment 100 is the same as that described in respect of the previous embodiments.
The above embodiments relate to the use of the sinker drive means according to the invention in a straight bar knitting machine. It will be appreciated that the drive means is adapted to be retrofitted in existing straight bar knitting machines.
It will also be appreciated that the drive means may be incorporated into other types of knitting or weaving machines requiring the sequential extension of a series of component parts.
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An elongate support body includes each of a plurality of pistons longitudinally translatable to urge movement of a corresponding sinker in a straight bar knitting machine. A piston chamber is disposed within or attached to the support body and includes a translatable piston head disposed therewithin. Each of a plurality of piston cylinders housing the respective ones of the plurality of pistons is in fluid communication with the piston chamber. Upon introduction of a fluid under pressure into the piston chamber on one side of the piston head, fluid pressure will be introduced serially into each piston cylinder to actuate each piston as the piston head translates along the piston chamber.
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The present application is a national stage application of and claims priority to International Patent Application No. PCT/US2006/042581, filed Nov. 2, 2006, and entitled “The Use of Apoptotic Cells Ex Vivo to Generate Regulatory T Cells,” which is related to and claims, under 35 USC §119(e), the benefit of U.S. Provisional Patent Application Ser. No. 60/732,847, filed Nov. 2, 2005, and entitled “The Use of Apoptotic Cells Ex Vivo to Generate Regulatory T Cells.” The present application incorporates herein by reference the disclosures of each of the above-referenced applications in their entireties.
BACKGROUND OF THE INVENTION
Many cell types in the body can remove apoptotic and cellular debris from tissues; however, the professional phagocyte, or antigen presenting cell (“APC”), has a high capacity to do so. The recognition of apoptotic cells (“ACs”) occurs via a series of evolutionarily-conserved, AC-associated molecular-pattern receptors (“ACAMPRs”) on APCs that recognize and bind corresponding apoptotic-cell-associated molecular patterns (“ACAMPs”). These receptors recognize ligands such as phosphotidyl serine and oxidized lipids found on apoptotic cells. Savill et al. (2002); and Gregory et al. (2004).
Both in vitro and in vivo that AC clearance by APCs in vivo regulates immune responses. Savill, et al. (2002). This immune modulation appears to occur primarily via an alteration of APC function with several hallmarks of a tolerance-inducing APC. These tolerogenic APCs induce tolerance via a variety of mechanisms including the generation of regulatory T cells (“Tregs”).
Tregs comprise a heterogeneous group of T lymphocytes, which actively inhibit immune responses. Groux et al. (1997); Sakaguchi et al. (2001); and Roncarolo et al. (2001). There is the potential to develop Treg therapies for a variety of diseases.
One way to generate Tregs in vivo is via the infusion of ACs. There is evidence from both animal models and human treatments that AC infusion, such as happens during extracorporeal photophoresis (“ECP”), induces Tregs. Maeda et al. (2005); Lamioni et al. (2005); Aubin et al. (2004); Mahnke et al. (2003); and Saas et al. (2002).
Other methods to generate Tregs ex vivo include exposing T cells to a variety of substances including: IL-10 (Roncarolo et al. (2001); and Zeller et al. (1999)); TGFβ (Zheng et al. (2004); Gray et al. (1998); Horwitz et al. (1999); Ohtsuka et al. (1999a); Ohtsuka et al. (1999b); Stohl et al. (1999); Gray et al. (2001); Horwitz, (2001); Yamagiwa et al. (2001); Horwitz et al. (2002); and Zheng et al. (2002)); αMSH (Luger et al. (1999); Taylor (2005); Namba et al. (2002); Nishida et al. (1999); Nishida et al. (2004); Streilin et al. (2000); Taylor et al. (1992); Taylor et al. (1994a); Taylor et al. (1994b); Taylor et al. (1996); Taylor (1999); Taylor (2003); and Taylor et al. (2003)); vitamin D3 (Willheim et al. (1999); Penna et al. (2000); Pedersen et al. (2004); May et al. (2004); Koren et al. (1989); Gregori et al. (2001); Cobbold et al. (2003); and Barrat et al. (2002)); dexamethasone (Pedersen et al. (2004); Barrat et al. (2002); and O'Garra et al. (2003)); and purification (Earle et al. (2005); Schwarz et al. (2000); Chatenoud et al. (2001); Tang et al. (2004); and Masteller et al. (2005)).
Autoimmune diseases involve inappropriate activation of immune cells that are reactive against self tissue. These activated immune cells promote the production of cytokines and autoantibodies involved in the pathology of the diseases. Other diseases involving T-cells include Graft versus Host Disease (GVHD) which occurs in the context of transplantation. In GVHD donor T-cells reject recipient's tissues and organs by mounting an attack against the recipient's body. A host of other diseases involve disregulation of the host immune system. Some are best treated with pharmaceuticals, some with biologicals, others with treatments such as extracorporeal photophoresis (ECP), and yet others have very limited treatment options.
ECP has been shown to be an effective therapy in certain T cell-mediated diseases. In the case of GVHD, photopheresis has been used as a treatment in association with topical triamcinolone ointment, antifungal, antiviral, antibiotics, inimunoglobulins, and methotrexate. ECP has also been used with immunosuppressive agents such as mycophenolate mofetil, tacrolimus, prednisone, cyclosporine, hydroxychloroquine, steroids, FK-506, and thalidomide for chronic GVHD (“cGVHD”) and refractory cGVHD. For solid organ transplants, ECP has been used in conjunction with immunosuppressive agents to reduce the number of acute allograft rejection episodes associated with renal allografts and cardiac tranplants. For example, ECP has been used with OKT3 and/or the immunosuppressive agents prednisone, azathioprine, and cyclosporine to reverse acute renal allograft rejection. ECP has also been used with cyclophosphamide, fractionated total body irradiation, and etoposide for allogeneic marrow transplantation for acute myeloid leukemia, acute lymphoblastic leukemia, chronic myeloid leukemia, non-Hodgkin's lymphoma,; or severe aplastic anemia.
SUMMARY OF THE INVENTION
Ex vivo incubation with leukocytes in an allogeneic system leads to generation of T cells with regulatory activity. This generates regulatory T cells (“Treg cells” or “T regs”) with activity to suppress immune responses against the alloantigen.
In an antigen specific and polyclonal activation systems an antigen specific result can be obtained by adding antigen or other stimulation with autologous apoptotic cells. (“ACs”).
The present invention encompasses a method of generating T cells with regulatory activity (T regs) by incubating leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
The present invention encompasses compositions of a population of T cells with regulatory activity (T regs) obtained by incubating leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
The present invention encompasses a method of treating autoimmune disorder or ameliorating one or more symptoms thereof, by administering to a patient in need thereof an effective amount of a composition of a population of T cells with regulatory activity (T regs) obtained by incubating autologous leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
The present invention encompasses a method of treating atopic disease or ameliorating one or more symptoms thereof by administering to a patient in need thereof an effective amount of a composition of a population of T cells with regulatory activity (T regs) obtained by incubating autologous leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
The present invention encompasses a method of administering to a transplant recipient an effective amount of a composition of a population of T cells with regulatory activity (T regs) obtained by incubating autologous leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
The present invention encompasses a method of administering to a GVHD patient an effective amount of a composition of a population of T cells with regulatory activity (T regs) obtained by incubating autologous leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
The present invention encompasses a method of treating patient with a disorder or the predisposition for a disorder by testing the patient to determine whether the patient has a disorder, and administering to a patient in need thereof an effective amount of a composition of a population of T cells with regulatory-activity (T regs) obtained by incubating autologous leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic showing A: Treg Generation; B: After T regulatory cells are generated, Treg cells placed into MLR.
FIG. 2 shows that regulatory T Cells generated via Co-incubation with ECP-treated PBMCs inhibit the proliferation of syngeneic T Cells
FIG. 3 shows that regulatory T Cells generated via co-incubation with ECP-treated PBMCs inhibit T Cell proliferation better than standard Tr1 cells.
FIG. 4 shows that generation of Regulatory T Cells via co-incubation with ECP-treated PBMCs can be reversed through the addition of lnterleukin-2.
FIG. 5 shows that suppressive activity of regulatory T cells generated via co-incubation with ECP-treated PBMCs is contact-dependent.
DETAILED DESCRIPTION
Ex Vivo Generation of Tregs Using ACs
The systems that occur in vivo to generate Tregs are quite complex and rely on a series of cell types and morphologic location. Nevertheless, the present invention shows that it is possible to generate these cells in vitro under the conditions described herein. Ex vivo incubation with leukocytes in an allogeneic system leads to generation of T cells with regulatory activity. This generates regulatory T cells (“Treg cells”) with activity to suppress immune responses against the alloantigen, important in a wide variety of disorders including, without limitation, autoimmune diseases, graft versus host disease (“GVHD”),and solid organ transplantation. In an antigen specific and polyclonal activation systems an antigen specific result can be obtained by adding antigen or other stimulation with autologous apoptotic cells (“ACs”).
This ex vivo production method offers several advantages over the drug-induced methods previously described. Importantly, the possible toxic and non-natural effects of these added molecules are avoided.
In addition, there are advantages to ex vivo generation over the in vivo utilization of apoptotic cells including, without limitation, increased control over the number, activity and function of these cells. This therapeutic control provides improved patient treatment protocols.
Generating T regs using a series of methods such as purification, activation, and addition of differentiation factors such as TGFβ, αMSH, anti-CD46, IL-10, vitamin D 3 and dexamethasone has proven that these cells can be generated ex vivo. Apoptotic cells provide a more “in vitro-like” method to induce these cells by generating tolerogenic APCs.
The present invention encompasses a method of generating T-cells with regulatory activity (T regs) by incubating leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
The present invention encompasses compositions of a population of T cells with regulatory activity (T regs) obtained by incubating leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
The present invention encompasses a method of treating autoimmune disorder or ameliorating one or more symptoms thereof, by administering to a patient in need thereof an effective amount of a composition of a population of T cells with regulatory activity (T regs) obtained by incubating autologous leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
Autoimmune disorders include, without limitation, acute transverse myelitis, alopecia areata, Alzheimer's disease, amyotrophic lateral sclerosis, ankylosing spondylitis, antiphospholipid syndrome, atherosclerosis, autoimmune Addison's disease, autoimmune hemolytic anemia, Behcet's disease, bullous pemphigoid, cardiomyopathy, celiac sprue-dermatitis, Cerebellar Spinocerebellar Disorders, spinocerebellar degenerations (spinal ataxia, Friedreich's ataxia, cerebellar cortical degenerations), chronic alcoholism, alcohol-induced hepatitis, autoimmune hepatitis, chronic fatigue immune dysfunction syndrome (CFIDS), chronic inflammatory bowel disease, chronic inflammatory demyelinating polyneuropathy, Churg-Strauss syndrome, cicatricial pemphigoid, cold agglutinin disease, CResT syndrome, Creutzfeldt-Jakob disease, Crohn's disease, Dejerine-Thomas atrophy, Dementia pugilistica, diabetes mellitus, Diffuse Lewy body disease, discoid lupus, disorders of the basal ganglia, disseminated intravascular coagulation, Down's Syndrome in middle age, drug-induced movement disorders, essential mixed cryoglobulinemia, fibromyalgia-fibromyositis, graft versus host disease, Graves' disease, Guillain-Barré syndrome, Hallerrorden-Spatz disease, Hashimoto's thyroiditis, Huntington's Chorea senile chorea, idiopathic pulmonary fibrosis, idiopathic thrombocytopenia purpura (ITP), IgA nephropathy, infantile or juvenile spinal muscular atrophy, insulin dependent diabetes, juvenile arthritis, Kawasaki's pathology, lesions of the corticospinal system, Leukemias, Hodgkin's lymphoma, non-Hodgkin's lymphoma, lichen planus, Ménière's disease, mixed connective tissue disease, multiple sclerosis, multiple systems degenerations (Mencel, Dejerine-Thomas, Shy-Drager, Machado-Joseph), myasthenia gravis, neurogenic muscular, Parkinson's disease, pemphigus vulgaris, pernicious anemia, polyarteritis nodosa, polychondritis, polyglandular syndromes, polymyalgia rheumatica, polymyositis dermatomyositis, primary agammaglobulinemia, primary biliary cirrhosis, Progressive supranuclear palsy, psoriasis, Raynaud's phenomenon, Reiter's syndrome, rheumatic fever, rheumatoid arthritis, sarcoidosis, scleroderma, Senile Dementia of Lewy body type, Sjögren's syndrome, stiff-man syndrome, Subacute sclerosing panencephalitis, systemic disorders (Refsum's disease, abetalipoprotemia, ataxia, telangiectasia, mitochondrial multi-system disorder), systemic lupus erythematosus (SLE), Takayasu arteritis, temporal arteritis/giant cell arteritis, thyroidosis, ulcerative colitis, uveitis, vasculitis, vitiligo, Wegener's granulomatosis, Wernicke-Korsakoff. syndrome.
The present invention encompasses a method of treating atopic disease or ameliorating one or more symptoms thereof by administering to a patient in need thereof an effective amount of a composition of a population of T cells with regulatory activity (T regs) obtained by incubating autologous leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
Atopic disorders include, without limitation, chronic inflammatory pathologies and vascular inflammatory pathologies, including chronic inflammatory pathologies such as sarcoidosis, chronic inflammatory bowel disease, ulcerative colitis, and Crohn's pathology and vascular inflammatory pathologies, such as, but not limited to, disseminated intravascular coagulation, atherosclerosis, and Kawasaki's pathology.
The present invention encompasses a method of administering to a transplant recipient an effective amount of a composition of a population of T cells with regulatory activity (T regs) obtained by incubating autologous leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
The present invention encompasses a method of administering to a GVHD patient an effective amount of a composition of a population of T cells with regulatory activity (T regs) obtained by incubating autologous leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
The present invention encompasses a method of treating patient with a disorder or the predisposition for a disorder by testing the patient to determine whether the patient has a disorder, and administering to a patient in need thereof an effective amount of a composition of a population of T cells with regulatory activity (T regs) obtained by incubating autologous leukocytes with autologous apoptotic peripheral blood mononuclear cells (ACs).
T regs can be administered to the patient according to a schedule including, without limitation, two days, one week prior to the transplantation; three days, one week prior to harvesting said transplant; two days a week for two weeks prior to the transplantation; and three days a week for three weeks prior to the transplantation.
Effective amounts of T regs for use in the methods of treatment of the present invention to obtain the required clinical benefit in a subject may vary depending on the source of cells, the subject's condition, the age and weight of the subject and other relevant factors, which are readily determinable by well-known methods. Preferably, the number of T regs administered to a patient are about 1×10 5 /kg to about 1×10 7 /kg. More preferably, the number of T regs administered to a patient are about 1×/10 6 kg.
The method of the present invention encompasses incubating the ACs and leukocytes for a time and under conditions sufficient to generate T regs. Incubation can be under any condition known in the art to be suitable for leukocytes and for about 1 to about 14 days. Preferably, incubation is for about 8 days.
The method of the present invention can further include selecting leukocytes expressing CD4 to obtain CD4+ cells. Preferably, thee cells are CD4+.
The method of the present invention includes incubation at any suitable concentration f ACs and CD4+ cells. Preferably, the cells are at about a 1:10 to about a 10:1 ratio of CD4+:ACs. More preferably, the cells are at a 2:1 to about a 1:2 ratio of CD4+:ACs.
The ACs of the present invention are obtained by an apoptosis-inducing treatment known in the art. Preferably, the apoptosis-inducing treatment is an ECP procedure that employs a photoactivatable compound together with light of a wavelength that activates the photoactivatable compound. Preferably, the photoactivatable compound is a psoralen and the light is UVA. Preferably, the psoralen is 8-MOP.
The method of the present invention can include the incubation with added factors that further enhance generation or function of the T regs. Suitable factors include, without limitation, are hormones, proteins, drugs or antibodies. Preferably, the factors include, without limitation, one of TGFβ, αMSH, anti-CD46, IL-10, vitamin D 3 , dexamethasone, rapamycin and IL-2. Preferably, the factor is IL-10. Preferably, the IL-10 is present at a concentration of about 1 ng/ml to about 100 ng/ml. Preferably, the IL-10 is present at a concentration of about 20 ng/ml.
The method of the present invention includes adding an antigen to the incubation to generate Tregs which regulate immune response to the antigen. Preferably, the antigen is an alloantigen. Such antigens can be selected from any known in the art.
The cell populations useful in the methods of this invention comprise “apoptotic cells,” which include cells and cell bodies, i.e., apoptotic bodies, that exhibit, or will exhibit, one or more apoptosis-characterizing features. An apoptotic cell may: comprise any cell that is in the Induction phase, Effector phase, or the Degradation phase. The cell populations in the therapies of the invention may also comprise cells that have been treated with an apoptosis-inducing agent that are still viable. Such cells may exhibit apoptosis-characterizing features at some point, for example, after administration to the subject. Preferably, the ACs are autologous PBMCs that have been treated with an apoptosis inducer. Preferably the apoptosis inducer is ECP.
ECP directly induces significant levels of apoptosis. This has been observed, for example, in lymphocytes of CTCL, GVHD, and scleroderma patients. The apoptotic cells contribute to the observed clinical effect.
Apoptosis-characterizing features may include, but are not limited to, surface exposure of phosphatidylserine, as detected by standard, accepted methods of detection such as Annexin V staining; alterations in mitochondrial membrane permeability measured by standard, accepted methods evidence of DNA fragmentation such as the appearance of DNA laddering on agarose gel electrophoresis following extraction of DNA from the cells or by in situ labeling. Salvioli et al. (1997); Teiger et al. (1996); and Gavrieli et al. (1992).
The cell population for use in the present invention is induced to become apoptotic ex vivo, i.e., extracorporeally, and is compatible with those of the subject, donor, or recipient. A cell population may be prepared from substantially any type of mammalian cell including cultured cell lines. For example, a cell population may be prepared from a cell type derived from the mammalian subject's own body autologous) or from an established cell line. Specifically, a cell population may be prepared from white blood cells of blood compatible with that of the mammalian subject, more specifically, from the subject's own white blood cell and even more specifically, from the subject's own leukocytes or T cells.
A cell population may also be prepared from an established cell line. A cell line that may be useful in the methods of the present invention includes, for example, Jurkat cells (ATCC No. TIB-152). Other cells lines appropriate for use in accordance with the methods of the present invention may be identified and/or determined by those of ordinary skill in the art. The cell population may be prepared extracorporeally prior to administration to the subject, donor, or recipient. Thus, in one embodiment, an aliquot of the subject's blood, recipient's blood, or the donor's blood may be withdrawn, e.g. by venipuncture, and at least a portion of the white cells thereof subjected extracorporeally to apoptosis-inducing conditions.
In one embodiment, the cell population may comprise a particular subset of cells including, but not limited to leukocytes or cells separated from leukocytes on the basis of their expression of CD4, that is CD4+ T cells. The separation and purification of blood components is well known to those of ordinary skill in the art. Indeed, the advent of blood component therapy has given rise to numerous systems designed for the collection of specific blood components. Several of these collection systems are commercially available from, for example, Immunicon Corp. (Huntingdon Valley, Pa.), Baxter International (Deerfield, Ill.), and Dynal Biotech (Oslo, Norway).
Immunicon's separation system separates blood components using magnetic nanoparticles (ferrofluids) coated with antibodies that conjugate, i.e., form a complex, to the target components in a blood sample. The blood sample is then incubated in a strong magnetic field and the target complex migrates away from the rest of the sample where it can then be collected. See, e.g., U.S. Pat. Nos. 6,365,362; 6,361,749; 6,228,624; 6,136,182; 6,120,856; 6,013,532; 6,013,188; 5,993,665; 5,985,153; 5,876,593; 5,795,470; 5,741,714; 5,698,271; 5,660,990; 5,646,001; 5,622,831; 5,591,531; 5,541,072; 5,512,332; 5,466,574; 5,200,084; 5,186,827; 5,108,933; and 4,795,698.
Dynal's Dynabeads® Biomagnetic separation system separates blood components using magnetic beads coated with antibodies that conjugate to the target components in a blood sample, forming a Dynabeads-target complex. The complex is then removed from the sample using a Magnetic Particle Concentrator (Dynal MPC®). Several different cell types may be collected using this separation system. T cells and T cell subsets can also be positively or negatively isolated or depleted from whole blood, buffy coat, gradient mononuclear cells or tissue digests using, for example, CELLection™ CD2Kit (Prod. No 116.03), Dynabeads® M-450 CD2 (Prod. No 111.01/02), Dynabeads®) CD3 (Prod. No 111.13/14), Dynabeads® plus DETACHaBEAD (Prod. No. 113.03), Dynabeads® M-450 CD4 (Prod. No 111.05/06), CD4 Negative Isolation Kit (T helper/inducer cells) (Prod. No. 113.17), CD8 Positive Isolation Kit (Prod. No. 113.05), Dynabeads® CD8 (Prod. No. 111.07/08), CD8 Negative Isolation Kit (Prod. No. 113.19), T Cell Negative Isolation Kit (Prod. No. 113.11), Dynabeads® CD25 (Prod. No 111.33/34), and Dynabeads® CD3/CD28 T Cell Expander (Prod. No. 111.31). Baxter International has developed several apheresis systems based on the properties of centrifugation, including the CS-3000 blood cell separator, the Amicus separator, and the Autopheresis-C system. The CS-3000 Plus blood cell separator collects both cellular apheresis, products and plasma. It comprises a continuous-flow separator with a dual-chamber centrifugal system that collects apheresis products. The Amicus operates in either a continuous-flow or intermittent-flow format to collect single donor platelets and plasma. The Autopheresis-C system is designed for the collection of plasma from donors and can collect more than 250 mL of plasma. See generally, U.S. Pat. Nos. 6,451,203; 6,442,397; 6,315,707; 6,284,142; 6,9'51,284; 6,033,561; 6,027,441; and 5,494,578.
In the most preferred embodiment of the invention, ECP is used to induce apoptosis. This involves a photoactivatable compound added to a cell population ex vivo. The photosensitive compound may be administered to a cell population comprising blood cells following its withdrawal from the subject, recipient, or donor, as the case may be, and prior to or contemporaneously with exposure to ultraviolet light. The photosensitive compound may be administered to a cell population comprising whole blood or a fraction thereof provided that the target blood cells or blood components receive the photosensitive compound. In another embodiment, a portion of the subject's blood, recipient's blood, or the donor's blood could first be processed using known methods to substantially remove the erythrocytes and the photoactive compound may then be administered to the resulting cell population comprising the enriched PBMC fraction.
Photoactivatable compounds for use in accordance with the present invention include, but are not limited to, compounds known as psoralens (or furocoumarins) as well as psoralen derivatives such as those described in, for example, U.S. Pat. Nos. 4,321,919; and 5,399,719. Preferred compounds include 8-methoxypsoralen; 4,5′8-trimethylpsoralen; 5-methoxypsoralen; 4-methylpsoralen; 4,4-dimethylpsoralen; 4,5′-dimethylpsoralen; 4′-aminomethyl-4,5′,8-trimethylpsoralen; 4′-hydroxymethyl-4,5′,8-trimethylpsoralen; 4′,8-methoxypsoralen; and a 4′-(omega-amino-2-oxa) alkyl-4,5′8-trimethylpsoralen, including but not limited to 4′-(4-amino-2-oxa)butyl-4,5′,8-trimethylpsoralen. In one embodiment, the photosensitive compound that may be used comprises the psoralen derivative, amotosalen(S-59) (Cerus Corp., Concord, Calif.). In another embodiment, the photosensitive compound comprises 8-methoxypsoralen (8 MOP).
The cell population to which the photoactivatable compound has been added is treated with a light of a wavelength that activates the photoactivatable compound. The treatment step that activates the photoactivatable compound is preferably carried out using long wavelength ultraviolet light (UVA), for example, at a wavelength within the range of 320 to 400 nm. The exposure to ultraviolet light during the photopheresis treatment preferably is administered for a sufficient length of time to deliver about 1-2 J/cm 2 to the cell population.
Extracorporeal photopheresis apparatus useful in the methods according to the invention include those manufactured by Therakos, Inc., (Exton, Pa.) under the name UVAR®. A description of such an apparatus is found in U.S. Pat. No. 4,683,889. The UVAR®system uses a treatment system and consists of three phases including: 1) the collection of a buffy-coat fraction (leukocyte-enriched), 2) irradiation of the collected buffy coat fraction, and 3) reinfusion of the treated white blood cells. The collection phase has six cycles of blood withdrawal, centrifugation, and reinfusion steps. During each cycle, whole blood is centrifuged and separated in a pheresis bowl. From this separation, plasma (volume in each cycle is determined by the UVAR® instrument operator) and 40 ml buffy coat are saved in each collection cycle. The red cells and all additional plasma are reinfused to the patient before beginning the next collection cycle. Finally, a total of 240 ml of buffy coat and 300 ml of plasma are separated and saved for UVA irradiation.
The irradiation of the leukocyte-enriched blood within the irradiation circuit begins during the buffy coat collection of the first collection cycle. The collected plasma and buffy coat are mixed with 200 ml of heparinized normal saline and 200 mg of UVADEX® (water soluble 8-methoxypsoralin). This mixture flows in a 1.4 mm thick layer through the PHOTOCEPTOR® Photoactivation Chamber, which is inserted between two banks of UVA lamps of the PHOTOSETTE®. PHOTOSETTE® UVA lamps irradiate both sides of this UVA-transparent PHOTOCEPTOR® chamber, permitting a 180-minute exposure to ultraviolet A light, yielding an average exposure per lymphocyte of 1-2 J/cm 2 . The final buffy coat preparation contains an estimated 20% to 25% of the total PBMC component and has a hematocrit from 2.5% to 7%. Following the photoactivation period, the volume is reinfused to the patient over a 30 to 45 minute period. U.S. patent application Ser. No. 09/480,893 describes another system for use in ECP administration. U.S. Pat. Nos. 5,951,509; 5,985,914; 5,984,887, 4,464,166; 4,428,744; 4,398,906; 4,321,919; WO 97/36634; and WO 97/36581 also contain description of devices and methods useful in this regard.
Another system that may be useful in the methods of the present invention is described in U.S. patent application Ser. No. 09/556,832. That system includes an apparatus by which the net fluid volume collected or removed from a subject may be reduced during ECP. The effective amount of light energy that is delivered to a cell population may be determined using the methods and systems described in U.S. Pat. No. 6,219,584.
A variety of other methods for inducing apoptosis in a cell population are well-known and may be adopted for use in the present invention. One such treatment comprises subjecting a cell population to ionizing radiation (gamma-rays, x-rays, etc.) and/or non-ionizing electromagnetic radiation including ultraviolet light, heating, cooling, serum deprivation, growth factor deprivation, acidifying, diluting, alkalizing, ionic strength change, serum deprivation, irradiating, or a combination thereof. Alternatively, apoptosis may be induced by subjecting a cell population to ultrasound.
Yet another method of inducing apoptosis comprises the extracorporeal application of oxidative stress to a cell population. This may be achieved by treating the cell population, in suspension, with chemical oxidizing agents such as hydrogen peroxide, other peroxides and hydroperoxides, ozone, permanganates, periodates, and the like. Biologically acceptable oxidizing agents may be used to reduce potential problems associated with residues and contaminations of the apoptosis-induced cell population so formed.
In preparing the apoptosis-induced cell population, care should be taken not to apply excessive levels of oxidative stress, radiation, drug treatment, etc., because otherwise there may be a significant risk of causing necrosis of at least some of the cells under treatment. Necrosis causes cell membrane rupture and the release of cellular contents often with biologically harmful results, particularly inflammatory events, so that the presence of necrotic cells and their components along with the cell population comprising apoptotic cells is best avoided. Appropriate levels of treatment of the cell population to induce, apoptosis, and the type of treatment chosen to induce apoptosis are readily determinable by those skilled in the art.
One process according to the present, invention involves the culture of cells from the subject, or a compatible mammalian cell line. The cultured cells may then be treated extracorporeally to induce apoptosis and to create a cell population therein. The extracorporeal treatment may be selected from the group consisting of antibodies, chemotherapeutic agents, radiation, ECP, ultrasound, proteins, and oxidizing agents. The cells, suspended in the subject's plasma or another suitable suspension medium, such as saline or a balanced mammalian cell culture medium, may then be incubated as indicated below.
Methods for the detection and quantitation of apoptosis are useful for determining the presence and level of apoptosis in the preparation to be incubated with leukocytes or T cells in the present invention. In one embodiment, cells undergoing apoptosis may be identified by a characteristic ‘laddering’ of DNA seen on agarose gel electrophoresis, resulting from cleavage of DNA into a series of fragments. In another embodiment, the surface expression of phosphatidylserine on cells may be used to identify and/or quantify an apoptosis-induced cell population. Measurement of changes in mitochondrial membrane potential, reflecting changes in mitochondrial membrane permeability, is another recognized method of identification of a cell population. A number of other methods of identification of cells undergoing apoptosis and of a cell population, many using monoclonal antibodies against specific markers for a cell population, have also been described in the scientific literature.
The administration of T regs finds utility in treating arthritis and other autoimmune diseases. They are also useful in the treatment or prophylaxis of at least one autoimmune-related disease in a cell, tissue, organ, animal, or patient including, but not limited to, acute transverse myelitis, alopecia areata, Alzheimer's disease, amyotrophic lateral sclerosis, ankylosing spondylitis, antiphospholipid syndrome atherosclerosis, autoimmune Addison's disease, autoimmune hemolytic anemia, Behcet's disease, bullous pemphigoid, cardiomyopathy, celiac sprue-dermatitis, Cerebellar Spinocerebellar Disorders, spinocerebellar degenerations (spinal ataxia, Friedreich's ataxia, cerebellar cortical degenerations), chronic alcoholism, alcohol-induced hepatitis, autoimmune hepatitis, chronic fatigue immune dysfunction syndrome (CFIDS), chronic inflammatory bowel disease, chronic inflammatory demyelinating polyneuropathy, Churg-Strauss syndrome, cicatricial pemphigoid, cold agglutinin disease, CResT syndrome, Creutzfeldt-Jakob disease, Crohn's disease, Dejerine-Thomas, Dementia pugilistica, diabetes mellitus, Diffuse Lewy body disease, discoid lupus, disorders of the basal ganglia, disseminated intravascular coagulation, Down's Syndrome in middle age, drug-induced movement disorders, essential mixed Cryoglobulinemia, fibromyalgia-fibromyositis, graft versus host disease, Graves' disease, Guillain-Barré, Hallerrorden-Spatz disease, Hashimoto's thyroiditis, Huntington's Chorea senile chorea, idiopathic pulmonary fibrosis, idiopathic thrombocytopenia purpura (ITP), IgA nephropathy, infantile or juvenile spinal muscular atrophy, insulin dependent diabetes, juvenile arthritis, Kawasaki's pathology, lesions of the corticospinal system, Leukemias, Hodgkin's lymphoma, non-Hodgkin's lymphoma, lichen planus, Ménière's disease, mixed connective tissue disease, multiple sclerosis, multiple systems degenerations (Mencel, Dejerine-Thomas, Shy-Drager, Machado-Joseph), myasthenia gravis, neurogenic muscular, Parkinson's disease, pemphigus vulgaris, pernicious anemia, polyarteritis nodosa, polychondritis, polyglandular syndromes, polymyalgia rheumatica, polymyositis dermatomyositis, primary agammaglobulinemia, primary biliary cirrhosis, Progressive supranuclear palsy, psoriasis, Raynaud's phenomenon, Reiter's syndrome, rheumatic fever, rheumatoid arthritis, sarcoidosis, scleroderma, Senile Dementia of Lewy body type, Sjögren's syndrome, stiff-man syndrome, Subacute sclerosing panencephalitis, systemic disorders (Refsum's disease, abetalipoprotemia, ataxia, telangiectasia, mitochondrial multi-system disorder), systemic lupus erythematosus (SLE), Takayasu arteritis, temporal arteritis/giant cell arteritis, thyroidosis, ulcerative colitis, uveitis, vasculitis, vitiligo, Wegener's granulomatosis, Wernicke-Korsakoff syndrome.
The present invention is also useful in treating graft rejection or graft versus host disease (GVHD). Acute solid organ transplantation rejection occurs in 30% to 60% of patients after lung transplantation and to a lower degree with liver, kidney, heart etc. due to the success of immunosuppressive agents. The lymphocyte (cell)-mediated immune reaction against transplantation antigens is the principal mechanism of acute rejection. A delayed or chronic rejection causes graft destruction in months to years after transplantation and is characterized by vascular destruction leading to necrosis of the transplanted tissue. This rejection is not currently suppressed to any large degree by standard regimens and thus the need for more sustainable immune tolerance is a significant unmet need.
Late graft deterioration occurs occasionally, and this chronic type of rejection often progresses insidiously despite increased immunosuppressive therapy. The pathologic picture differs from that of acute rejection. The arterial endothelium is primarily involved, with extensive proliferation that may gradually occlude the vessel lumen, resulting in ischemia and fibrosis of the graft.
Immunosuppressants are currently widely used to control the rejection reaction and are primarily responsible for the success of transplantation. However, these drugs suppress all immunologic reactions, thus making overwhelming infection the leading cause of death in transplant recipients.
Existing immunosuppressant treatment can differ in the case of different types of transplants. Liver allografts are less aggressively rejected than other organ allografts. For example, hyperacute rejection of a liver transplant does not occur invariably in patients who were presensitized to HLA antigens or ABO incompatibilities. Typical immunosuppressive therapy in an adult involves using cyclosporine, usually given IV at 4 to 6 mg/kg/day starting at the time of transplantation and then 8 to 14 mg/kg/day po when feeding is tolerated. Doses are adjusted, downward if renal dysfunction occurs, and blood levels are used as approximate measures of adequate dosage.
In heart transplantation, immunosuppressive regimens are similar to those for kidney or liver transplantation. However, in lung and heart-lung transplants acute rejection occurs in >80% of patients but may be successfully managed. Patients are treated with corticosteroids, given rapidly IV in high dosage, ATG, or OKT3. Prophylactic ALG or OKT3 is also frequently given during the first two post-transplant weeks. Pancreas transplantation is unique among the vascularized organ transplants: instead of being used to save a life, it attempts to stabilize or prevent the devastating target organ complications of type I diabetes. Because the recipient exchanges the risks of insulin injection with the risks of immunosuppression, pancreas transplantation has been generally limited primarily to patients who already need to receive immunosuppressive drugs (i.e., diabetics with renal failure who are receiving a kidney transplant).
Patients with acute myeloid or lymphoblastic leukemia may benefit from bone marrow transplant (BMT). Pediatric BMT has expanded because of its potential for curing children with genetic diseases (e.g., thalassemia, sickle cell anemia, immunodeficiencies, inborn errors of metabolism). Another option for BMT is autologous transplantation (removal of a patient's own marrow when a complete remission has been induced, followed by ablative treatment of the patient with the hope of destruction of any residual tumor and rescue with the patient's own bone marrow). Since an autograft is used, no immunosuppression is necessary other than the short-term high-dose chemotherapy used for tumor eradication and bone marrow ablation; posttransplant problems with GVHD are minimal.
The rejection rate is <5% in transplants for leukemia patients from HLA-identical donors. For multiply transfused patients with aplastic anemia, the rejection rate has also been significantly decreased because of increased immunosuppression during transplant induction. Nonetheless, complications can arise including rejection by the host of the marrow graft, acute GVHD, and infections. Later complications include chronic GVHD, prolonged imnmunodeficiency, and disease recurrence.
Numerous other transplantations can be made more effective with the treatment of the present invention. Examples include, corneal transplantation, skin allografts, cartilage allografts, bone grafts, and small bowel transplants.
A host of other disorders can be treated more effectively using the methods of the present invention. For example, cutaneous T cell lymphoma is a disease in which T lymphocytes become malignant and affect the skin. Three kinds of treatment are commonly used: radiation; chemotherapy; and photopheresis. Treatment of cutaneous T cell lymphoma depends on the stage of the disease, and the patient's age and overall health. Standard treatment may be considered because of its effectiveness in patients in past studies, or participation in a clinical trial may be considered. Most patients with cutaneous T cell lymphoma are not cured with standard therapy and some standard treatments may have more side effects than are desired. Treatment using the method of the present invention can be used in the treatment of this disease as well.
The methods of the present invention may also be used in implant surgery, for example, with implant surgery commonly performed in cosmetic or non-cosmetic plastic surgery. Such implants may include dental, fat grafting, for example to the cheeks, lips and buttocks, facial implants, including those to the nose, cheeks, forehead, chin and skull, buttocks implants, breast implants, etc. Other implants include, but are not limited to, corneal ring, cortical, orbital, cochlear, muscle (all muscles, including pectoral, gluteal, abdominal, gastrocnemius, soleus, bicep, tricep), alloplastic joint and bone replacement, bone repair implants (screws, rods, beams, bars, springs), metal plates, spinal, vertebral hair; botox/collagen/restylane/perlane injections, penile implants, prostate seed implants, breast implants (cosmetic and reconstructive), intrauterine devices, hormonal implants; fetal or stem cell implantation, pacemaker, defibrillator, artificial arteries/veins/valves, and artificial organs.
Autoimmune diseases can also be more effectively treated using the methods of the present invention. These are diseases in which the immune system produces autoantibodies to an endogenous antigen, with consequent injury to tissues. Individuals may be identified as having a disease by several methods, including, but not limited to, HLA linkage typing, blood or serum-based assays, or identification of genetic variants, e.g., single nucleotide polymorphisms (SNPs). For example, once an individual is determined to have the HLA DR4 linkage and has been diagnosed to have rheumatoid arthritis, T reg treatment can be prescribed. Other HLA alleles, also known as MHC alleles, that are associated with autoimmune diseases include B27 (Ankylosing spondylitis); DQA1*0501 and DQB1*0201 (Celiac disease); DRB1*03, DRB1*04, DQB1*0201, DQB1*0302, and DMA*0101 (Type I Diabetes); and Cw6 (Psoriasis). These alleles may also be used to determine whether an individual is experiencing an autoimmune disease and, thus, whether T reg treatment may be efficacious.
Blood- or serum-based assays may be used to assess predisposition to a disease. There is, for example, an assay that detects the presence of autonuclear antibodies in serum, which may lead to the onset of lupus. Serum-based assays also exist for predicting autoimmune myocarditis. In addition, serum-based assays may be used to determine insulin levels (diabetes) or liver or heart enzymes for other diseases. T3 levels may be predictive of Hashimotos thyroiditis. After an individual is determined to be having a disease using a blood or serum-based assay, the, methods of the present invention may be used to prevent, or delay the onset of, or reduce the effects of these diseases. Individuals may be identified as being predisposed for disease through the identification of genetic variations, including, but not limited to, SNPs. Thus, in a further aspect of the invention, a determination is first made that a patient has an autoimmune disorder or is predisposed to one and that patient is then prescribed treatment with T regs.
The methods of this invention are also applicable to the treatment of atopic diseases, which are allergic diseases in which individuals are very sensitive to extrinsic allergens. Atopic diseases include, but are not limited to, atopic dermatitis, extrinsic bronchial asthma, urticaria, allergic rhinitis, allergic enterogastritis and the like. Standard diagnostic tests can be used to determine whether a patient has a disorder of the type described above.
The following examples are provided to illustrate but not limit the claimed invention. All references cited herein are hereby incorporated herein by reference.
EXAMPLE 1
Apoptotic Induction Via 8MOP/UVA
Normal donor human leukocytes were passed over Ficoll-paque and PBMC collected and washed before placing at approximately 10 7 cells/ml in a T-75 tissue culture flask; To this flask 200 ng/ml 8-MOP was added before UVA irradiation (˜3 J/cm 2 ). Cells were quickly removed from the flask, in order to avoid adherence, and placed at the appropriate concentration for Treg generation.
Treg Generation
Normal donor human leukocytes were passed over Ficoll-paque and PBMC were collected. T lymphocytes were purified from PBMCs using magnetically activated cell sorter columns and CD4 + negative selection antibody cocktail (Miltenyi Biotec). The purified naive CD4 T cells were co-incubated with ECP-treated PBMCs at a 2:1 ratio (CD4:PBMCs) with 20 ng/ml IL-10 for 8 days ( FIG. 1A ). After 8 days, the CD4 + T cells were purified using MACs and CD4 positive selection antibody cocktail (Miltenyi Biotec). IL-10 is not required but, in some instances, induces a more consistent phenotype.
Treg Evaluation
Treg suppressive activity was evaluated by a secondary mixed lymphocyte reaction (“MLR”) ( FIG. 1B ). Syngeneic CD4 + T cells were placed in a 96 well plate at 10,000, cells/well. Allogeneic dendritic cells were added to the well at 2000 cells per well. The Tregs were titrated into the MLR starting at a ratio of 1 Treg cell to 4 responder T cells. Proliferation was measured on day 5 by bromodeoxyuridine (“BRDU”) incorporation using Roche's Cell Proliferation BRDU chemiluminescent ELISA. Chemiluminescence was measured using TopCount (Perkin Elmer).
EXAMPLE 2
T Reg Activity Is Found In Generation Of T cells By The Present Method
CD4+ T cells were incubated with ECP treated peripheral blood cells for 8 days in the presence of 20 ng/mL IL-10. T regs were purified from the culture using MACs and CD4 positive selection antibody cocktail (Miltenyi Biotec). To assess their regulatory activity, the T regs were then added into an ML consisting of 10,000 syngeneic CD4+ T cells and 2000 allogeneic dendritic cells. Proliferation in these cultures was measured on day 5 by BRDU incorporation. The results are shown in FIG. 2 .
EXAMPLE 3
T Reg Activity Is Found In Generation Of T cells By The Present Method
Tr1 cells were generated by incubating CD4+ T cells in the presence of 20 ng/ml IL-10. T regs were generated by incubating CD4+ T cells with ECP treated peripheral blood cells for 8 days in the presence of 20 ng/ml IL-10. T regs were purified from the culture using MACs and CD4 positive selection antibody cocktail (Miltenyi Biotec). To assess their regulatory activity, the T regs were then added into an MLR consisting of 10,000 syngeneic CD4+ T cells and 2000 allogeneic dendritic cells. Proliferation in these cultures was measured on day 5 by BRDU incorporation. The results are shown in FIG. 3 .
EXAMPLE 4
T Reg Phenotype Is Found In Generation Of T Cells With The Present Method
CD4+ T cells were incubated with ECP treated peripheral blood cells for 8 days in the presence of 20 ng/mL IL-10. T regs were purified from the culture using MACs and CD4 positive selection antibody cocktail (Miltenyi Biotec). The T regs were then added to an MLR consisting of 10,000 syngeneic CD4+ T cells and 2000 allogeneic dendritic cells. IL-2 was added to the MLR at 2 ng/ml. Proliferation in these cultures was measured on day 5 by BRDU incorporation. The results are shown in FIG. 4 .
EXAMPLE 5
T Reg Phenotype Is Found In Generation Of T Cells With The Present Method
Tregs generated by co-incubation with ECP-treated PBMCs were evaluated in a MLR using a 24-well transwell insert system (Nunc Tissue Culture 0.2 μM Anopore Insert system #136935). A MLR consisting of 500,000 syngeneic CD4+ T cells and 100,000 allogeneic dendritic cells were placed in the bottom portion of the transwell. 250,000 Tregs were placed in either the transwell insert or directly into the bottom well with the responder T cells and allogeneic dendritic cells. On day 5, the inserts were removed and proliferation was measured on day 5 by BRDU incorporation. The results are shown in FIG. 5 .
EXAMPLE 6
Mouse Model In Vivo Application) (Prophetic)
Mice
Male C3H/HeJ (C3H; H2k), (B6XC3H)F1 (H2bXk), (B6XDBA/2)F1 (H2bXd), C57BU6 (B6; H2b), and CBA/JCr (CBA; H2k) mice will be purchased from the National Cancer Institute Research and Development Center (Frederick, Md.). B10.BR (H2k) mice will be purchased from the Jackson Laboratories (Bar Harbour, Me.). Mice used for experiments will be between 6-10 weeks of age, and housed in sterile microisolator cages within a specific pathogen-free facility, receiving autoclaved food and water ad libitum.
Media
Phosphate-buffered saline (PBS) supplemented with 0.1% bovine serum albumin (BSA; Sigma Chemical Co., St Louis, Mo.) will be used for all in vitro manipulations of the donor bone marrow and lymphocytes. Immediately prior to injection, the cells will be washed and resuspended in PBS alone. For maintaining cell lines and for in vitro assays, RPMI 1640 medium (Mediatech, Herndon, Va.) will be used, supplemented with 10% fetal bovine serum (FBS; GIBCO, Grand Island, N.Y.), 2 mmol/L L-glutamine, 50 IU/mL penicillin, and 50 μg/mL streptomycin.
Antibodies
Experimental Photopheresis
Splenocytes will be harvested from syngeneic littermate healthy mice and made into single cell suspension by grinding with the back end of a syringe in PBS. These cells will be re-suspended and cells washed twice with PBS before re-suspending at 12.5×10 6 cells/mL PBS. Upon washing cells they will be resuspended in ice-cold medium and seeded at approximately 106 cells/ml in a T75 flask. Psoralen (UVADEX solution) will be added to a final concentration of 200 ng/ml, which is a 100 fold dilution from the stock solution provided by Therakos. The flask will be placed lying down in the UVA irradiation chamber and given approximately 1.5 J/cm 2 of light which corresponds to 1.5 minutes of bottom light when the tray is 6 cm from the light, source. Cells will be quickly removed from the flask to avoid adherence and placed at the appropriate concentration for injection. If there is adherence, the flask will be gently scraped or tapped to remove most of the cells.
Bone Marrow Transplantation
Bone marrow will be harvested from the tibia and femurs of donor mice by flushing with PBS containing 0.01% BSA (PBS/BSA). Bone marrow cells will be depleted of T cells using an anti-Thy 1.2 nAb (J1j; American Type Culture Collection, Rockville, Md.) at a 1:100 dilution and guinea pig complement (Rockland Immunochemicals, Gilbertsville, Pa.) at a dilution of 1:6 for 45 minutes at 37° C. Lymphocytes will be isolated from spleens and lymph nodes of donor mice. Splenocytes will be treated with Gey's balanced salt lysing solution containing 0.7% ammonium chloride (NH 4 Cl) to remove red blood cells (RBCs). After RBC depletion, spleen and lymph node cells will be pooled and depleted of B cells by panning on a plastic Petri dish, precoated with a 5 mg/ml dilution of goat anti-mouse IgG for 1 hour at 4° C. These treatments are expected to result in donor populations of approximately 90%-95% CD3+ cells, as quantitated by fluorescent flow cytometry. T cells subsets will be then isolated via negative selection using either anti-CD8 (3.168) or anti-CD4 mAb (RL172) and complement. These treatments are expected to reduce the targeted T cell subset populations to background levels, as determined by flow cytometric analysis. Recipient mice will be exposed to 13 Gy whole body irradiation from a 137CS source at 1.43 Gy/min, delivered in a split dose of 6.5 Gy each, separated by 3 hours. These mice will be then be transplanted with 2×10 6 anti-Thy 1.2 treated bone marrow cells (ATBM; T cell-depleted) along with the indicated number of appropriate cells (donor CD4 or CD8 enriched T cells), intravenously (i.v.) via the tail vein. Mice will be treated with T regs 1 day before transplantation and again on days 0, 4, 8, and 12 (all at 0.5 mg; i.p.). For GVL experiments, B6 recipient mice will be challenged with an injection of T regs one day before transplantation of donor ATBM and T cells, with a similar schedule of T reg treatment. In both GVHD and GVL experiments, the mice will be checked daily for morbidity and mortality until completion. The data will be pooled firm 2-3 separate experiments, and median survival times (MST) will be determined as the interpolated 50% survival point of a linear regression through all of the day of death data points, including zero. Statistical comparisons for survival between experimental groups will be performed by the nonparametric Wilcoxon signed rank test. Significance for weight comparisons will be determined by the T-test at individual time points.
Flow Cytometry
Appropriate pbs in volumes of 25 μL will be incubated with 2-5×10 5 cells in the wells of a 96-well U-bottom microplate at 4° C. for 30 minutes, centrifuged at 1500 rpm for 3 minutes, and washed with PBS containing 0.1% BSA and 0.01% sodium azide (wash buffer). The percentage positive cells, and the arithmetic mean fluorescence intensity will be calculated for each sample.
Pathological Analysis
Full thickness ear biopsies (3×2 mm) will be sampled from each mouse of the various treatment groups and immediately fixed in 4% glutaraldehyde overnight and then rinsed with 0.1 M sodium cacodylate buffer (pH 7.4). Tissues will be post-fixed with 2% osmium tetroxide for 2 h, dehydrated in graded ethanol and embedded in Epon 812. One-micron-thick sections will be cut with a Porter-Blum MT2B ultramicrotome, stained with toluidine blue, and finally dipped in 95% ethanol for light microscopic analysis. The number of dyskeratotic epidermal cells/linear mm, as previously determined, will be counted under a ×100 objective and a ×10 eye piece of a light microscope. More than ten linear mm of the epidermis will be assessed in each animal and each time point. The analysis will be performed under blinded conditions as to the treatment groups.
Additional animal models for T regs are provided for instance by 20030157073; Kohm, A et al. (2002); Tang, Q et al. (2004); and Schwarz, A et al. (2004).
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Nishida et al. (1999) “Specific aqueous humor factors induce activation of regulatory T cells” Invest Ophthalmol Vis Sci 410:2268-2274 Nishida et al. (2004) “Anti-inflammatory effects of alpha-melanocyte-stimulating hormone against rat endotoxin-induced uveitis and the time course of inflammatory agents in aqueous humor” Int Immunopharmacol 4:1059-1066 O'Garra et al. (2003) “In vitro generation of IL-10-producing regulatory CD4+ T cells is induced by immunosuppressive drugs and inhibited by Th1- and Th2-inducing cytokines” Immunol Lett 85:135-139 Ohtsuka et al. (1999a) “Cytokine-mediated down-regulation of B cell activity in SLE: effects of interleukin-2 and transforming growth factor-beta” Lupus 8:95-102 Ohtsuka et al. (1999b) “The relationship between defects in lymphocyte production of transforming growth factor-beta1 in systemic lupus erythematosus and disease activity or severity” Lupus 8:90-94 Pedersen et al. (2004) “Induction of regulatory dendritic cells by dexamethasone and 1alpha, 25-Dihydroxyvitamin D(3)” Immunol Lett 91:63-69 Penna et al. (2000) “1 Alpha, 25-dihydroxyvitamin D3 inhibits differentiation, maturation, activation, and survival of dendritic cells leading to impaired alloreactive T cell activation” J Immunol 164:2405-2411 Roncarolo et al. (2001) “Type 1 T regulatory cells” Immunol Rev 182:68-79 Saas et al. (2002) “Cell-based therapy approaches using dying cells: from tumour immunotherapy to transplantation tolerance induction” Expert Opin Biol Ther 2:249-263 Sakaguchi et al. (2001) “Immunologic tolerance maintained by CD25+ CD4+ regulatory T cells: their common role in controlling autoimmunity, tumor immunity, and transplantation tolerance” Immunol Rev 182:18-32 Salvioli et al. (1997) FEBS Let 411:77-82 Savill et al. (2002) “A blast from the past: clearance of apoptotic cells regulates immune responses” Nat Rev Immunol 2:965-975 Schwartz et al. (2000) “Evidence for functional relevance of CTLA-4 in ultraviolet-radiation-induced tolerance” J Immunol 165:1824-1831 Stohl et al. (1999) “Impaired cytotoxic T lymphocyte activity in systemic lupus erythematosus following in vitro polyclonal T cell stimulation: a contributory role for non-T cells” Lupus 8:293-299 Streilein et al. “Neural control of ocular immune privilege” Ann N Y Acad Sci 917:297-306 Tang et al. (2004) “In vitro-expanded antigen-specific regulatory T cells suppress autoimmune diabetes” J Exp Med 199:1455-1465 Taylor (1999) “Ocular immunosuppressive microenvironment” 73:72-89 Taylor (2003) “Modulation of regulatory T cell immunity by the neuropeptide alpha-melanocyte stimulating hormone” Cell Mol Biol (Noisy-le-grand) 49:143-149 Taylor (2005) “The immunomodulating neuropeptide alpha-melanocyte-stimulating hormone (alpha-MSH) suppresses LPS-stimulated TLA4 with IRAK-M in macrophages” J Neuroimmunol 162:43-50 Taylor et al. (1992) “Identification of alpha-melanocyte stimulating hormone as a potential immunosuppressive factor in aqueous humor” Curr Eye Res 11:1199-1206 Taylor et al. (1994a) “Immunoreactive vasoactive intestinal peptide contributes to the immunosuppressive activity of normal aqueous humor” J Immunol 153:1080-1086 Taylor et al. (1994b) “Alpha-melanocyte-stimulating hormone suppresses antigen-stimulated T cell production of gamma-interferon” Neuroimmunomodulation 1:188-194 Taylor et al. (1996) “Inhibition of antigen-stimulated effector T cells by human cerebrospinal fluid” Neuroimmunomodulation 3:112-118 Taylor. et al. (2003) “Somatostatin is an immunosuppressive factor in aqueous humor” Invest Ophthalmol Vis Sci 44:2644-2629 Teiger. et al. (1996) J Clin Invest 97:2891-97 Willheim et al. “Regulatory effects of 1alpha, 25-dihydroxyvitamin D3 on the cytokine production of human peripheral blood lymphocytes” J Clin Endocrinol Metab 84:3739-3744 Yamagiwa (2001) “A role for TGF-beta in the generation and expansion of CD4+CD25+ regulatory T cells from human peripheral blood” J Immunol 166:7282-7289 Zeller et al. (1999) “Induction of CD4+ T cell alloantigen-specific hyporesponsiveness by IL-10 and TGF-beta” J Immunol 163:3684-3691 Zheng et al. (2002) “Generation ex vivo of TGF-beta-producing regulatory T cells from CD4+CD2-precursors” J Immunol 169:4183-4189 Zheng et al. (2004) “CD4+ and CD8+ regulatory T cells generated ex vivo with IL-2 and TGF-beta suppress a stimulatory graft-versus-host disease with a lupus-like syndrome” J Immunol 172:1531-1539
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Many cell types in the body can remove apoptotic and cellular debris from tissues; however, the professional phagocyte, or antigen presenting cell (“APC”), has a high capacity to do so. The recognition of apoptotic cells (“ACs”) occurs via a series of evolutionarily-conserved, AC associated molecular-pattern receptors (“ACAMPRs”) on APCs that recognize and bind corresponding apoptotic-cell-associated molecular patterns (“ACAMPs”). These receptors recognize ligands such as phosphotidyl serine and oxidized lipids found on apoptotic cells. Savill et al. (2002); and Gregory et al. (2004).
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RELATED APPLICATION(S)
[0001] This application claims the benefit of U.S. Provisional application No. 61/972,192 filed Mar. 28, 2014, which is incorporated by reference in its entirety herein.
TECHNICAL FIELD
[0002] The present invention relates to color sample display devices in the form of a color fan deck for paint products where paint is illustrated on one or both sides of the fan blades of the fan deck.
BACKGROUND
[0003] Paint colors often are displayed on color swatches mounted on a flat planar base, multiple ones of which are joined together to form a deck or a fan deck with fan blades that are pivotally spread or fanned to display color. Each blade in the deck has one or more color swatches or painted areas that display one or more colors. The blades with the paint coated swatches or painted areas on one or both sides of the blades form a fan deck with potentially large numbers of blades and colors. The blades are held at one end of the deck and pivot around a fastener such as a screw or rivet such that the blades can swivel around a longitudinal body of the fastener to display colors to the user. A fan deck is an effective way to display large numbers of colors and color tones.
[0004] Advantageously, a fan deck can display many colors with many blades. Users typically will swivel one fan blade out from the fan deck and hold the fan deck by that blade when evaluating a color such as by holding the fan blade up to a wall or other surface to be painted. A problem exists in that the fastener pivotally holding the blades has to be removed, sometimes by destroying the fastener and/or the blades, to free the blades to add new or revised blades with revised colors to the fan deck or to replace blades already in the fan deck. Hours can be spent in unfastening and then re-fastening the fastener to slip in a new blade or revised blade, and care must be taken to not lose or misarrange fan blades during the time the fastener is not secure. Moreover, the fan blades themselves must have sufficient strength to withstand the rigors of use including supporting the weight of the fan deck during color evaluation by a user.
[0005] An object of the fan deck described herein is to provide fan blades for a changeable color fan deck with a plurality of blades that can be changed by adding to the fan blades of the deck or removing fan blades of the deck without removing the fastener holding the individual blades pivotally together.
[0006] Other objects will become more apparent with reference to the description set forth below.
SUMMARY
[0007] Generally speaking, pursuant to these various embodiments, the fan blade and color display fan deck described herein provide a changeable color display product because the fan deck blades can be added to and removed from the fan deck without opening the fastener to which the fan blades are pivotally attached. Despite being removable from the fan deck, the blades can withstand the normal wear and tear associated with use in a color fan deck such as supporting the weight of the whole fan deck when a user holds an individual fan blade.
[0008] In one approach, the blades have openings or holes surrounding the fastener which has a body width. The fastener, for example, may be a post with heads at each end of the posts or a ring. A planar connector of the fan blade defines a channel extending from a first channel end at the opening around which the blade pivots to a second channel end at an edge of the fan blade through which the fastener body moves when adding or removing a fan blade. The channel permits removal and/or addition of the fan blade from/to the fastener to effect a changing of the color display fan deck without the fastener being opened or removed from the color display fan deck. In other words, the channel provides a reusable path for the fastener to slide to and from the opening when adding the blade to and removing the blade from the fan deck. In one aspect, an overlay flap may extend from the connector and fold over at least a portion of the channel without covering the opening in the planar connector around which the blades pivot.
[0009] In one aspect, a portion of the channel (such as a shoulder in the channel) has a width less than the width of the body of the fastener to keep the fan blade from sliding off of the fastener and inadvertently separating from the fastener. This portion also has sufficient stiffness to keep the blade from twisting away from the fastener. The planar connector has flexibility and resiliency to flex sufficiently to permit opening the channel to a width larger than the body width of the fastener to allow removal and/or addition of the fan blade from/to the fastener when desired. The planar connector has a deformation strength sufficient to hold the fan deck's weight without deformation to prevent separation of the fan deck from the fastener when the fan deck is held by one blade having the opening and channel. This feature allows the fan deck to be updated with new or different color tones as may be available from a given paint supplier without dismantling the whole fan deck, risking mixing or losing fan blades.
[0010] In one example, the planar connector will hold a fan deck when the fan deck has a weight of from about 1.5 to about 30 ounces excluding the weight of the blade by which the fan deck is held. Such strength thereby allows a user to hold a fan blade apart from the other fan blades, for example to evaluate a color, without the fan blade separating from the fan deck. In one aspect, the planar connector may comprise an extension adhered to the planar base of the fan blade.
[0011] In a further aspect, a polymeric film may be added to the fan blade, surrounding the opening and/or the channel without covering the opening around which the blade pivots, to provide additional strength to the planar connector to support the fan deck. In another aspect, the film can provide an overlay flap that folds over itself, for example, along a score line, to releasably adhere to, cover, and secure at least a portion of the channel to further prevent inadvertent removal of the fan blade from the fan deck.
[0012] Also disclosed herein is a method of revising a color fan deck having a plurality of fan blades as described above without removing the fastener that pivotally holds the fan blades together. The method includes moving the fastener through the channel in the planar connector so that the planar connector surrounds the fastener, where the planar connector has sufficient strength to hold the fan deck's weight without deformation to prevent separation of the fan deck from the fastener when the fan deck is held by one blade having the opening and channel.
[0013] A method for making the fan blades is also described herein.
[0014] The blades of the fan decks described herein may be any known in the art including a swatch bearing blade including a flat elongated base paper laminated on one or both sides with a paint coated polymeric film as described in U.S. Pat. No. 8,007,621, or the blade may be a paint coated paper blade as described in United States Patent Application Publication No. 2014/0045149 filed Aug. 5, 2013, both of which are incorporated by reference as if fully rewritten herein.
BRIEF DESCRIPTION OF THE DRAWINGS
[0015] FIG. 1 is a top view of a fan deck with the individual blades precisely aligned on top of each other.
[0016] FIG. 2 is a top view of a color fan deck with the blades rotatably or pivotally moved so that the color on each side of the blade can be seen.
[0017] FIG. 3 is a side plan view of one example fan blade according to various embodiments of the invention.
[0018] FIG. 4 is a side view of one example fan deck according to various embodiments of the invention.
[0019] FIG. 5 is a top view of one example fan blade according to various embodiments of the invention.
[0020] FIG. 6 is a top view of one example fan blade having a polymeric film according to various embodiments of the invention.
[0021] FIG. 7 is a schematic view showing dimensions of one example design for the film layer of the example fan blade of FIG. 6 .
[0022] FIG. 8 is a schematic view showing dimensions of one example design for the film layer having the optional foldable flap of the example fan blade of FIG. 6 .
[0023] FIG. 9 is a side plan view of one example fan blade according to various embodiments of the invention.
[0024] FIG. 10 is a top view of one example fan blade having a polymeric tongue extending from a fan blade according to various embodiments of the invention.
[0025] FIG. 11 is a side plan view of one example fan blade according to various embodiments of the invention.
[0026] FIG. 12 is a schematic view showing dimensions of one example design for the polymeric tongue of the example fan blade of FIG. 10 .
[0027] FIG. 13 is a schematic view showing dimensions of one example design for the polymeric tongue having the optional foldable flap of the example fan blade of FIG. 10 .
[0028] FIG. 14 is a flow diagram of example methods of making fan blades according to various embodiments of the invention.
[0029] Skilled artisans will appreciate that elements in the figures are illustrated for simplicity and clarity and have not necessarily been drawn to scale. For example, the dimensions and/or relative positioning of some of the elements in the figures may be exaggerated relative to other elements to help to improve understanding of various embodiments of the present invention. Also, common but well-understood elements that are useful or necessary in a commercially feasible embodiment are often not depicted in order to facilitate a less obstructed view of these various embodiments. It will further be appreciated that certain actions and/or steps may be described or depicted in a particular order of occurrence while those skilled in the art will understand that such specificity with respect to sequence is not actually required. It will also be understood that the terms and expressions used herein have the ordinary technical meaning as is accorded to such terms and expressions by persons skilled in the technical field as set forth above except where different specific meanings have otherwise been set forth herein.
DETAILED DESCRIPTION
[0030] Turning now to the drawings and, in particular, FIGS. 1-4 , an example color display fan deck 100 will be described in accordance with various aspects of the invention. The color display fan deck 100 includes a plurality of fan blades 105 , individual ones 107 , 108 , and 109 of which include a planar base 115 with a top surface 120 and a bottom surface 130 . In one example, the fan blades can be between about one and four inches wide and between about two and eight inches in length. The planar base 115 illustrates paint color on at least one side of the fan blade 107 . The fan blade 107 further includes a planar connector 150 at an edge 152 of the at least one individual fan blade 107 .
[0031] The fan blade 107 itself can be constructed in any number of ways, including any of those known in the art. With reference to FIGS. 3 and 9 , two such examples will be described. In FIG. 3 , the planar base 115 of the fan blade includes a top surface 120 and a bottom surface 130 . The top surface 120 includes a paint layer 125 suitable to display the paint color when the fan blade 107 is swiveled away from the other fan blades 108 and 109 of the fan deck 100 . The paint layer 125 is disposed on a paper layer 140 . Similarly, a separate paint layer 135 is disposed on a bottom surface 130 of the planar base 115 . The second paint layer 135 may be the same color as the first paint layer 125 or a different color. United States Patent Application Publication No. 2014/0045149 describes one method of making a paint chip or fan blade according to the example of FIG. 3 , which document is incorporated by reference herein. Another example fan blade is described with reference to FIG. 9 . In this example, the planar base starts with a film layer 142 . A layer of adhesive 144 is applied to the film layer 142 so that a paper layer 146 can be adhered to the film layer 142 . The paper may be a 10 point paper sufficient to provide a stiffness to the fan blade and provide sufficient color backing so that the displayed paint color is true. Accordingly, a paint layer 148 is applied to the paper layer 146 . A clear top coat 149 is applied to the paint layer 148 to help maintain the color integrity of the paint layer 148 . U.S. Pat. No. 8,007,621 describes in more detail one approach to creating a fan blade such as in the example of FIG. 9 , which patent is incorporated by reference herein as though fully rewritten.
[0032] A fan deck 100 includes a fastener 160 , which, as illustrated in FIG. 4 , includes a body 162 and ends 164 . The fastener 160 ends or heads 164 are wider than the fastener body 162 to secure the fan blades 105 within the fan deck 100 . In a different approach, the fastener 160 may instead be a ring similar to a key ring to secure the plurality of fan blades 105 within the fan deck 100 .
[0033] Referring now to the example of FIG. 5 , the planar connector 550 includes at least one opening 570 . The opening 570 has an opening width that surrounds the fastener 160 at the fastener body 162 to permit the individual fan blade 507 to be swivelably held within the fan deck 100 . For example, the opening 570 can be between about 0.20 inch and about 0.50 inch wide. By one approach, the planar connector 550 of the individual fan blade 507 defines a channel 572 extending from a channel end 574 to the at least one opening 570 to permit removal and/or addition of the fan blade 507 from/to the fastener 160 . This channel 572 can effect a changing of the fan deck 100 without the fastener 160 being opened or removed from the fan deck 100 .
[0034] At least a portion of the channel 572 has a width less than the body width of the fastener 160 . In the example of FIG. 5 , the channel 572 defines a shoulder 576 or narrowing next to the opening 570 . The narrowing or shoulder 576 pinches around the fastener 160 so that the fan blade 507 stays secured on the fastener 160 . The channel 572 may define further or other narrowings such as that at narrowing portion 577 to further secure the fan blade 507 to the fastener 160 . The planar connector 550 has flexibility and resiliency to flex efficiently to permit opening the channel 572 effective to allow removal and/or addition of the fan blade 507 from/to the fastener 160 and a deformation strength sufficient to hold the fan deck 100 's weight without deformation. This prevents separation of the fan deck 100 from the fastener 160 when the fan deck 100 is held by one blade 507 having the opening 570 and the channel 572 .
[0035] In the example of FIG. 5 , the planar connector 550 is integral with the body of the fan blade 507 . In other words, the opening 570 and channel 572 are cut from the body of the fan blade 507 . In this embodiment, the portion 580 of the fan blade 507 comprises a tongue that wraps around the fastener 160 and together with a further cut portion 582 of the fan blade 507 define the channel 572 through which the fastener 160 passes when adding the fan blade 507 to the fan deck 100 , or removing it from the fan deck 100 . In this way, the fastener 160 can pass through the edge 552 of the fan blade 507 via the channel 572 and sit within the opening 570 . In various embodiments, the planar connector 550 has a thickness of from about 0.5 mils to about 100 mils (about 0.0005 inch to about 0.10 inch) wherein the thickness corresponds to the thickness of the fan blade 507 . The thickness and materials of the fan blade 507 provide the deformation strength such that the planar connector 550 will hold a fan deck 100 when the fan deck 100 is held by the individual blade having the opening 570 and the channel 572 . A typical fan deck 100 that will include such a fan blade has a weight from about 1.5 to about 30 ounces excluding weight of the individual blade by which the fan deck 100 is held.
[0036] Referring to FIGS. 3 , 6 , and 7 , in one aspect, a polymeric film 602 is disposed on one or both sides of the planar connector 550 such that the polymeric film 602 surrounds the opening 570 and the channel 572 . In this example, the polymeric film 602 strengthens the planar connector 550 to provide additional strength such that the fan blade 507 is better able to support the weight of the fan deck 100 without accidently coming loose during regular use by a user. For example, the polymeric film 602 can have a thickness from about five point to about seven point depending on the fan blade 507 to which the polymeric 602 is applied. Inherently stronger fan blades 507 can use polymeric films 602 having a smaller thickness or no polymeric film at all. The polymeric film 602 in different embodiments may be selected from the group consisting of polyethylene, polypropylene, and polyethylene terephthalate.
[0037] Referring to FIG. 3 , the polymeric film 602 can be disposed on merely one side of the planar base 115 . The polymeric film 602 may be adhered to the planar base 115 using an adhesive 603 . In other approaches, the polymeric film 602 may be laminated to the fan blade 507 to effect bonding between the polymeric film and fan blade 507 , in which case a layer of one to four mil (0.001 to 0.004 inch) thick paper 603 is disposed between the film 602 and the fan blade 507 to facilitate adhesion. The thickness of the polymeric film can be between about 0.5 mils to about 100 mils (about 0.0005 inch to about 0.1 inch). By another approach, a second polymeric film 604 may be applied to the back or bottom of the fan blade 507 separately from or in addition to the polymeric film 602 applied to the top or front portion of the fan blade 507 . In still a further approach, the polymeric film may be wrapped around the edge of the fan blade resulting in a portion of polymeric film 606 wrapping around the edge of the fan blade 507 . The dimensions for one example polymeric film that can be applied to a fan blade are illustrated in FIG. 7 . In this case, the opening and channel formed by the polymeric film 602 match that of the fan blade 507 . In one approach that can simplify the manufacturing process, the polymeric film 602 without a pre-cut opening or channel can be applied to the fan blade 507 , which combined polymeric film and fan blade are die-cut once at the same time to provide the opening 570 and channel 572 used for the planar connector 550 . In this case, the planar connector 550 will include a portion of at least the fan blade 507 and the polymeric film 602 having therefore a combined thickness from about 1 mil to about 200 mils (about 0.001 inch to about 0.20 inch). The planar connector 550 having this combination of elements will hold the fan deck 100 when the fan deck 100 is held by the one individual blade 507 having the opening 570 and channel 572 through both the polymeric film 602 and the fan blade 507 . The fan deck has a weight from about 1.5 to about 30 ounces excluding weight of the individual fan blade by which the fan deck 100 is held.
[0038] With reference to FIGS. 6 , 8 , and 9 , another approach includes a foldable overlay flap 621 that is configured to be folded along a fold line 623 , which may be a perforated or scored portion of the film. In the illustrated example, the foldable overlay flap 621 is made of the same polymeric film 602 that is adhered to the fan blade 507 . The overlay flap 621 is removably adhered to cover at least a portion of the channel 572 to block removal of the at least one individual blade 507 from the fastener 160 by blocking movement of the planar connector 550 relative to the fastener 160 . In other words, by adhering the portions of the fan blade and polymeric film that define the channel 572 together, the channel 572 is unlikely to open during regular use such that the fan blade 507 inadvertently becomes removed from the fastener 160 . FIG. 8 illustrates example dimensions for one such approach to having a polymeric film 602 including a foldable overlay flap 621 to secure the channel 572 . FIG. 9 illustrates one such example with the overlay flap adhered to the channel 572 . In this example, the polymeric film 602 is adhered to the planar base 115 using adhesive 603 . The adhesive 603 is a long term and non-removable adhesive to secure the polymeric film 602 to the fan blade 507 . In contrast, a removable adhesive 613 is applied to either the polymeric film surface 602 or to the inside of the overlay flap 621 such that when the overlay flap 621 is folded along a fold line 623 , the removable adhesive 613 adheres the overlay flap 621 to the polymeric film 602 over at least a portion of the channel 572 . In this way, the overlay flap 621 may be readily peeled off of the polymeric film 602 and the channel 572 to allow the individual blade 507 to be removed from or added to a fan deck 100 .
[0039] Turning to FIGS. 10 and 11 , the planar connector 1050 comprises a polymeric tongue 1002 connected to and extending from the edge 1012 of the fan blade 1007 . By one approach, the polymeric tongue 1002 is comprised of the polymeric film such as that described above. In this example, the at least one opening 1070 in the fan blade 1007 is defined not by the fan blade body itself but instead by the polymeric tongue 1002 which extends from the edge 1012 of the fan blade 1007 . Similarly, the channel 1072 is defined by the polymeric tongue 1002 . The channel 1072 may have any of the features described above with respect to the other approaches to the channel including, for example, having a narrowing or shoulder 1076 next to the opening 1070 to help secure the fastener 160 within the opening 1070 . The channel 1072 then will extend to the edge 1052 of the tongue 1002 where the fastener 160 can slide out of the channel end 1074 during removal of the fan blade 1007 from the fan deck 100 .
[0040] Referring to FIG. 11 , the polymeric tongue 1002 can be adhered to the fan blade 1007 using a non-removable adhesive 1003 . As illustrated in FIG. 11 , the polymeric tongue 1002 may be adhered to the back or bottom of the fan blade 1007 , or, as illustrated in FIG. 10 , the polymeric tongue 1002 may be adhered to the top or front of the fan blade 1007 . By still another approach, the polymeric tongue 1002 may be laminated or adhered via legs to both or either of the top and bottom of the fan blade 1007 with the opening 1070 and channel 1072 being positioned above the edge 1012 of the fan blade 1007 . In this approach, the fan blade 1007 need not be die-cut during the manufacturing process; instead the opening 1070 and channel 1072 is only die-cut into the polymeric tongue 1002 either before or after being adhered to the fan blade 1007 . FIG. 12 illustrates one example set of dimensions for the polymeric tongue 1002 , and other dimensions and shapes are possible for the polymeric tongue 1002 . Referring to FIG. 13 , the polymeric tongue 1002 may further include an optional foldable overlay flap 1021 that folds along a line 1023 , which may be a perforated or scored portion of the film, to adhere to and cover at least a portion of the channel 1072 . Accordingly, the flap 1021 can be adhered to the channel 1072 to further strengthen the channel and prevent flexing of the planar connector 1050 to secure the fastener within the opening 1070 . As discussed above, the thickness of the polymeric tongue 1002 and the necessity of having the flap 1021 depends upon, in part, the weight of the fan deck that would be supported by the individual blade 1007 when a user holds the fan deck by the one individual blade 1007 during typical use.
[0041] So configured, an individual fan blade displaying paint on one or both sides is particularly configured to be added to and removed from a color display fan deck without having to open the fastener of the color display fan deck. The configuration or dimensions of the opening and channel of a particular version of the planar connector for the individual fan blade can be tailored to a particular application such that the planar connector 1050 will not deform and the fan blade 1007 will not accidently be removed from the fan deck during typical use. Thus, each of the options described above can be combined in different ways to achieve a satisfactory deformation strength of the planar connector 1050 to support the fan deck. In this way, a color fan deck can be modified and fan blades can be replaced or added to a given fan deck by moving the fastener for a given fan deck through the individual blade's channel so that the opening surrounds the fastener to pivotably secure the individual blade within the fan deck. The planar connector of the individual blade holds the fan deck's weight without deformation to prevent separation of the individual blade from the fastener when the fan deck is held by one individual blade.
[0042] Example methods of making a fan blade for displaying paint color that is removable from a color fan deck having a plurality of fan blades without removing the fastener that pivotably holds the fan blades together will be described with reference to FIG. 14 . One method includes receiving 410 the fan blade that may be made pursuant to any applicable fan blade construction method. The fan blade is die-cut 1420 to define within the fan blade an opening having an opening width configured to surround a fastener to permit the fan blade to be pivotably held with a plurality of other fan blades within a color display fan deck. The die-cutting also defines within the fan blade a planar connector of the fan blade defining a channel that extends from a first channel end at the opening to a second channel end at or near an edge of the fan blade. The channel permits removal and/or addition of the fan blade to/from the fastener to effect a changing of the color display fan deck without the fastener being opened or removed from the color display fan deck. The die-cutting will be adapted to provide cutting the fan blade such that the planar connector having a thickness from thickness of from about 0.5 mils to about 100 mils (about 0.0005 inch to about 0.10 inch) will have a deformation strength sufficient to hold the color display fan decks weight from the fastener without deformation to prevent opening the channel to a width larger than the fasteners width. The planar connector will further have flexibility and resiliency to flex sufficiently to permit opening the channel to a width larger than the fasteners width to allow removable and/or addition of the fan blade from/to the fastener when desired.
[0043] Where a polymeric film is used, the method may include adhering 1415 the polymeric film to one or both sides of the individual blade where the polymeric film surrounds the at least one opening and the channel. The polymeric film may have a width of about five point to about seven point depending on the deformation strength sufficient to hold the fan deck in which the fan blade is contemplated to be used. As discussed above, the polymeric film to be adhered to the fan blade may be one of polyethylene, polypropylene, and polyethylene terephthalate or other suitable material. When using the polymeric film, the step of die-cutting 1420 , the fan blade may further include die-cutting the fan blade together with the polymeric film after the polymeric film has been adhered 1415 to one or both sides of the fan blade. Such an approach would remove the need for precision in aligning the polymeric film having its own opening and channel with the opening and channel of the fan blade.
[0044] In the option where the polymeric film includes an overlay flap, the method may include applying releasable adhesive 1425 to releasably adhere a portion of the polymeric film over at least a portion of the channel. The flap may be folded 1430 where the flap is a portion of the polymeric film over itself to cover at least a portion of the channel. The releasable adhesive adheres the flap of the polymeric film to itself over the portion of the channel.
[0045] Whether the planar connector is made out of the fan blade itself, a combination of the fan blade and the polymeric film, or just out of the polymeric film in the form of a tongue extending from the fan blade, the fan blade is mounted 1435 to a fastener to help create a fan deck. So configured, the fan blades can be readily adapted for use in a fan deck to provide flexibility and provision of color pallets to users and customers without the difficulties in undoing a fastener or otherwise destroying a fan deck in the process of modifying the color pallet. The fan blade may be simply die-cut with a particular channel and opening sufficient to hold the weight of the fan deck, or a further in-line process may be applied to a fan blade manufacturing process to adhere or laminate a polymeric film to the fan blade to provide additional or supplemental strength for the planar connector used to connect the fan blade to the fan deck's fastener.
[0046] Those skilled in the art will recognize that a wide variety of modifications, alterations, and combinations can be made with respect to the above described embodiments without departing from the scope of the invention, and that such modifications, alterations, and combinations are to be viewed as being within the ambit of the inventive concept.
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A fan blade and color display fan deck provide a changeable color display product because the fan deck blades can be added to and removed from the fan deck without opening the fastener to which the fan blades are pivotally attached. Despite being removable from the fan deck, the blades can withstand the normal wear and tear associated with use in a color fan deck such as supporting the weight of the whole fan deck when a user holds an individual fan blade.
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This application claims the benefit of the priority of provisional application 61/212,002, filed Apr. 6 2009, and is a continuation of co-pending application Ser. No. 12/798,547; and said prior applications are hereby incorporated by reference in their entirety.
FIELD OF THE INVENTION
The present invention relates generally to apparatus and method for applying paint to one or more paint pads that have a particular size and or configuration. In particular, a paint tray, including a paint reservoir and one or more paint applicators which can be placed in fluid communication with the paint reservoir, is configured to apply paint onto one or more paint pads suitably matched in size and shape to the paint applicators. The apparatus and method are particularly useful when working near boundaries of areas to be painted.
DESCRIPTION OF THE RELATED ART
Paint pads are used to “cut in” edges of a surface to be painted. In particular, paint pads may be used to paint edges of the surface to be painted that border other surfaces that are not being painted. For example, surfaces to be painted may comprise walls that border a ceiling that is not being painted. A paint pad is used to paint or cut in the walls along border edges up to the ceiling without painting the ceiling. In other examples, a wall may include windows, doors, trim and other elements that are not to be painted. The paint pad is used to paint or cut in the walls along border edges up to the windows, doors, trim and other elements.
In these examples, the shape and dimensions of the paint pad may be somewhat arbitrary. An example of a paint pad suitable for cutting in wall edges is disclosed in U.S. Pat. No. 2,810,148 which shows a paint absorbing pad made from mohair fabric supported on a substantially rigid backing. A user handle, for easy handling while painting, is attached to a base plate. In this example of the paint pad, the base plate, rigid backing and paint absorbing pad are rectangular in shape and the paint absorbing pad is removable from the base plate for replacement with a new paint absorbing pad or for cleaning the paint absorbing pad as may be required. In addition, the example paint pad includes a paint edge follower comprising a pair of wheels rotatably attached to the base plate along a guided or leading edge of the paint pad. In use, the wheels make rolling contact with a guide surface such as a ceiling, wall, door frame, window frame, trim or other feature that is not being painted in order to guide the leading edge of the paint pad as the paint pad is moved linearly with the guide surfaces in order to apply paint onto the surface being painted right up to the border edge between the surface being painted and the guide surface, but without applying any paint onto the guide surface. In the '148 patent example, the paint pad is approximately planar and rectangular in shape and the guided or leading edge of the paint pad is substantially collinear with a line formed by the edge follower which in this example is the rolling contact points made by the wheels with the guide surface.
In a further example, paint pads are available in different sizes and shapes to paint a particular feature such as a window mullion, a molding, trim piece or the like. Moreover, such paint pads do not necessarily include a paint edge follower but instead rely on the skill of the user to guide the paint pad along the surface being painted without applying paint to bordering surfaces that are not being painted. In particular, a paint pad having a width dimension sized to match the width of the window mullion, molding or trim piece may be used to paint these elements without painting bordering elements such as a window pane, ceiling, floor, or other border feature that is not being painted. When the width of the paint pad approximates the width of the feature being painted, two opposing edges of the paint pad may be bordering a surface that is not being painted, and it is important that the two edges of the paint pad paint right up to edges of the surface being painted without applying any paint onto a bordering surface that is not being painted.
Typically, paint is applied onto a paint pad by dipping the paint pad into a paint reservoir, such as a conventional paint tray used to apply paint to a paint roller, a paint can, a pail or other container. However, paint-absorbing pads usually absorb too much paint from the paint reservoir, and this leads to paint drops dripping from the paint pad. One problem is that paint may drip from the paint pad as the user transfers the paint pad from the reservoir to the surface being painted. Another problem is paint getting onto the guide wheels or edge follower and then inadvertently transferring the paint to the surfaces that are not to be painted. Another problem is that excess paint may be forced out of the paint pad during initial painting strokes and the excess paint can drip down the surface being painted or fall onto surfaces that are not being painted. Another problem is that a user may apply too much paint pressure on the paint pad, especially during initial painting strokes, such that excess paint can be forced out of the leading edge of the paint pad and onto the guide surface that is not being painted.
Another problem that occurs when the width of the paint pad approximates the width of the feature being painted is that excess paint on the paint pad can be forced out of the paint pad along edges and onto surfaces that are not being painted. Since paint that falls on surfaces that are not being painted must be cleaned away before the paint dries and since excess paint that falls onto a surface that is being painted must be uniformly spread onto the surface before the paint dries, any paint that drips or is otherwise expelled from a paint pad tends to slow the painting process and leads to undesirable results. In addition, there is a problem when not enough paint is applied to a paint pad since a lack of paint on the paint pad can lead to paint holidays and non-uniform coverage along border edges which are also undesirable results.
To avoid the problem of excess paint on the paint pad, the user removes excess paint from the paint pad after it has been dipped in the paint reservoir. This is typically done by wiping the paint pad over an edge or flat surface of the paint container or by contacting the paint pad with a flat surface and applying a force on the paint pad along a direction that forces excess paint to flow out of the porous paint absorbing pad or by wiping excess paint with a rag. Alternately a combination of wiping the paint pad and forcing the paint pad against a flat surface can be used to remove excess paint. One problem with the prior art method of applying paint to a painting pad and removing excess paint from the paint pad is that paint is often not applied uniformly over the entire area of the pad and this may cause paint to drip out of the paint pad and or lead to non-uniform surface painting.
An alternative device and method for applying paint to a paint pad is disclosed in U.S. Pat. No. 4,164,803, which includes a cylindrically shaped paint transfer roller, rotatably supported in a conventional paint tray with the transfer roller partially submerged in a paint reservoir. To apply paint to a paint pad, the paint pad is moved across the top of the transfer roller thereby causing the transfer roller to rotate with respect to the paint reservoir. Rotation of the roller picks up paint from the reservoir and the paint picked up by the transfer roller is transferred to the entire surface of the paint pad by wicking or absorption. The transfer roller allows a user to apply paint to a paint pad without dipping the paint pad into the reservoir and therefore helps to reduce the amount of excess paint absorbed by the paint pad.
In another example of the prior art, a painting kit, including a paint tray, a paint pad and a cover that fits over an opening of the paint tray to close the paint tray, is disclosed in U.S. Pat. No. 5,553,701. The paint tray is sized to package the paint pad inside for display and storage purposes. The tray includes a trough formed by a front wall, side walls and a downwardly and inwardly inclined rear wall rising from the base of the front wall. The trough provides a paint reservoir. The downwardly and inwardly inclined rear wall provides the painting supply surface for the entire surface of the paint pad. The inclined rear wall is formed with larger dimensions so that the paint pad can be stored inside the tray with the cover on.
Conventional paint pads and devices for applying paint to paint pads can leave the paint pad non-uniformly coated with paint. As a result, paint “holidays” (skipped areas) may occur if not enough paint is applied to the paint pad, or paint can drip or otherwise be inadvertently expelled from the paint pad if too much paint is applied to the paint pad. As a result, paint coverage along cut in edges is non-uniform and the work of painting edges with a paint pad is slowed down to correct the non-uniform coverage and to clean paint from surfaces that are not being painted.
Paint trays with rollers for transferring the paint from a reservoir in the tray to a paint pad assembly are known in the art. The relative size of the roller to the paint pad size affects the performance and ease of using the painting kit. For example, a larger roller is generally desired over a smaller roller as it will allow more paint in the tray reservoir thereby decreasing the need to refill the reservoir frequently. There can be a problem when larger rollers are used with relatively smaller paint pad assemblies such as paint pad assembly ( 40 ). When a larger roller rotates during the transfer of paint process to the smaller paint pad, the larger roller only rotates a small percentage of its circumference, due to the relatively short longitudinal length of the smaller paint pad, thereby advancing only a small amount of paint out from the reservoir and onto the transferring surface of the larger roller. The small rotation of the larger roller will not advance the paint enough to be acquired by the smaller roller. The advanced paint on the larger roller will cause an imbalance to the equilibrium of the larger roller and cause the larger roller to counter rotate and allow the section of the roller still containing paint roll back into the reservoir, leaving a “bare” spot at the top of the roller. The smaller paint pad must be placed again on the larger roller for another attempt at the transfer of paint process, but will be unsuccessful due to the paint roller turning back into the reservoir after each attempt. The generally practiced solution to this problem is to very quickly perform the transfer of paint process, trying to over-spin the larger roller and very quickly repeating the transfer of paint process before the advanced paint can sink back into the reservoir. The problem causes great frustration as the practiced solution is a difficult skill to acquire and can cause splashing of paint.
SUMMARY OF THE INVENTION
The present invention overcomes the problems cited in the prior art by providing a painting kit that includes one or more paint pads, a paint tray that includes a paint reservoir, and one or more transfer surfaces associated with the paint tray for transferring paint from a paint reservoir to the paint pad. In addition, each paint transfer surface is sized to transfer paint only onto selected portions of the paint pad in order to leave some regions of the paint pad, and especially edges of the paint pad, without paint, so as to allow those areas to absorb or wick excess paint to prevent the excess paint from being expelled from edges of the paint pad.
It is an object of the present invention to provide a painting kit that includes a paint pad configured with an edge follower suitable for cutting in edges of a flat surface being painted, a reservoir for holding a paint supply, and a transfer surface associated with the paint tray for transferring paint from the reservoir to a selected portion of the paint pad.
It is a further object of the present invention to provide a paint application system that includes a paint pad sized and/or shaped to paint a non flat surface such as a window mullion, molding or other trim element being painted, a reservoir for holding a paint supply and a transfer surface associated with the paint tray for transferring paint from the reservoir to a selected portion of the paint pad.
It is a further object of the present invention to provide a method for painting with a paint pad that includes the step of applying paint to less than the entire area of the paint pad. Other objectives and advantages of the invention will become apparent from the following description of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
The features of the present invention will best be understood from a detailed description of the invention and preferred embodiments thereof selected for the purposes of illustration and shown in the accompanying drawings in which:
FIG. 1 is a perspective view of a first painting kit shown with a first paint pad in contact with a paint transfer roller according to the present invention.
FIG. 2 is a perspective view of the first painting kit shown with a second paint pad in contact with a paint transfer roller according to the present invention.
FIG. 3 is a top plan view of the first painting kit shown with a first paint pad in contact with a paint transfer roller according to the present invention.
FIG. 4 is a sectional view 4 - 4 taken through the paint transfer roller with the first paint pad in contact therewith according to the present invention.
FIG. 5 is a top plan view of the first painting kit shown with a second paint pad in contact with a paint transfer roller according to the present invention.
FIG. 6 is a sectional view 6 - 6 taken through the paint transfer roller with the second paint pad in contact therewith according to the present invention.
FIG. 7 is a perspective view of a second painting kit shown with a third paint pad in contact with a first pedestal paint transfer surface and a second paint pad in contact with a second pedestal paint transfer surface according to the present invention.
FIG. 8 is a side plan view of the second painting kit according to the present invention.
FIG. 9 is a sectional view 9 - 9 taken through the third paint pad in contact with the first pedestal transfer surface according to the present invention.
FIG. 10 is a top plan view of the second painting kit according to the present invention.
FIG. 11 is a sectional view 11 - 11 taken through a longitudinal axis of the second painting kit according to the present invention.
FIG. 12 is a perspective view of a third painting kit that is shown with the paint roller elevated above the paint tray, for clarity.
FIG. 13 is a detail of a roller support feature with an alternative anti-rotation means.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
This invention is directed to improved methods and devices for application of fluid coatings to surfaces. The exemplary embodiment is the painting of a wall or other conventionally painted surface. However, the applicator devices of the invention are capable of a wider range of use. Such a range covers at least other forms of decorative or protective coatings, such as, but not limited to, varnish, lacquer, whitewash, stain, moisture barriers, sealants, primers, antifriction agents, texturizing agents, controlled release preparations, and other sorts of coverings suitable for application by a paint roller or a functional equivalent thereof. Other surface-coating fluids are included in the term “paint” as used herein wherever such incorporation is functional.
Referring to FIGS. 1-6 , with like reference numbers used to describe like elements, a first painting kit ( 14 ) according to the present invention includes a paint tray ( 15 ) made from a suitable material such as high density polyethylene plastic formed in a process such as vacuum forming or injection molding. The paint tray is formed with a longitudinal length and a shorter transverse width. The paint tray ( 15 ) includes a rolling paint applicator (paint transfer roller). The rolling paint applicator comprises a cylindrical roller ( 30 ) having a rotation axis disposed along the transverse width of the tray ( 15 ) with the cylindrical roller ( 30 ) supported for rotation with respect to opposing sidewalls ( 18 ) of the tray ( 15 ). The cylindrical roller ( 30 ) is partially submerged in a paint reservoir formed by the tray ( 15 ). The outside diameter of the cylindrical roller ( 30 ) provides a paint transfer surface for making contact with a paint pad in order to transfer paint from the reservoir to the paint pad in response to rotation of the cylindrical roller ( 30 ). The cylindrical roller ( 30 ) is made from a suitable plastic material such as polypropylene and is formed by a process such as blow molding or gas assist injection molding. Other cylindrical roller embodiments are usable without deviating from the present invention.
Referring to FIGS. 1-6 , the first painting kit ( 14 ) includes a first paint pad assembly ( 50 ) suitable for application of paint in the process of cutting in edges of a surface to be painted. The first painting kit ( 14 ) may also include a second paint pad assembly ( 40 ) suitable for painting window mullions, moldings or other trim items. Each paint pad assembly ( 40 ) or ( 50 ) includes a paint absorbing pad ( 45 ) or ( 55 ) ( FIG. 6 , FIG. 4 ) suitable for absorbing or wicking paint therein and releasing the paint onto a surface being painted when the paint pad ( 45 ) or ( 55 ) is placed in contact with and moved along an edge of the surface being painted. The paint absorbing pads ( 45 ) and ( 55 ) comprise brush bristles, open cell foam, woven fabric or various other fluid absorbing or wicking materials suitable for painting. Each paint pad assembly ( 40 ) and ( 50 ) further includes a handle ( 41 , 51 ) formed to allow a user to manipulate the paint pad assembly. The handle ( 41 , 51 ) is attached to a base plate ( 42 , 52 ) of generally planar rectangular shape. The base plates and handles are preferably formed from a suitable plastic material such as polyethylene and formed in a process such as injection molding.
In a preferred embodiment, a rigid backing ( 43 , 54 ) is disposed between the paint pad ( 45 , 55 ) and the base plate ( 42 , 52 ) with the rigid backing removably attached to the base plate and with the paint pad ( 45 , 55 ) fixedly attached to the rigid backing ( 43 , 54 ), e.g. by adhesive, heat welding, chemical bonding or other suitable attaching means. The rigid backing ( 43 , 54 ) is preferably made from a suitable sheet plastic material such as polyethylene and formed in a suitable process such as die cutting and heat forming. Alternately, the rigid backing can be formed in a process such as injection molding.
The rigid backing ( 43 , 54 ) is generally shaped and sized to match the size and shape of the paint pad and serves to keep the paint pad flat on the paint surface. Preferably, the rigid backing ( 43 , 54 ) and attached paint pad ( 45 , 55 ) are removable from base plate ( 42 , 52 ) for cleaning or replacement. Accordingly both the rigid backing ( 43 , 54 ) and the base plate ( 42 , 52 ) may include features suitable for attaching the rigid back to the base plate such as friction and or compression clamps, fasteners or other suitable attaching means. In other embodiments, the paint pad assemblies ( 40 ) and or ( 50 ) may be disposable after a single use and configured with the paint pad ( 45 , 55 ) permanently attached directly to the base plate ( 42 , 52 ).
The first paint pad ( 55 ) includes opposing and substantially parallel longitudinal edges ( 56 ) and ( 57 ) and opposing substantially parallel transverse edges. The first paint pad assembly ( 50 ) includes an edge follower, e.g. the wheels ( 53 ), disposed along a leading or guided longitudinal edge ( 56 ) of the paint pad ( 55 ) for guiding the first paint pad assembly ( 50 ) along a guide surface during painting. Other edge followers are usable with out deviating from the present invention.
The second paint pad ( 45 ) includes opposing and substantially parallel longitudinal edges ( 46 ) and ( 47 ) and opposing substantially parallel transverse edges. The second paint pad assembly ( 40 ) includes an edge follower ( 44 ) disposed along a leading or guided edge ( 46 ) of the paint pad ( 45 ) for guiding the second paint pad assembly ( 40 ) along a guide surface being painted. Other edge followers are usable with out deviating from the present invention.
The tray ( 15 ) comprises a bottom floor ( 16 ) which along with a pair of opposing end walls ( 22 ) originating from the bottom floor ( 16 ) and extending substantially vertically upward therefrom to a periphery top flange ( 17 ) and a pair of opposing side walls ( 18 ) originating from the bottom floor ( 16 ) and extending substantially vertically upward to horizontal ledges ( 19 ) form a reservoir for holding paint or another fluid. Each side wall ( 18 ) is formed to provide a longitudinal guide surface ( 20 ). Each guide surface ( 20 ) is used to locate and guide a longitudinal guide edge ( 48 ) and ( 58 ) of a corresponding paint pad ( 40 ) or ( 50 ) as paint is transferred to the paint pad by the cylindrical paint roller ( 30 ). In addition, each side wall ( 18 ) is further formed to provide a substantially horizontal ledge ( 19 ). The horizontal ledge ( 19 ) is used to horizontally orient a corresponding paint pad ( 40 ) or ( 50 ) as paint is transferred to the paint pad by the cylindrical paint roller ( 30 ).
The tray ( 15 ) may include wipers ( 23 ) formed integral with opposing ends walls ( 22 ) for wiping excess paint from the paint pads if needed. In FIGS. 1-6 , the wipers ( 23 ) originate from the bottom floor ( 16 ) and rise above top flange ( 17 ), then descend to valley drains ( 24 ) and terminate into end walls ( 22 ).
The side walls ( 18 ) are formed with roller support features ( 25 ), e.g. a blind slot, positioned approximately midway along the longitudinal length of the tray ( 15 ). The cylindrical transfer roller ( 30 ) includes journals ( 31 ), e.g. fixed cylindrical shaft portions, extending out from each end of the cylindrical paint transfer roller ( 30 ), coaxial with a central axis of the cylinder outside diameter(s), and the journals ( 31 ) define a rotation axis of the roller ( 30 ). The journals ( 31 ) engage with the roller support features ( 25 ), e.g. by dropping into the slot, such that the paint roller ( 30 ) is rotationally supported with respect to the side walls ( 18 ).
The paint transfer roller ( 30 ) further includes two paint transfer surfaces comprising a first cylindrical diameter ( 32 ) and a second cylindrical diameter ( 33 ), which in the preferred embodiment are coaxial and have the same diameter. The first cylindrical diameter ( 32 ) has a first axial length that extends from a first edge ( 35 ) to a second edge ( 36 ). In particular, the first axial length is less than the transverse width of the paint absorbing pad ( 55 ) of the first paint pad assembly ( 50 ) such that less than the entire width of the paint absorbing pad ( 55 ) of the first paint pad assembly ( 50 ) is coated with paint by the first cylindrical diameter ( 32 ). The second cylindrical diameter ( 33 ) has a second axial length that extends from a first edge ( 37 ) to a second edge ( 38 ). In particular, the second axial length is less than the transverse width of the paint absorbing pad ( 45 ) of the second paint pad assembly ( 40 ) such that less than the entire width of the paint absorbing pad ( 45 ) is coated with paint by the second cylindrical diameter ( 33 ).
Referring now to FIGS. 3 and 4 , after paint is poured into tray ( 15 ) to approximately the level of the journals ( 31 ), the first paint pad assembly ( 50 ) is positioned into tray ( 15 ). The first paint pad assembly ( 50 ) is positioned in a paint transfer position which places its paint absorbing pad ( 55 ) in contact with the first cylindrical diameter ( 32 ) and the longitudinal guide edge ( 58 ) in contact with the side guide ( 20 ) that is proximate to the first cylindrical diameter ( 32 ) and the underside of the longitudinal edge ( 57 ) resting on the horizontal ledge ( 19 ) that is proximate to the first cylindrical diameter ( 32 ). The paint pad assembly ( 50 ) is then moved longitudinally with respect to the paint tray while keeping the longitudinal guide edge ( 58 ) in contact with the side guide ( 20 ) and the underside of the paint pad longitudinal edge ( 57 ) in contact with the horizontal ledge ( 19 ).
As the paint pad assembly ( 50 ) is moved in reciprocating motion over the cylindrical roller ( 30 ), the roller ( 30 ) picks up paint from the reservoir and transfers paint to the paint absorbing pad ( 55 ). The horizontal ledge ( 19 ) prevents the paint absorbing pad ( 55 ) from tilting into the paint reservoir and absorbing too much paint. The side guide ( 20 ) locates the longitudinal guide edge ( 58 ) with respect to each of the cylindrical roller diameter edges ( 35 ) and ( 36 ) and the transverse width of the paint absorbing pad ( 55 ) is made larger than the axial length of the first cylindrical diameter ( 32 ) to ensure that neither of the longitudinal edges ( 56 ) and ( 57 ) of the paint absorbing pad ( 55 ) makes contact with the roller diameter ( 32 ) such that paint in not transferred to the paint absorbing pad ( 55 ) along either of the longitudinal edges ( 56 ) and ( 57 ). In a preferred embodiment the transverse width of the paint absorbing pad ( 55 ) is generally centered over the axial length of the cylindrical diameter ( 32 ) and the paint pad transverse width exceeds the axial length of the cylindrical diameter ( 32 ) by 0.125 to 0.5 inches. After the first paint pad ( 50 ) has been supplied with paint, a user may wipe excess paint from the paint pad by moving the pad over one of the wipers ( 23 ). Excess paint falling on the wipers ( 23 ) will flow from valley drains ( 24 ) and wipers ( 23 ) back into bottom ( 16 ).
To use the first paint pad assembly ( 50 ) to cut in and paint a straight border between abutting surfaces that form an inside angle such as at the junction of a wall and a ceiling, the paint pad assembly ( 50 ) is placed on a surface to be painted such as a wall. While keeping wheel followers ( 53 ) abutted against the ceiling or other border edge, the paint pad assembly ( 50 ) is moved in a linear reciprocating motion along the border edge. A compression or painting force applied through the handle to the paint absorbing pad ( 55 ) forces the paint pad against the wall being painted and forces paint to flow out of the paint pad and onto the wall. Since the longitudinal edges ( 56 ) and ( 57 ) were not supplied with paint, paint will flow from the region of the paint absorbing pad ( 55 ) that received paint to the longitudinal edges ( 56 ) and ( 57 ) and then onto the wall surface.
Thus according to one aspect of the present invention, when paint is not transferred to the paint absorbing pad ( 55 ) along its longitudinal edges ( 56 ) and ( 57 ), there is less paint proximate to the longitudinal edges to drip out of the paint pad when a paint pressure is applied to the paint pad. This provides an improved painting method which produces a crisp straight borderline at the junction between the wall being painted and a border such as a ceiling or edges of the wall not being painted. It should be noted that alternately, wheel followers ( 53 ) could abut against the tray side guide ( 20 ) to affect loading of paint, but if paint mistakenly gets on the side guide ( 20 ), wheel followers ( 53 ) will pick up paint and undesirably transfer paint to ceiling or other guide surfaces not to be painted.
Referring now to FIGS. 5 and 6 , after paint is poured into tray ( 15 ) to approximately the level of the journals ( 31 ) of the paint transfer roller ( 30 ), the second paint pad assembly ( 40 ) is positioned into tray ( 15 ). The second paint pad assembly ( 40 ) is positioned in a paint transfer position which places its paint absorbing pad ( 45 ) in contact with the second cylindrical diameter ( 33 ), with the longitudinal guide edge ( 48 ) in contact with the side guide ( 20 ) that is proximate to the second cylindrical diameter ( 33 ) and with the underside of the paint absorbing pad ( 40 ) longitudinal edge ( 47 ) resting on the horizontal ledge ( 19 ) that is proximate to the second cylindrical diameter ( 33 ). The paint pad assembly ( 40 ) is then moved longitudinally with respect to the paint tray while keeping the longitudinal guide edge ( 48 ) in contact with the side guide ( 20 ) and the longitudinal edge ( 47 ) in contact with the horizontal ledge ( 19 ). As the paint pad assembly ( 40 ) is moved in a reciprocating motion over the cylindrical roller ( 30 ), the roller ( 30 ) picks up paint from the reservoir and transfers paint to the paint absorbing pad ( 45 ). The horizontal ledge ( 19 ) prevents the paint absorbing pad ( 45 ) from tilting into the paint reservoir and absorbing too much paint. The side guide ( 20 ) locates the longitudinal guide edge ( 48 ) with respect to each of the cylindrical roller diameter edges ( 37 ) and ( 38 ). The transverse width of the paint absorbing pad ( 45 ) is made larger than the axial length of the second cylindrical diameter ( 33 ) to ensure that neither of the longitudinal edges ( 46 ) and ( 47 ) of the paint absorbing pad ( 45 ) makes contact with the roller diameter ( 33 ) such that paint is not transferred to the paint absorbing pad ( 45 ) along either of the longitudinal edges ( 46 ) and ( 47 ). In a preferred embodiment the transverse width of the paint absorbing pad ( 45 ) is generally centered over the axial length of the second cylindrical diameter ( 33 ) and the transverse width of the paint absorbing pad ( 45 ) exceeds the axial length of the second cylindrical diameter ( 33 ) by 0.125 to 0.5 inches. After the second paint pad ( 40 ) has been supplied with paint, a user may wipe excess paint from the paint absorbing pad ( 45 ) by moving the paint pad assembly ( 40 ) over one of the wipers ( 23 ). Excess paint falling on the wipers ( 23 ) will flow from valley drains ( 24 ) and wipers ( 23 ) back into bottom ( 16 ).
To use the second paint pad assembly ( 40 ) to cut in and paint a window mullion, molding, trim element or other surface to be painted, the paint pad assembly ( 40 ) is placed on the surface to be painted with its protruding longitudinal edge follower ( 44 ) in contact with a guide surface such as a window pane or other surface that is not being painted. While keeping edge follower ( 44 ) abutted against the guide surface, the paint pad assembly ( 40 ) is moved in a linear reciprocating motion along the element being painted. A compression or painting force applied through the handle to the paint absorbing pad ( 45 ) forces the paint absorbing pad against the element being painted and forces paint to flow out of the paint absorbing pad and onto the element being painted. Since the paint absorbing pad ( 45 ) longitudinal edges ( 46 ) and ( 47 ) were not supplied with paint, paint will flow from the region of the paint absorbing pad ( 45 ) that received paint to the longitudinal edges ( 46 ) and ( 47 ) and then onto the element being painted. It should be noted that alternately, edge follower ( 44 ) could abut against the tray side guide ( 20 ) to effect loading of paint, but if paint mistakenly gets on the side guide ( 20 ), edge follower ( 44 ) will pick up paint and undesirably transfer paint to the surface that is not being painted.
Thus according to one aspect of the present invention when paint is not transferred to the paint absorbing pad ( 45 ) along its longitudinal edges ( 46 ) and ( 47 ) there is less paint proximate to the longitudinal edges to drip out of the paint pad ( 40 ) when a paint pressure is applied to the paint absorbing pad ( 45 ). This provides an improved painting method which produces a crisp straight borderline at the junction between the element being painted and a border such as a window pane or other guide surface that is not being painted.
In other embodiments of the present invention, the position of the side guides ( 20 ), the axial length of the roller diameters ( 32 , 33 ) and/or the position of the roller edges ( 35 , 36 , 37 , 38 ) may be configured differently to apply paint onto other selected regions of the paint pads ( 45 , 55 ) e.g. to apply paint over the entire area of the pad except along one or the other longitudinal edge ( 46 , 47 , 56 , 57 ).
Referring now to FIGS. 7-11 with like reference numbers used to describe like elements, a second painting kit ( 69 ) according to the present invention includes a paint tray ( 70 ) made from a suitable material such as high density polyethylene plastic and formed in a process such as vacuum forming or injection molding. The paint tray ( 70 ) is formed with a longitudinal length and a shorter transverse width. The paint tray ( 70 ) includes one or more pedestal surfaces ( 79 ) and ( 82 ) which when coated with paint are usable to transfer the paint coated thereon onto paint pads placed in contact with the pedestal surfaces. The second paint tray ( 69 ) includes a third paint pad assembly ( 60 ), which is similar to the first paint pad assembly ( 50 ) described above, and a second paint pad assembly ( 40 ) which is substantially identical to the second paint pad assembly ( 40 ) described above.
The tray ( 70 ) comprises a bottom surface which has a substantially horizontally disposed front portion ( 71 ), an inclined drain portion ( 74 ) and a rear portion that forms a leg ( 87 ) that supports the paint tray with respect to a floor or other support surface. The tray ( 70 ) further includes a front wall ( 72 ) that extends substantially vertically up from the bottom wall front portion ( 71 ) and terminates on the top at peripheral top lip ( 73 ) and opposing side walls ( 77 ) that extend substantially vertically up from side edges of the bottom wall front portion ( 71 ) that also terminate on the top at peripheral top lip ( 73 ). Both side walls ( 77 ) further includes a guide surface ( 78 ) that is used to locate the paint transfer position of the third paint pad assembly ( 60 ) when the third paint pad assembly is in contact with the first paint pedestal surface ( 79 ). The bottom wall front portion ( 71 ) along with the front wall ( 72 ), the front portions of the side walls ( 77 ), the stepped wall ( 80 ) and some of the inclined drain portion ( 74 ) together form a reservoir for holding paint or other fluids. The tray ( 70 ) further includes include a sloped top lip ( 76 ) formed at the top of guide surface ( 78 ), a skirt ( 90 ) which originates from sloped top lip ( 76 ), and peripheral top lip ( 73 ) extending substantially vertically downwardly and terminating at a generally horizontal flange ( 89 ). Further included is a leg wall ( 88 ), originating from leg ( 87 ), at the bottom and extending substantially vertically upward to terminate at sloped top lip ( 76 ).
The first paint pedestal surface ( 79 ) is suitable for transferring paint to the third paint pad assembly ( 60 ), and a second paint pedestal surface ( 82 ) is suitable for transferring paint to the second paint pad assembly ( 40 ). Each of the paint pedestal surfaces ( 79 , 82 ) is disposed vertically above the level of fluid in the reservoir and vertically above the drain portion ( 74 ). The second pedestal surface ( 82 ) preferably originates at a back end of first pedestal surface ( 79 ) and is preferably disposed at an obtuse angle with respect thereto. The pedestal surfaces ( 79 , 82 ) are connected to the drain portion ( 74 ), on both opposing sides, by substantially vertically disposed trough walls ( 81 ), at the front end by a substantially vertically disposed stepped wall ( 80 ) and at the rear end by a substantially vertically disposed back wall ( 86 ).
Each paint pedestal surface comprises a flat rectangular inclined surface formed with a longitudinal length and a transverse width. The first paint pedestal surface ( 79 ) has a longitudinal length that extends along the longitudinal length of the tray ( 70 ) and is equal to or greater than the longitudinal length of the paint absorbing pad ( 55 ) of the third paint pad assembly ( 60 ). As shown in FIG. 9 , the first paint pedestal surface ( 79 ) has a transverse width extending from a front edge ( 85 ) to the rear edge ( 68 ) and the transverse width of the first paint pedestal surface ( 79 ) is less than the transverse width of the paint absorbing pad ( 55 ) of the third paint pad assembly ( 60 ). The second paint pedestal surface ( 82 ) has a longitudinal length that extends along the transverse axis of the tray ( 70 ) and is equal to or greater than the longitudinal length of the paint absorbing pad ( 45 ) of the second paint pad ( 40 ). As shown in FIG. 11 , the second paint pedestal surface ( 82 ) has a transverse width that extends, along the longitudinal axis of the tray ( 70 ), from a front edge ( 83 ) to a back edge ( 84 ), and the transverse width of the second paint pedestal surface ( 82 ) is less than the transverse width of the paint absorbing pad ( 45 ) of the second paint pad ( 40 ).
It should be noted that although paint pedestal surfaces ( 79 ) and ( 82 ) are depicted as inclines to the horizontal, with slight modification to the design, pedestal surfaces ( 79 ) and ( 82 ) could be repositioned to be parallel to the horizontal and placed vertically higher than the reservoir holding paint or other fluids. Alternatively, paint pedestal surfaces such as ( 79 ) and ( 82 ) could be replenished with paint using an applicator, such as a paint brush or pad, or a roller, or other suitable device.
Referring now to FIGS. 7, 8 and 9 , paint is poured into tray ( 70 ) to a level approximately to the top edge of stepped wall ( 80 ). In its normal resting position on a floor or flat horizontal surface, the front portion ( 71 ) of the bottom wall is substantially horizontal. To coat one or both paint pedestal surfaces the tray ( 70 ) is tilted by lifting the front edge by the peripheral top lip ( 73 ) until paint from the reservoir flows over the stepped wall ( 80 ) and up the inclined drain portion ( 74 ) until it covers the first paint pedestal surface ( 79 ) and if need the second paint pedestal surface ( 82 ). The tray is then lowered to its normal resting position and any excess paint drains back to the reservoir. The third paint pad assembly ( 60 ) is then positioned onto the first paint pedestal surface ( 79 ) to transfer the coating of paint applied thereto to the paint absorbing pad ( 55 ) of the third paint pad assembly ( 60 ). Alternately or additionally, the second paint pad ( 40 ) may be positioned onto the second paint pedestal surface ( 82 ) to transfer the coating of paint applied thereto to the paint absorbing pad ( 45 ) of the second paint pad assembly ( 40 ).
Referring to FIG. 9 , the third paint pad assembly ( 60 ) includes a guide edge ( 59 ) which is disposed to contact the side wall guide surface ( 78 ) when the third paint pad assembly ( 60 ) is mounted onto the first paint pedestal surface ( 79 ). The guide edge ( 59 ) locates the paint absorbing pad ( 55 ) of the third paint pad assembly ( 60 ) along the transverse axis and specifically positions the paint absorbing pad ( 55 ) so that neither of its longitudinal edges ( 85 ) and ( 86 ) is in contact with the first paint pedestal surface ( 79 ) to thereby prevent the longitudinal edges ( 85 ) and ( 86 ) from having paint applied thereto by the first paint pedestal surface ( 79 ).
Referring now to FIGS. 4 and 9 , it should be noted that the third paint pad assembly ( 60 ) could be used with tray ( 15 ) with minor changes to tray ( 15 ). The longitudinal ledge ( 19 ) could be repositioned vertically higher than its position as shown in tray ( 15 ). This would allow the guide edge ( 58 ) of paint pad assembly ( 60 ) to align with the longitudinal ledge ( 19 ) of paint tray ( 15 ). After paint is poured into tray ( 15 ) to approximately the level of the journals ( 31 ), the third paint pad assembly ( 60 ) is positioned into tray ( 15 ) in a paint transfer position. This places paint absorbing pad ( 55 ) in contact with the first cylindrical diameter ( 32 ) as shown in FIG. 4 , with guide edge ( 58 ) in contact with the side guide ( 20 ) that is proximate to the first cylindrical diameter ( 32 ) and with the underside of the guide edge ( 58 ) resting on the horizontal ledge ( 19 ) that is proximate to the first cylindrical diameter ( 32 ).
The paint pad assembly ( 60 ) is then moved longitudinally with respect to the paint tray while keeping the guide edge ( 58 ) in contact with the side guide ( 20 ) and the underside of the guide edge ( 58 ) in contact with the horizontal ledge ( 19 ). As the paint pad ( 60 ) is moved in reciprocating motion over the cylindrical roller ( 30 ), the roller ( 30 ) picks up paint from the reservoir and transfers paint to the paint pad ( 55 ). The horizontal ledge ( 19 ) prevents the paint absorbing pad ( 55 ) from tilting into the paint reservoir and absorbing too much paint.
The side guide ( 20 ) locates the guide edge ( 58 ) with respect to each of the cylindrical roller diameter edges ( 35 ) and ( 36 ). The transverse width of the paint absorbing pad ( 55 ) is made larger than the axial length of the first cylindrical diameter ( 32 ) to ensure that neither of the longitudinal edges ( 56 ) and ( 57 ) of the paint absorbing pad ( 55 ) makes contact with the roller diameter ( 32 ) such that paint in not transferred to the paint absorbing pad ( 55 ) along either of the longitudinal edges ( 56 ) and ( 57 ).
In a preferred embodiment, the transverse width of the paint absorbing pad ( 55 ) is generally centered over the axial length of the cylindrical diameter ( 32 ) and the paint pad transverse width exceeds the axial length of the cylindrical diameter ( 32 ) by 0.125 to 0.5 inches. It should be noted that the transverse width of the paint absorbing pad ( 55 ) could be not centered, but instead be biased to one side to prevent the paint transfer to only one longitudinal edge ( 56 ) or ( 57 ). After the third paint pad ( 60 ) has been supplied with paint, a user may wipe excess paint from the paint pad by moving the pad over one of the wipers ( 23 ). Excess paint falling on the wipers ( 23 ) will flow from valley drains ( 24 ) and wipers ( 23 ) back into bottom ( 16 ).
Referring to FIG. 11 , the second paint pad assembly ( 40 ) includes a aligner guide edge ( 49 ) disposed on the handle ( 41 ) and the aligner guide edge ( 49 ) is disposed to mate with a back guide wall ( 75 ) formed on the tray ( 70 ) when the second paint pad assembly ( 40 ) is mounted onto the second paint pedestal surface ( 82 ). The aligner guide edge ( 49 ) locates the paint absorbing pad ( 45 ) of the second paint pad assembly ( 40 ) and specifically positions the paint absorbing pad so that neither of its longitudinal edges ( 46 ) and ( 47 ) are in contact with the second paint pedestal surface ( 82 ) to thereby prevent the longitudinal edges ( 46 ) and ( 47 ) from having paint applied thereto by the paint pedestal surface ( 82 ).
Each of the paint pads ( 40 ) and ( 60 ) is used to cut in straight borders between abutting surfaces such as to paint window mullions, moldings and trim elements as described above.
The problem of backwards rotation of the transfer roller, resulting in uneven transfer of paint to an applicator, such as a paint pad assembly, have been described above. The present invention overcomes these problems with a novel anti-rotation means to prevent the larger roller from counter-rotating between the transfer of paint process, allowing the advanced paint on the paint transfer roller ( 110 ) to be acquired by the paint pad assembly.
Referring now to FIGS. 12 and 13 , the third painting kit ( 100 ) is similar to the first painting kit ( 14 ) with additional features. The paint transfer roller ( 110 ) is similar to the cylindrical roller ( 30 ) with additional features. The paint transfer roller ( 110 ) also includes, extending from and coaxial with the journals ( 31 ), polygon shaped protruding polygon ends ( 111 ). The polygon ends ( 111 ) consist of three or more surfaces, typically of equal or approximately equal length, joining at equal or approximately equal angles to each other. The corners of the angles preferably fall on a circle concentric with the journals ( 31 ).
The paint holding tray ( 101 ) also includes one or more horizontal anti-rotation means ( 102 ) or one or more angled anti-rotation means ( 103 ). The horizontal anti-rotation means ( 102 ) consists of a generally planar surface attached and spaced above the support feature ( 25 ), allowably positioned either horizontally or at an angle to the horizontal. The angled anti-rotation means ( 103 ) consists of one or more generally planar surfaces attached and spaced above the support feature ( 25 ). Preferred positions range from horizontal to an inclined slope.
Paint transfer roller ( 110 ) is hollow, or solid with a density less than the fluid within the reservoir, with the ability to float on the fluid. (For example, the roller could be filled with a foam.) The journals ( 31 ) supported in roller support features ( 25 ) allow vertical motion of the paint transfer roller ( 110 ). The anti-rotation means ( 102 ) or ( 103 ), spaced above the roller support features ( 25 ), capture and prevent rotation of the polygon ends ( 111 ) of paint transfer roller ( 110 ) when the paint transfer roller ( 110 ) floats up due to the buoyancy of the paint in the reservoir, effecting a blockage of rotation of the paint transfer roller ( 110 ). Applying downward pressure on the paint transfer roller ( 110 ) during the paint transfer process, by using the paint pad assembly ( 40 ), ( 50 ) or ( 60 ) to press on the paint transfer roller ( 110 ) downwardly, releases the polygon ends ( 111 ) from the anti-rotation means ( 102 ) or ( 103 ), allowing rotation of the paint transfer roller ( 110 ). Repeating the paint transfer process will advance the rotation of the paint transfer roller ( 110 ) supplying paint to the paint pad assembly ( 40 ), ( 50 ) or ( 60 ). Thus, well-wetted surfaces of the roller are always available at the upper surfaces of the roller, to efficiently and reliably transfer paint to the paint pad. It should also be noted that alternate anti-rotation means, such as mechanical ratchets, clutches, surface textures, and inverted tapered journal supports, could also be employed to prevent reversed rotation of the transfer roller, without departing from the spirit of the invention.
It will also be recognized by those skilled in the art that, while the invention has been described above in terms of preferred embodiments, it is not limited thereto. Various features and aspects of the above described invention may be used individually or jointly. Further, although the invention has been described in the context of its implementation in a particular environment, and for particular applications, e.g. as a painting kit, those skilled in the art will recognize that its usefulness is not limited thereto and that the present invention can be beneficially utilized in any number of environments and implementations where it is desirable to apply a paint coating up to an edge of a surface. In addition to paint, a variety of other fluids that might be applied with the device of the invention are listed above, as non-limiting examples. Accordingly, the claims set forth below should be construed in view of the full breadth and spirit of the invention as disclosed herein.
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A painting kit includes one or more paint pads and a paint tray. The paint tray includes a reservoir for holding a supply of paint, and means for transferring paint to a paint pad. In one embodiment the paint tray includes a rotating cylinder to transfer paint from the paint reservoir to one or more paint pads. In another embodiment, one or more paint pedestal surfaces are coated with paint from the reservoir in order to transfer paint to paint pads. Each of the paint pads and the trays includes features to selectively apply paint to the paint pad and to avoid applying paint to selected longitudinal edges of the paint pad. The lack of paint along the longitudinal edges helps to prevent paint from dripping or being forced from the longitudinal edge onto adjacent dry surfaces, and thereby enables a user to paint uniformly near edges while avoiding adjacent areas.
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CROSS-REFERENCE TO RELATED APPLICATIONS
The present application claims the benefit under 35 U.S.C. §119 (e) of the Provisional Patent Application Ser. No. 61/327,418, titled Integrated System for Stormwater Management, which was filed on Apr. 23, 2010. The contents of Provisional Patent Application Ser. No. 61/327,418 are hereby incorporated by reference.
FIELD OF THE INVENTION
The invention is directed to modular water retention and detention systems, the application of internal flow control systems for secondary usages and methods of assembly of such systems. The invention is also directed to modular liquid storage with controlled outflow devices and methods of assembly and application of such systems.
BACKGROUND OF THE INVENTION
Stormwater retention and detention systems (for example, also known as storage structures with controlled outflow devices) are systems typically installed underground, that are used for accommodating surface stormwater runoff by diverting and storing water to prevent pooling of water at the ground surface.
Although stormwater (or water) is being referenced generally for descriptive purposes, such liquid identification for this patent can be interchangeable with stormwater, groundwater, drinking water, irrigation water, sewerage and wastewater, or industrial process water and the associated characteristics of such specific liquid being referenced for management purposes.
Liquid retention and detention systems typically consist of a structural support component (in the form of a container or vessel), with an available storage volume and a controlled outlet flow device for metering discharge from the system. These systems are typically installed underground, but can be designed for above ground applications. The industry historically locates these systems at a lower elevation than the collection basin surface (or system) so as to take advantage of the natural potential energy (head) associated with liquid flows to eliminate the need for mechanical devices such as pumps. Stormwater systems are typically located in close vicinity of the collection area, such as under a parking lot, roadway or building to optimize the use of the land area.
Other uses of storage and controlled outflow systems involves having greywater piped into the system directly from a building, groundwater which flows into the system through the ground, and blackwater, which is pumped into the system. Greywater includes wastewater generated from domestic activities such as laundry, dishwashing, and bathing, which can be recycled on-site. Blackwater includes greywater and anything that goes down drains, including toilet water.
Water storage with controlled outflow systems are generally large structures, and thus, may be provided as modular systems that can be assembled in pieces yet meet the same intent as a singular large structure. There is a need to provide modular systems because modular systems are easier to install, allow for greater design flexibility, and have lower installation costs than nonmodular systems. This is because water storage and controlled outflow systems typically require very large storage volumes requiring heavy structural components to contain them.
It is also an advantage for the structure of a modular system to be accessible and large enough for a person to enter the system in the event servicing of a module is required.
For example, such systems are manufactured of concrete with a reinforced steel core, or interconnecting pipes or chambers constructed of metal or plastics supported by a structural stone bedding and backfill material or ponds with an open water surface.
There are various existing designs of water storage and controlled outflow systems that are known in the art. These systems, while being designed to retain and detain water and/or displace water, however, have significant disadvantages that are overcome by the presently described invention.
U.S. Pat. No. 7,621,695 to Smith et al. discloses a subsurface cubic water system having modules with pillars forming a generally cruciform cross section. U.S. Pat. No. 7,344,335 to Burkhart discloses a water retention system having modules with continuous lateral and longitudinal channels, the continuous lateral and longitudinal channels extending from one end of the system to the other allowing for unimpeded flows in any or all directions during operations.
U.S. Pat. Nos. 7,056,058, 6,779,946 and 5,810,510 to Urriola et al. disclose a transport corridor drainage system having vertical channels and no horizontal deck. The '510 patent in particular discloses an underground drainage system having channels for flow.
U.S. Pat. No. 5,249,887 to Phillips discloses an apparatus for control of liquids having modules in series; U.S. Patent Application No. 2009/0226260 to Boulton et al. discloses a method and apparatus for capturing, storing and distributing water; and U.S. Patent Application No. 2009/0279953 to Allard et al. discloses modular units having an arched opening in each of six faces, such that passages for water flow extend through the center of the structure to each opposing face.
All of these designs, however, while being designed for the storage of water and function as large holding vessels for water, do not provide a system that is designed for providing indirect flow of water internally within a system. Furthermore, these systems do not disclose the use of a modular system having beams, walls and/or weirs, the modular system allowing for a serpentine or semi-serpentine flow of water within the modules and system.
Instead, existing systems have primarily functioned as large holding vessels for water, with treatment and flow control devices occurring outside of the system structure. Existing systems do not apply and integrate the principles of treatment or internal flow control methods that affect the velocity, the potential energy (head), time attenuation (retention) flow and/or turbulence control within the system. Flow controls, such as weirs, baffles, walls, orifices, standpipes and particular intended combinations of these devices, have not been provided internally in the existing systems. Furthermore, existing systems have not used these flow controls to cause water to purposely flow indirectly internally within the system for a means of secondary application such as treatment or conditioning.
Indirect flow of water internally within storage with controlled outflow systems has advantages over existing systems. Such a design allows for water to flow through a system for a controlled period of time. Indirect flow of water internally through a storage and controlled outflow system allows for the amount of time that water is present within the system to be optimized based upon the cross-sectional area of the system (i.e., the water stays in the system for the optimal amount of time based on the cross-sectional area of the system). This allows the water to be controlled within the system and also allows for water to accumulate in the system in a controlled and systematically intended manner. This allows for optimal increased storage of water in the system and the application of controlling the flow for other purposes such as treatment, temperature regulation, flow attenuation, and other purposes for water treatment and conditioning.
Indirect flow of water internally within a retention and detention system also allows the water to be controlled within the system to achieve treatment. This allows the water to be treated or conditioned as the water flows internally within the system. A system with a purposely intended controlled indirect flow, prepares the proper environment and conditions conducive to treatment and conditioning applications. Such an intended system design can create the optimum conditions for gravity separation (allowing for both oil water separation and particle separation), neutrally buoyant materials control, trash, debris and solids control, filtering, extended detention for nutrient reduction, temperature reduction, and chemical addition. The result of such a system design may be for the use of conditioning process water or for the removal of various components (either soluble or insoluble) from the flow regime prior to the water being discharged from the system. Furthermore, indirect flow of water internally within a system has other advantages as it allows for compartmentalized flow within the system that allows for various configurations and interchangeability of applications of the system to be provided.
Additionally, indirect flow of water internally within a system may allow for systems where one compartment of the system has a solid floor, while other compartment of the system has a permeable or gravel floor, allowing water to exit the system through the bottom. This may allow for one compartment of the system to be used for water retention, while having other compartments of the system used for water treatment or other applications. In short, a system with internal indirect flow of water is desirable as it solves problems related to uncontrolled flow, such as “short circuiting”, that is common in existing systems. Moreover, internal indirect flow of water solves problems that have not been recognized in the prior art, as it requires the use of beams or other such diversionary structures that diverts the water in an indirect manner. These additional beams and/or material for diverting the water in an indirect manner involves creating systems with additional cost as extra concrete and/or other material used to divert water has to be supplied as material costs.
A system incorporating beams is also more flexible then existing systems as the beams allow for control of the water directing it into a “low flow channel” formed by the restrictive nature or the beam as a barrier and a function of the cross sectional area of the water surface area below the level of the beam. As a result of this concept, for a given period of time greater amounts of water may remain in the system with the beam design, allowing for an increased detention capacity of the system for its available storage volume. The increase in detention time is a direct result of the extended attenuation time (or flow lagging) caused by the indirect serpentine flow pattern allowing for the water to remain in the system for a longer period of time.
As none of these existing systems provide for a design having indirect flow, it is desirable to provide a design that achieves these objectives, and achieves the advantages of such a system. It is further desirable to provide a modular system that hinders the flow of water in a lateral direction, while allowing for longitudinal flow. It is further desirable to provide a modular system that hinders the flow of water in a longitudinal direction, while allowing for lateral flow.
It is also desirable to provide a system that allows for serpentine or semi-serpentine flow of water in the system and allows for control of the flow of water. It is further desirable to provide for a system that allows for internal treatment and conditioning applications of water and also allows for storage and controlled discharge of water. It is also desirable to provide a system that allows for optimal treatment of the water.
Such a water storage with controlled outflow system is novel and unobvious over the prior art. Existing systems have not recognized the problems associated with controlling “short circuiting” by establishing the indirect flow of water through a system where the level of the water is controlled by the height of the beams, walls or weirs. Such existing systems, and persons of skill in the art making such systems, would not have recognized the problem of having indirect flow as all of the existing systems simply are designed principally to store water and work to move the water through the system directly or work to retain water. Existing systems are not designed to control the flow of water in an indirect manner and to maximize treatment of the water.
Having systems with beams may allow for internal indirect flow when the level of the water is below the level (or top of the vertical height) of the beams in the system. In occasions where the level of water is higher than the top of the vertical height of the beams, such as a 2, 10, 25, 50 or even 100 year storm, it is advantageous to have beams as the system may then allow for flow of water that is unimpeded in all directions. This is advantageous over having impervious walls instead of beams, as water would not be able to pass thru the walls. However, a system incorporating impervious walls is also contemplated by the disclosure and utilized specifically when an impeded barrier is required for an application purpose.
A system that has internal indirect flow achieves both storage and controlled outflow capabilities, while allowing for treatment of water, and allowing for water to move through the system in an indirect manner, which optimizes by attenuation (or flow lagging) the amount of time the water is retained in the system. A system that achieves these objects, such as described below, is certainly desirable. Furthermore, a system that controls the velocity, the potential energy (head), time attenuation (flow lagging), flow and turbulence internally within a system is also desirable. A system that has a positive impact on the environment is also desirable.
SUMMARY OF THE INVENTION
Accordingly, it is an object of the present invention to provide a structural system that has indirect flow of water internally within the system. Water as discussed in this application may refer to stormwater, groundwater, drinking water, irrigation water, sewerage and wastewater, or industrial process water. Water may also refer to dirty water and water with various other materials, impurities and/or constituent characteristics such as temperature associated with the water type.
It is another object of the invention to provide a system that hinders the flow of water in a lateral direction, while allowing for the flow of water in a longitudinal direction, when the level of the water is below the level or vertical height of the beams. It is also an object of the invention to provide a system that hinders the flow of water in a longitudinal direction, while allowing for the flow of water in a lateral direction, when the level of the water is below the level or vertical height of the beams. It is an object of the invention to control the flow of water when the water is below the height of the beams.
It is another object of the invention to provide a system that allows for serpentine or semi-serpentine flow of water within the system. It is another object of the invention to provide a system where the water enters the system and progresses in a serpentine or semi-serpentine manner within and around the system. There are advantages to this design as it allows for the intended optimization of the amount of time the water is present within the system (attenuation or retention) as a function of the cross-sectional area and length of the flow channel within the system. Other advantages of this design allow for the water to be controlled and treated as it progresses within the system.
It is another object of the invention to provide a system that allows for flow control of water and for treatment of water. It is another object of the invention to provide for a system that allows for storage and controlled outflow of water. It is another object of the invention to provide a modular system made from various separate modules with different design intentions, but integral to the overall function of the management system. It is recognized that there are fluid dynamic hydraulic similarities between applications that are incorporated in and a reflection of the indirect flow capabilities of the system.
It is another object of the invention to integrate treatment and flow controls into modules which affect and take advantage of the velocity, the potential energy (head), time attenuation (retention), flow and or turbulence control of the fluid within the system.
It is another object of the invention to provide a system that has a positive impact on the environment. It is an object of the invention to provide a smaller environmental footprint than existing systems. It is an object of the invention to have more optimal use of the area of the system via its geometry than existing systems.
These and other objectives are achieved by providing a modular system for controlling a flow of water comprising: a plurality of modules, at least some of the plurality of modules comprising a horizontal deck supported by four vertical members, each of the four vertical members having a bottom edge, the plurality of modules being arranged in a grid having an x-axis and a y-axis, the plurality of modules forming: one or more longitudinal channels, the one or more longitudinal channels being defined in the direction along the y-axis of the modular system, and one or more lateral channels, the one or more lateral channels being defined in the direction along the x-axis of the modular system, wherein at least some of the plurality of modules have at least one beam extending across from one of the vertical members to another one of the vertical members of one of the modules, wherein the at least one beam extends partially upwards from the bottom edge of the one of the four vertical members towards the horizontal deck thereby creating a window.
The system may have the at least one beam direct the flow of the water when the level of the water is below the level or top of the vertical height of the beam. The vertical height of the beam extends from the bottom of the floor up towards the horizontal deck. The beam height is preferred to be approximately 12 inches from the floor or ground, when modules are preferred to be approximately 5 feet, 8 inches. However, the beam height may be adjusted in various embodiments of the invention and may be greater than or less than 12 inches in embodiments of the invention.
The system may control the flow of the water in an indirect path. An indirect path is defined as a path that is not in a straight line. Such a path may be a path that changes direction, such as allowing the water to travel in a longitudinal direction across a module and then being diverted to go in a lateral direction across another module, and vice-versa.
The system may have the plurality of the modules be stackable. Such a stackable design, allows for the system to have various levels. The system may have one, or two, or even more module levels. Such a system with more than one level is referred to a multilevel system. Stackable multilevel systems have modules that are adapted to be stacked. Such modules have structural indentations on the top of the modules that allow for the legs of other modules to be stacked upon them. Such indentations are adapted to receive the legs of other modules. In addition a lower module may or may not have an impervious deck system, an opening to allow for vertical water flow or a flow control device between layers for the intentions of controlling flow as a purposeful design.
The system may also provide for uninterrupted flow across the one or more of the longitudinal channels. The system may provide for uninterrupted flow across the one or more of the lateral channels. Uninterrupted flow is flow through a module that is not interrupted by a beam. A beam is an example of an element that causes the flow of the water to be interrupted. A wall is another example of an element that causes the flow of the water to be interrupted. Other such elements may cause the flow of the water to be interrupted.
The system may have at least some of the plurality of modules be located on the external edge of the system defining a perimeter. The system may have the perimeter of the plurality of modules be perforate. Perforate is defined as allowing for water to travel through the wall of the module via holes. The holes that allow for the wall to be perforate may be of various diameters. Typically, such holes have a diameter of approximately 1-4 inches in diameter, but are sized based on an intended controlled flow rate.
The system may have a porous surface on the bottom of the system, the plurality of modules being located on the porous surface. The porous surface may be made from gravel or other such materials that allow for the water to seep through the surface.
The system may also be located on an impermeable surface. The impermeable surface may be a material such as concrete or another material that water cannot easily travel through.
The system may have certain modules be located on a permeable surface, while other modules are located on an impermeable surface.
The system may further have at least one inlet and at least one outlet for the water to enter or exit the system in a controlled flow rate. Infiltration of the water through pervious base or perimeter materials shall be considered a type of outlet device. As would a mechanic device such as a pump or siphon device be considered a type of outlet device incorporated in the system. The system may have more than one inlet and more than one outlet. Such an inlet or outlet may be an orifice or a standpipe. An orifice is defined as a type of opening or aperture having a pipe or tubing connected to the opening allowing for the water to enter or exit the system at a purposefully designed controlled flow rate.
The system may also comprise corner modules, the corner modules each having two of the four vertical members attached to one another via walls, the walls extending from the bottom of the horizontal deck to the bottom of the vertical members and across the entire length of one edge of the horizontal deck; end modules, the end modules each having a single beam and a single wall, the single beam extending from the one of the four vertical members to another one of the four vertical members wherein the single beam extends partially upwards from the bottom edge of the one of the four vertical members towards the horizontal deck thereby creating a window, and wherein the single wall extends from the bottom of the horizontal deck to the bottom of the vertical members and across the entire length of one edge of the horizontal deck; and internal modules, the internal modules each having two beams, each of the two beams extending from the one of the four vertical members to another one of the four vertical members, wherein the two beams extend partially upwards from the bottom edge of the one of the four vertical members towards the horizontal deck thereby creating two windows. The system may have each of its beams integrated together with their corresponding vertical members. Such an integrated structure may have the beams and corresponding vertical members be fused together as one piece. In certain embodiments, the beams and corresponding vertical members may be manufactured together as one piece during the construction of the modules. In other embodiments, the beams and corresponding vertical members may be manufactured as separate pieces which are integrated together using various industry techniques.
The system may have each of the beams direct the flow of the water when the level of the water is below the level or vertical height of each of the beams (i.e., when the water is below the maximum height of the beams). When the level of the water is greater than the beam height, then the water may travel over the beams. This typically will happen per purposeful design intent, such as in a 2, 10, 25, 50 or 100 year storm.
The system may have its walls perforated with holes. These holes may allow the water to flow through the holes. Such walls with holes that allow for the water to travel through them are defined as being perforate.
The system may have modules, which contain an inlet or an outlet, also be nonperforate. Nonperforate is defined as not letting water through. A solid wall is an example of a nonperforate wall. Nonperforate walls may exist having an opening, inlet or outlet (such as an orifice), which will allow water to enter or exit the system through the opening, inlet or outlet.
The system may have at least some of the modules have at least one such opening or orifice. The system may have modules that are nonperforate also have a weir to allow the flow of water out of the modules. The modules with nonperforate walls may be located on an impermeable surface. The system may have modules have weirs, baffles, beams, orifice holes, and particular combinations of these elements that are used to control the flow of water internally within the system. A completely enclosed module consisting of a watertight storage space (with #4 non-perforated walls and an impervious floor) may be used as an isolation chamber capable of watertight containment integrated into the system.
Other objectives of the invention are achieved by providing a module for controlling a flow of water comprising: a horizontal deck; four vertical members each having a bottom edge, the four vertical members supporting the horizontal deck and being arranged in the four corners below the horizontal deck; a first beam extending across from the one of the four vertical members to another one of the four vertical members, wherein the first beam extends partially upwards from the bottom edge of the one of the four vertical members towards the horizontal deck. The first beam is typically provided as having its upper surface be parallel to the horizontal deck. In other embodiments, the first beam may have its upper surface be approximately parallel to the horizontal deck and/or may have its upper surface be angled with respect to the horizontal deck.
The module may have the first beam form a window between the top of the beam and the bottom of the horizontal deck. Such a window may have various shapes. However, the window does not involve having the module have more concrete above the beam than the beam itself. The window is different than a weir, as the window is formed based upon the beam, not based upon cutting a hole in a solid wall. A hole is a solid wall is defined as being an opening. A window, is not simply an opening, but rather is the open area from the top of the beam to approximately the bottom of the horizontal deck. The window does not extend all the way up to the bottom of the horizontal deck. There is a structural section a few inches wide between the deck and the top of the window opening.
The module may have the first beam direct the flow of the water when the water is below the top of the vertical height of the first beam. The first beam may allow the water to flow indirectly through the module and/or system.
The module may have one of the vertical members be attached to another one of the vertical members via a first wall, the first wall extending from the bottom of the horizontal deck to the bottom of the vertical member and across the entire length of one edge of the horizontal deck. The module may have the wall have perforated holes.
The module may have a second beam extending across from the one of the four vertical members to another one of the four vertical members. The second beam may extend partially upwards from the bottom edge of the one of the four vertical members towards the horizontal deck.
The second beam may form a window between the top of the second beam and the bottom of the horizontal deck. The second beam may direct the flow of the water when the level of the water is below the top of the vertical height of the second beam (i.e., below the beam height).
The module may have the first beam be integrated together with two of the four vertical members it extends across. The module may have the second beam be integrated together with two of the four vertical members it extends across. The beam may be manufactured with the vertical members as one piece or may be separate pieces that are connected together using conventional techniques known in the industry. The module may be stackable. Such modules have indentations on the top of the modules that allow for the legs of other modules to be stacked upon them. The module may form at least one channel through the module. The module may have a structural component with a storage capacity. The module may made of a steel core within the module and be reinforced by concrete.
Other objectives of the invention are achieved by providing a method for controlling a flow of water in a modular system comprising: providing a plurality of modules, each of the plurality of modules comprising: a horizontal deck supported by four vertical members, the plurality of modules being arranged in a grid having an x-axis and a y-axis, the plurality of modules forming one or more longitudinal channels, the one or more longitudinal channels being defined in the direction along the y-axis of the modular system, one or more lateral channels, the one or more lateral channels being defined in the direction along the x-axis of the modular system; and wherein the at least some of the plurality of modules have at least one beam extending from the one of the four vertical members to another one of the four vertical members, wherein the at least one beam extends partially upwards from the bottom edge of the one of the four vertical members towards the horizontal deck thereby creating a window; inserting the water into the plurality of modules by natural or artificial means, wherein the water is directed through the system by the at least one beam in the plurality of modules, wherein the at least one beam directs the flow of the water when the water is below the level or vertical height of the beam.
The water in the method may be routed through the modular water system in a serpentine or semi-serpentine manner. A serpentine or semi-serpentine manner involves the water flowing in a snakelike fashion where the water may travel through various modules in one direction and then turn and travel in a different direction which may be different and/or opposite to the original direction. Travelling in a serpentine or semi-serpentine manner involves having the water change directions at least once as it travels through the system.
In other embodiments, the water may travel in a single or double row system (such that the beam hinders movement of the water laterally while allowing it to move longitudinally). In these embodiments, the water may not move in a serpentine or semi-serpentine manner.
Other objectives of the invention are achieved by providing a modular system for controlling a flow of water comprising: a plurality of modules, at least some of the plurality of modules comprising a horizontal deck supported by four vertical members, the plurality of modules being arranged in a grid having an x-axis and a y-axis, the plurality of modules forming: one or more longitudinal channels, the one or more longitudinal channels being defined in the direction along the y-axis of the modular system, and one or more lateral channels, the one or more lateral channels being defined in the direction along the x-axis of the modular system, wherein the modular system provides for serpentine flow through the longitudinal and lateral channels.
The modular system may provide for serpentine flow because of a plurality of horizontal beams that direct the flow of the water when the level of the water is below the top of the vertical height of each of the plurality of horizontal beams. When the water flows into the beams, the water is diverted into a different direction.
The modular system may have various internal flow controls, such as weirs, baffles, walls, beams, orifice holes, and particular combinations of these devices. Such internal flow controls are used to control the internal flow of the system so it has indirect flow.
Other objects of the invention and its particular features and advantages will become more apparent from consideration of the following drawings and accompanying detailed description. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a grid view of an embodiment of the system;
FIG. 2 is a perspective view of a module of the system of FIG. 1 ;
FIG. 2A is a top view of the module of FIG. 2 ;
FIG. 2B is a cross section view of FIG. 2 taken along axis A-A;
FIG. 2C is a cross section view of FIG. 2 taken along axis B-B;
FIG. 3 is a perspective view of a module of the system of FIG. 1 ;
FIG. 3A is a top view of the module of FIG. 3 ;
FIG. 3B is a cross section view of FIG. 3 taken along axis A-A;
FIG. 3C is a cross section view of FIG. 3 taken along axis B-B;
FIG. 4 is a perspective view of a module of the system of FIG. 1 ;
FIG. 4A is a top view of the module of FIG. 4 ;
FIG. 4B is a cross section view of FIG. 4 taken along axis A-A;
FIG. 4C is a cross section view of FIG. 4 taken along axis B-B;
FIG. 5 is a perspective view of a module of the system of FIG. 1 ;
FIG. 5A is a top view of the module of FIG. 5 ;
FIG. 5B is a cross section view of FIG. 5 taken along axis A-A;
FIG. 5C is a cross section view of FIG. 5 taken along axis B-B;
FIG. 6 is a perspective view of a module of the system of FIG. 1 ;
FIG. 6A is a top view of the module of FIG. 6 ;
FIG. 6B is a cross section view of FIG. 6 taken along axis A-A;
FIG. 6C is a cross section view of FIG. 6 taken along axis B-B;
FIG. 7 is a perspective view of a module of the system of FIG. 1 ;
FIG. 7A is a top view of the module of FIG. 7 ;
FIG. 7B is a cross section view of FIG. 7 taken along axis A-A;
FIG. 7C is a cross section view of FIG. 7 taken along axis B-B;
FIG. 8 is a perspective view of a module of the system of FIG. 1 ;
FIG. 8A is a top view of the module of FIG. 8 ;
FIG. 8B is a cross section view of FIG. 8 taken along axis A-A;
FIG. 8C is a cross section view of FIG. 8 taken along axis B-B;
FIG. 9 is a perspective view of another embodiment of the system;
FIG. 9A is a side view of the system shown in FIG. 9 ;
FIG. 10 is a grid view of the top portion of the system shown in FIG. 9 ;
FIG. 10A is a grid view of the bottom portion of the system shown in FIG. 9 ;
FIG. 11 is a perspective view of a module of the system of FIG. 1 ;
FIG. 11A is a top view of the module of FIG. 11 ;
FIG. 11B is a cross section view of FIG. 11 along axis A-A;
FIG. 11C is a cross section view of FIG. 11 along axis B-B;
FIG. 12 is a perspective view of a module of the system of FIG. 1 ;
FIG. 12A is a top view of the module of FIG. 12 ;
FIG. 12B is a cross section view of FIG. 12 along axis A-A;
FIG. 12C is a cross section view of FIG. 12 along axis B-B;
FIG. 13 is a perspective view of a module of the system of FIG.
FIG. 13A is a top view of the module of FIG. 13 ;
FIG. 13B is a cross section view of FIG. 13 along axis A-A;
FIG. 13C is a cross section view of FIG. 13 along axis B-B;
FIG. 14 is a perspective view of a module of the system of FIG.
FIG. 14A is a top view of the module of FIG. 14 ;
FIG. 14B is a cross section view of FIG. 14 along axis A-A;
FIG. 14C is a cross section view of FIG. 14 along axis B-B;
FIG. 15 is a perspective view of a module of the system of FIG.
FIG. 15A is a top view of the module of FIG. 15 ;
FIG. 15B is a cross section view of FIG. 15 along axis A-A;
FIG. 15C is a cross section view of FIG. 15 along axis B-B;
FIG. 16 is a grid view of another embodiment of the system; and
FIG. 17 is a perspective view of a module of the system of the invention;
FIG. 18 . is a perspective view of a module of the system of the invention;
FIG. 19 is a perspective view of a module of the system of the invention;
FIG. 20 is a perspective view of a module of the system of the invention;
FIG. 21 is a perspective view of a module of the system of the invention; and
FIG. 22 is a perspective view of a module of the system of the invention;
FIG. 23 is a perspective view of a module of the system of the invention;
FIG. 24 is a perspective view of a module of the system of the invention;
FIG. 25 is a perspective view of a module of the system of the invention;
FIG. 26 is a perspective view of a module of the system of the invention;
FIG. 27 is a perspective view of a module of the system of the invention; and
FIG. 28 is a perspective view of a module of the system of the invention.
DETAILED DESCRIPTION OF THE INVENTION
Referring to FIG. 1 , storage and control outflow system 1000 is shown. System 1000 is made of various modules and is an example of an embodiment of the system disclosed by the present invention. System 1000 is shown having three inlets 110 and one outlet 120 . However, there may be more inlets or less inlets 110 and outlets 120 for system 1000 than shown in FIG. 1 . System 1000 has a legend on the left of the system showing what FIG. 1 and FIGS. 10 and 10A mean by a perforated wall, 12″ beam wall, window, solid wall and weir. System 1000 also has an x-axis as shown (lateral direction) and y-axis (longitudinal direction), which shows the flow of the water through the system in lateral and longitudinal channels, respectively.
System 1000 also has arrows through the system that show the direction of the flow of water within the system. This is an example of a serpentine flow of the water as the arrows show that the water travels in a snakelike manner through the system, where the flow of water changes direction at least once. System 1000 also reduces the turbulence the water as the water changes direction.
System 1000 achieves the advantages of the present invention. Such advantages involve achieving indirect flow of the water internally within system 1000 , which is advantageous over existing systems. System 1000 allows for the water to flow through system 1000 for a controlled period of time. System 1000 may allow water to be treated by a treatment system and method as the water flows within system 1000 . Such a treatment system may filter the water, removing various components of the water from the system prior to the water exiting the system. Such a treatment system may be present in various modules of system 1000 .
System 1000 also allows for the optimization of the amount of time that the water is present within system 1000 based upon the cross-sectional area of the system. This allows for the water to accumulate in system 1000 in a controlled and systematic manner. This allows for increased storage of the water in system 1000 . Moreover, greater amounts of the water may be in system 1000 at a given time, as it has 12 inch beams, allowing for increased storage and retention capacity of the system per its cross-sectional area. If the beam height is increased, the system is able to retain more water per cross-sectional area at a given time.
Dimensions of system 1000 are shown as having 12 inch beams (12 inches being the beam height); however, beams with other heights may be used in the system, such as having beams that have a height of greater than 12 inches. System 1000 is made of various modules. Modules typically are approximately 8 feet wide and 8 feet deep and have a height of 5 feet 8 inches when employing 12 inch beams. The beam height to height of the module ratio thus is typically 1:8.5. However, the ratio of height of the module to beam height may vary depending upon the system and can range from 1:3-1:20. Modules can also have a height that ranges from 3 feet to a height of 12 feet. Modules less than 3 feet are difficult to work with as it is difficult for a man to enter a smaller module to service it.
Furthermore, modules typically have the ability to support 10,000 to 14,000 pounds of weight. However, modules may support additional weight based on materials used, such as having a steel frame internal to the concrete outer shell. Modules may be made of other materials known in the art, and may be made of materials that are more expensive and have greater load bearing capabilities, if desired.
System 1000 has modules having two perforated walls, such as module 300 ; modules having one perforated wall and one beam, such as module 400 and module 800 ; and modules having two beams, such as module 200 .
System 1000 also has modules that have two or more solid walls, such as module 600 , module 700 and module 1100 (with 3 solid walls); and modules that have two solid walls and a weir, such as module 500 . System 1000 may be located on a solid surface, which is impermeable. System 1000 may be located on a permeable surface, such as crushed granite. The system may have certain modules located on a permeable surface and may have other modules located on a solid impermeable surface such as concrete. Preferably, modules 500 , 600 , 700 and 1100 are located on an impermeable surface. These modules typically have a floor which is impermeable. Preferably, modules 200 , 300 , 400 , 800 , and 1200 are located on a permeable surface. However, various modules can be arranged on various surfaces and or materials.
FIG. 2 shows one type of module in system 1000 . Module 200 is shown having four legs 220 , 225 , 230 and 235 . Four legs 220 , 225 , 230 and 235 support horizontal deck 210 . Each of the four legs 220 , 225 , 230 and 235 has a bottom edge.
Legs 220 and 225 are connected together via beam 240 . Legs 230 and 235 are connected together via beam 250 . Beams 240 and 250 are preferably about 12 inches in height from the bottom edge to the top of the beam. The height of the module 200 is preferably 5 feet 8 inches.
Beams 240 and 250 , however, may vary in height to be more or less than 12 inches in height from the bottom edge to the top of the beam. Beams 240 and 250 are used to control the flow of the water so that it moves in an indirect manner within the system. Beams 240 and 250 are also used, to allow the water to flow around the system in a serpentine or semi-serpentine manner.
FIG. 2 also shows window 245 formed in the space between beam 240 and horizontal deck 210 and window 255 formed in the space between beam 250 and horizontal deck 210 . Module 200 also has a channel which extends through the module from 265 to 275 . Channel 265 / 275 allows for the water to flow uninterrupted within module 200 . The height of the channel 265 / 275 is preferably 4 feet 6 inches when using a module with a height of 5 feet 8 inches; however this may vary in various embodiments. The ratio of the height of the channel to the height of the module ranges from 1:2 to 4:5. Such dimensions are applicable to all modules described in the system.
Moreover, channel height may vary within various modules as the height of the floor may vary. However, typically the channel has a standard cross-sectional area through the channel. Such a cross-sectional area is approximately the same within various modules in a system.
FIGS. 2A , 2 B and 2 C show various views of module 200 . FIG. 2A provides a top view where axes A-A and B-B are shown. FIG. 2B is a view across axis A-A where channel 275 / 265 is shown. Legs 225 and 230 are also shown in this view as well as beam 240 and beam 250 and window 245 and window 255 . FIG. 2C is a view across axis B-B where beam 240 and window 245 are shown as well as legs 220 and 225 .
FIG. 3 shows another type of module in system 1000 . Module 300 is shown having four legs 320 , 325 , 330 and 335 . Four legs 320 , 325 , 330 and 335 support horizontal deck 310 . Each of the four legs 320 , 325 , 330 and 335 has a bottom edge.
Legs 325 and 330 are connected together via wall 370 . Legs 330 and 335 are connected together via wall 350 . Wall 370 and wall 350 are shown as having perforations 380 . Perforations 380 allow for the water to exit the system. Perforations may be holes that have a minimum diameter of one inch. The holes may be larger than one inch; however, holes and perforations are smaller than the openings defined in this invention.
FIG. 3 also shows channels 345 and 365 formed in the space between the bottom edges of the four legs to the underside of horizontal deck 310 . Channels 345 and 365 allow for the water or fluid to flow through module 300 . As shown the entrance way of channel 345 , there is a height of the channel from the bottom of the floor to the underside of the deck. However, the underside of the deck may have a greater height to the floor in the middle of the module than the height of bottom of the floor to the underside of the deck in the channel opening.
FIGS. 3A , 3 B and 3 C show various views of module 300 . FIG. 3A provides a top view where axes A-A and B-B are shown. FIG. 3B is a view across axis A-A where wall 370 is shown. Legs 325 and 330 are also shown in this view as well as channel 345 and wall 350 . FIG. 3C is a view across axis B-B where channel 345 is shown.
FIG. 4 shows another type of module in system 1000 . Module 400 is shown having four legs 420 , 425 , 430 and 435 . The four legs 420 , 425 , 430 and 435 each support horizontal deck 410 . Each of the four legs 420 , 425 , 430 and 435 has a bottom edge.
Legs 420 and 435 are connected together via beam 460 . Legs 425 and 430 (hidden from FIG. 4 ) are connected together via wall 470 . Beam 460 is preferably about 12 inches in height or greater from the bottom edge to the top of the beam. Beam 460 is used to control the flow of the water so that it moves in an indirect manner within the system. Beam 460 is also used to allow the water to flow around the system in a serpentine manner. Wall 470 has perforations 480 . Perforations 480 may allow for the water to exit the system. Perforations 480 typically have a diameter of a few inches.
FIG. 4 also shows window 465 formed in the space between beam 460 and horizontal deck 410 . Module 400 also has a channel 445 which extends through the module from 445 to 455 . The channel 445 / 455 allows for the water to flow uninterrupted through module 400 .
FIGS. 4A , 4 B and 4 C show various views of module 400 . FIG. 4A provides a top view where axes A-A and B-B are shown. FIG. 4B is a view across axis A-A where wall 470 is shown. Legs 425 and 430 are also shown in this view. FIG. 4C is a view across axis B-B where channel 445 / 455 is shown.
FIG. 5 shows another type of module in system 1000 . Module 500 is shown having four legs 520 , 525 , 530 and 535 . The four legs 520 , 525 , 530 and 535 each support horizontal deck 510 . Each of the four legs 520 , 525 , 530 and 535 has a bottom edge. Each of the four legs 520 , 525 , 530 and 535 is supported by floor 590 . Floor 590 is shown as being a solid impermeable floor.
Legs 520 and 525 are connected together via wall 540 . Legs 530 and 535 are connected together via wall 550 . Legs 520 and 535 are connected together via wall 560 . Walls 540 , 550 and 560 are shown as solid walls.
FIG. 5 also shows channel 575 formed in the space between floor 590 and the underside of horizontal deck 510 . Channel 575 allows for the water to flow through the module. FIG. 5 also has either weir 580 or opening 585 . Opening 585 allow an inlet or outlet to be connected to the module (such as inlet 110 or outlet 120 shown in FIG. 1 ). If a weir 585 is provided, an inlet or outlet is typically not attached.
FIGS. 5A , 5 B and 5 C show various views of module 500 . FIG. 5A provides a top view where axes A-A and B-B are shown. FIG. 5B is a view across axis A-A where channel 575 is shown. Legs 525 and 530 are also shown in this view. FIG. 5C is a view across axis B-B where wall 540 is shown.
FIG. 6 shows another type of module in system 1000 . Module 600 is shown having four legs 620 , 625 , 630 and 635 . The four legs 620 , 625 , 630 and 635 each support horizontal deck 610 . Each of the four legs 620 , 625 , 630 and 635 has a bottom edge. These legs are supported on a floor 690 . Preferably, floor 690 is impermeable.
Legs 620 and 625 are connected together via wall 640 . Legs 630 and 635 are connected together via wall 650 . Walls 640 and 650 are shown as solid walls. Wall 640 may have an opening 685 attached to the wall. This opening 685 may allow an inlet or outlet to be connected to the module (such as inlet 110 shown in FIG. 1 ). Such an opening 685 is optional to module 600 .
FIG. 6 also shows channel 665 formed in the space between the floor 690 and the underside of horizontal deck 610 . FIG. 6 also shows channel 675 formed in the space between floor 690 and the underside of horizontal deck 610 . The channel height may vary in the module shown in FIG. 6 . Channel 675 allows for the water to flow through the module and is connected to channel 665 forming channel 665 / 675 .
FIGS. 6A , 6 B and 6 C show various views of module 600 . FIG. 6A provides a top view where axes A-A and B-B are shown. FIG. 6B is a view across axis A-A where channel 665 / 675 is shown. Legs 625 and 630 are also shown in this view. FIG. 6C is a view across axis B-B where wall 640 is shown.
FIG. 7 shows another type of module in system 1000 . Module 700 is shown having four legs 720 , 725 , 730 and 735 . The four legs 720 , 725 , 730 and 735 each support horizontal deck 710 . Each of the four legs 720 , 725 , 730 and 735 has a bottom edge. These legs are supported on a floor 790 . Preferably, floor 790 is impermeable.
Legs 725 and 730 are connected together via wall 770 . Legs 730 and 735 are connected together via wall 750 . Walls 770 and 750 are shown as solid walls. Wall 750 may have an opening 785 . This opening 785 may allow an inlet or outlet to be connected to the module (such as inlet 110 shown in FIG. 1 ). Such an opening 785 is optional to module 700 ,
FIG. 7 also shows channel 765 formed in the space between floor 790 and the underside of horizontal deck 710 . Channel 765 allows for the water to flow through module 700 . FIG. 7 also shows channel 745 formed in the space between floor 790 and the underside of horizontal deck 710 . Channel 745 allows for the water to flow through module 700 and is connected to channel 765 . Channels 745 and 765 may have various heights as the channel height in the center of module 700 is greater than the channel height as the edge of module 700 .
FIGS. 7A , 7 B and 7 C show various views of module 700 . FIG. 7A provides a top view where axes A-A and B-B are shown. FIG. 7B is a view across axis A-A where wall 770 is shown. Legs 725 and 730 are also shown in this view. FIG. 7C is a view across axis B-B where channel 745 is shown.
FIG. 8 shows another type of module in system 1000 . Module 800 is shown having four legs 820 , 825 , 830 and 835 . The four legs 820 , 825 , 830 and 835 each support horizontal deck 810 . Each of the four legs 820 , 825 , 830 and 835 has a bottom edge.
Legs 820 and 825 are connected together via beam 840 . Legs 820 and 835 are connected together via wall 860 . Wall 860 is shown as a wall with perforations 880 . Window 845 is also shown between the underside of horizontal deck 810 and the top of beam 840 .
FIG. 8 also shows channel 875 formed in the space between bottom edges of the leg 825 and 830 to the underside of horizontal deck 810 . Channel 875 allows for the water to flow through module 800 . FIG. 8 also shows channel 855 formed in the space between bottom edges of the leg 830 and 835 to the underside of horizontal deck 810 . Channel 855 allows for the water to flow through the module and is connected to channel 875 .
FIGS. 8A , 8 B and 8 C show various views of module 800 . FIG. 8A provides a top view where axes A-A and B-B are shown. FIG. 8B is a view across axis A-A where channel 875 is shown. Legs 825 and 830 are also shown in this view. FIG. 8C is a view across axis B-B where beam 840 and window 845 are shown.
FIG. 11 shows another type of module in system 1000 . Module 1100 is shown having four legs 1120 , 1125 , 1130 and 1135 . Each of the four legs 1120 , 1125 , 1130 and 1135 support horizontal deck 1110 . Each of the four legs 1120 , 1125 , 1130 and 1135 has a bottom edge. Furthermore, module 1100 has floor 1190 .
Legs 1120 and 1125 are connected together via wall 1140 . Legs 1125 and 1130 are connected together via wall 1170 . Legs 1120 and 1135 are connected together via wall 1160 . Walls 1140 , 1160 and 1170 are shown as solid walls. Wall 1160 has an opening 1180 , which allows for an inlet or outlet to be connected to module 1100 . FIG. 11 also shows channel 1155 formed in the space between floor 1190 and the underside of horizontal deck 1110 . Channel 1155 allows for the water to flow through the module. The water may flow through and enter/exit the module via opening 1185 or channel 1155 .
FIGS. 11A , 11 B and 11 C show various views of module 1100 . FIG. 11A provides a top view where axes A-A and B-B are shown. FIG. 11B is a view across axis A-A where wall 1170 is shown. Legs 1125 and 1130 are also shown in this view. FIG. 11C is a view across axis B-B where wall 1140 is shown.
FIG. 12 shows a type of module in system 1000 . Module 1200 is shown having four legs 1220 , 1225 , 1230 and 1235 . The four legs 1220 , 1225 , 1230 and 1235 support horizontal deck 1210 . Each of the four legs 1220 , 1225 , 1230 and 1235 has a bottom edge.
Legs 1220 and 1225 are connected together via wall 1240 . Legs 1220 and 1235 are connected together via wall 1260 . Walls 1240 and 1260 are shown having perforations 1280 . Legs 1225 and 1230 are connected together via wall 1270 . Wall 1270 is shown as being a solid wall. In certain embodiments solid wall 1270 may be replaced by a beam and a window. Wall 1260 also may have opening 1295 allowing for an inlet or outlet to be connected to module 1200 . Such an opening 1295 is optional to module 1200 .
FIG. 12 also shows channel 1255 formed in the space between bottom edges of the leg 1230 and 1235 to the underside of horizontal deck 1210 . Channel 1255 allows for the water to flow through the module.
FIGS. 12A , 12 B and 12 C show various views of module 1200 . FIG. 12A provides a top view where axes A-A and B-B are shown. FIG. 12B is a view across axis A-A where wall 1270 is shown. Legs 1225 and 1230 are also shown in this view. FIG. 12C is a view across axis B-B where wall 1240 is shown.
FIGS. 9 and 9A each show another embodiment of the invention, system 900 . System 900 is made of various modules, and may have some of the modules previously described. System 900 is shown having an inlet 910 and having two stacks of modules, upper stack 950 and lower stack 960 . Various modules previously described (modules 200 , 300 , 400 , 500 , 600 and 800 ) may be used in system 900 . Furthermore, additional modules may also be used in system 900 .
FIGS. 10 and 10A show a schematic or grid view of system 900 . FIG. 10 is a view of upper stack 950 . FIG. 10A is a view of lower stack 960 . Various modules previously described may be used for upper stack 950 and lower stack 960 . Upper stack 950 and lower stack 960 work together as a coordinated multilayer system. Inlet/outlet 595 is shown in FIG. 10 . Other inlets and/or outlets may be incorporated into system 900 .
FIG. 13 shows a type of module in system 900 . Module 1300 is shown having four legs 1320 , 1325 , 1330 and 1335 . The four legs 1320 , 1325 , 1330 and 1335 support horizontal deck 1310 . Each of the four legs 1320 , 1325 , 1330 and 1335 has a bottom edge.
Legs 1325 and 1330 are connected together via wall 1370 . Wall 1370 is shown as a solid wall. Legs 1330 and 1335 are connected together via wall 1350 . Wall 1350 is shown having perforations 1380 .
FIG. 13 also shows channel 1345 formed in the space between bottom edges of the leg 1320 and 1325 to the underside of horizontal deck 1310 . Channel 1345 allows for the water to flow through the module. FIG. 13 also shows channel 1365 formed in the space between bottom edges of the leg 1320 and 1335 to the underside of horizontal deck 1310 . Channel 1365 allows for the water to flow through the module and is connected to channel 1345 .
FIGS. 13A , 13 B and 13 C show various views of module 1300 . FIG. 13A provides a top view where axes A-A and B-B are shown. FIG. 13B is a view across axis A-A where wall 1370 is shown. Legs 1325 and 1330 are also shown in this view. FIG. 13C is a view across axis B-B where channel 1345 is shown.
FIG. 14 shows another type of module in system 900 . Module 1400 is shown having four legs 1420 , 1425 , 1430 and 1435 . The four legs 1420 , 1425 , 1430 and 1435 support horizontal deck 1410 . Each of the four legs 1420 , 1425 , 1430 and 1435 has a bottom edge.
Legs 1425 and 1430 are connected together via beam 1470 . Window 1475 is shown between the underside of horizontal deck 1410 and the top of beam 1470 .
FIG. 14 also shows channel 1445 formed in the space between the underside of horizontal deck 1410 and the floor and between leg 1420 and leg 1425 . Channel 1445 allows for the water to flow through the module. FIG. 14 also shows channel 1455 formed in the space between the underside of horizontal deck 1410 and the floor and between leg 1430 and leg 1435 . Channel 1455 allows for the water to flow through the module and is connected to channel 1445 . FIG. 14 also shown channel 1465 formed in the space between the underside of horizontal deck 1410 and the floor and between leg 1420 and leg 1435 . Channel 1465 allows for the water to flow through the module and is connected to channel 1445 and channel 1455 .
FIGS. 14A , 14 B and 14 C show various views of module 1400 . FIG. 14A provides a top view where axes A-A and B-B are shown. FIG. 14B is a view across axis A-A where beam 1470 and window 1475 are shown. Legs 1425 and 1430 are also shown in this view. FIG. 14C is a view across axis B-B where channel 1445 / 1465 is shown.
FIG. 15 shows another type of module in system 900 . Module 1500 is shown having four legs 1520 , 1525 , 1530 and 1535 . The four legs 1520 , 1525 , 1530 and 1535 support horizontal deck 1510 . Each of the four legs 1520 , 1525 , 1530 and 1535 has a bottom edge.
Legs 1520 and 1535 are connected together via wall 1560 . Wall 1560 is shown as having perforations 1580 .
FIG. 15 also shows channel 1545 formed in the space between bottom edges of the leg 1520 and 1525 to the underside of horizontal deck 1510 . Channel 1545 allows for the water to flow through the module. FIG. 15 also shows channel 1575 formed in the space between bottom edges of the leg 1525 and 1530 to the underside of horizontal deck 1510 . Channel 1575 allows for the water to flow through the module and is connected to channel 1545 . FIG. 15 also shows channel 1555 formed in the space between bottom edges of the leg 1530 and 1535 to the underside of horizontal deck 1510 . Channel 1555 allows for the water to flow through the module and is connected to channel 1545 and 1575 .
FIGS. 15A , 15 B and 15 C show various views of module 1500 . FIG. 15A provides a top view where axes A-A and B-B are shown. FIG. 15B is a view across axis A-A where channel 1575 is shown. Legs 1525 and 1530 are also shown in this view. FIG. 15C is a view across axis B-B where channel 1545 / 1555 is shown.
FIG. 16 shows a storage and controlled outflow system 1600 . System 1600 is made of various modules. System 1600 is shown having three inlets 110 and one outlet 120 . However, there may be more inlets or less inlets 110 and outlets 120 for system 1600 than shown in FIG. 16 . The modules previously described (modules 200 , 300 , 400 , 500 , 600 , 700 , 800 , 1100 and 1200 ) are shown as being used for system 1600 . Furthermore, system 1600 is shown having a liner 1650 . This liner may be non-perforate and may not allow (i.e. prevent or stop) the water to exit the system through liner 1650 . This acts to retain the water in the system. The liner may increase the amount of the water in the system, until it exits through various openings in the system.
The modules of various embodiments of the invention are preferably made of concrete, however they may be made of other material, such as cement, gravel, aggregate (such as crushed rock or gravel made of limestone or granite, plus a fine aggregate such as sand). Such materials should be able to support a load. The modules preferably have a reinforced steel frame within the modules for support, and an outer concrete shell. Such a steel frame allows the modules strength to support a load.
The modules may have a man hole located at the top of the modules. The man hole allows maintenance people to enter the module in the event trash enters the module, and/or the modules need to be cleaned. In certain embodiments, the openings the modules are large enough to allow a man to enter the modules.
The modules may have an outlet weir with trash rack installed across the weir opening. The modules may have baffles located within the modules. The modules may have other such advantages that allow for flow control in the module.
Such flow control may also allow the modules to have a sump feature. The modules may also have an optional orifice located on various walls of the modules. The optional orifice may be larger than the perforations shown in the modules, which typically have a diameter of only a few inches. The orifice is typically 24 inches in diameter, however, the orifice described may be larger or smaller than 24 inches depending upon the size of the module.
Other objectives of the modular system may be met by providing various other modules to assist in flow control of the water within a system. These modules may have water treatment advantages that allow for the water to be treated as it flows through the system.
These treatment modules may have perforated walls and beams. The treatment modules may have an outlet hole or backwall. The outlet hole on backwall may be 24 inches. The modules may have a 12 inch sump height. The treatment modules may have a filter media to treat the water. The modules may have a trash rack and weir system to control the flow of water. The modules may have filtering, oil/water separation, TSS (total suspended solids), removal, trash and debris removal, nutrient reduction, soluble chemical capture, all dependent on placement of weirs, walls, baffles, beams, and internal outlet control devices. The treatment modules may have filtering, temperature regulation, oxygenation, introduction of chemical treatment, and sterilization capabilities all related to compartmentalized and indirect flow systems).
The treatment modules may have filter media within the modules. The modules may have an underflow collection system within the modules. The treatment modules may have an outlet pipe that is connected to the filter media. The treatment modules may be located where the modules have a floor such as modules 500 , 600 and 1100 . The treatment modules may also be located where the floor of the system is made of stone.
The treatment modules may be arranged in a flow pattern that is serpentine. This allows the water to stay in the system for the optimal amount of time for treatment before exiting the system. This allows for optimal treatment of the water.
FIG. 17 shows a type of treatment module in the modular system of the invention. Module 1700 is shown having four legs 1720 , 1725 , 1730 and 1735 . The four legs 1720 , 1725 , 1730 and 1735 support horizontal deck 1710 . Each of the four legs 1720 , 1725 , 1730 and 1735 has a bottom edge.
Legs 1720 and 1725 are connected together via a wall 1740 . Legs 1720 and 1735 are connected together via wall 1760 . Baffle 1765 is shown beneath wall 1760 . The space between legs 1725 and 1730 forms channel 1775 . Wall 1750 is shown as being a solid wall between legs 1730 and 1735 . The module 1700 is also shown having a floor 1790 .
FIG. 18 shows a type of treatment module in the modular system of the invention. Module 1800 is shown having four legs 1820 , 1825 , 1830 and 1835 . The four legs 1820 , 1825 , 1830 and 1835 support horizontal deck 1810 . Each of the four legs 1820 , 1825 , 1830 and 1835 has a bottom edge. Horizontal deck 1810 has riser 1805 . Riser 1805 may be 24 inches in height. Riser 1805 may be more or less than 24 inches in height.
Legs 1820 and 1825 are connected together to form a channel 1845 . Legs 1820 and 1835 are connected together via wall 1860 . Legs 1825 and 1830 are connected together to form a low wall 1870 . An opening 1875 is shown above low wall 1870 . The module 1800 is also shown having a floor 1890 .
FIG. 19 shows a type of treatment module in the modular system of the invention. Module 1900 is shown having four legs 1920 , 1925 , 1930 and 1935 . The four legs 1920 , 1925 , 1930 and 1935 support horizontal deck 1910 . Each of the four legs 1920 , 1925 , 1930 and 1935 has a bottom edge. Horizontal deck 1910 has riser 1905 . Riser 1905 may be 24 inches in height. Riser 1905 may be more or less than 24 inches in height.
Legs 1920 and 1925 are connected together via low wall 1940 . Window 1945 is shown above low wall 1940 . Legs 1925 and 1930 are connected to form a wall 1970 . Opening 1975 is shown in the wall connected to an outlet 1915 . Legs 1930 and 1935 are connected together to form a wall 1950 . Legs 1920 and 1935 are connected together via channel 1965 . The module 1900 is also shown having a floor 1990 .
FIG. 20 shows a type of treatment module in the modular system of the invention. Module 2000 is shown having four legs 2020 , 2025 , 2030 and 2035 . The four legs 2020 , 2025 , 2030 and 2035 support horizontal deck 2010 . Each of the four legs 2020 , 2025 , 2030 and 2035 has a bottom edge. Horizontal deck 2010 has riser 2005 . Riser 2005 may be 24 inches in height. Riser 2005 may be more or less than 24 inches in height. Inside module 2000 is filter media 2030 and outlet pipe 2085 . Legs 2030 and 2035 are connected by wall 2050 .
FIG. 21 shows a type of treatment module in the modular system of the invention. Module 2100 is shown having four corners 2120 , 2125 , 2130 and 2135 . Module 2100 is actually made up of two separate modules 2110 and 2115 . Located inside module 2100 is filter media 2130 and output pipe 2180 . Output pipe 2180 is connected to underflow collection system 2185 . Filter media 2130 is used to filter and/or treat water.
FIG. 22 shows a type of treatment module in the modular system of the invention. Module 2200 is shown having four legs 2220 , 2225 , 2230 and 2235 . The four legs 2220 , 2225 , 2230 and 2235 support horizontal deck 2210 . Each of the four legs 2220 , 2225 , 2230 and 2235 has a bottom edge. Horizontal deck 2210 has riser 2205 . Riser 2205 may be 24 inches in height.
Legs 2220 and 2225 are connected together to form a channel 2245 . Legs 2220 and 2235 are connected together via wall 2260 . Weir 2265 is above wall 2260 . Trash rack 2262 is shown installed in weir 2265 . Legs 2225 and 2230 are connected together via wall 2270 . Module 2200 is also shown having a floor 2290 .
Various embodiments of the system may be arranged as either sealed or non-sealed systems. Sealed systems may have a non-perforate liner or another such barrier that will prevent the water from leaving the system. Sealed systems typically only allow water to leave the system via inlets and outlets.
Non-sealed systems do not have a non-perforate liner. Water may leave the non-sealed systems via perforations in the walls of the perimeter modules and the outlets of the system. Furthermore, in a non-sealed system, water may leave through the floor of the system.
Other embodiments of the invention involve having stackable systems with a drop outlet structure with control orifice. The drop outlet structure is for a multilayer or stackable system (as shown in FIGS. 9 , 9 A, 10 and 10 A), where the water drops from a module in the upper stack to a module in the lower stack. In such a system, the modules may be arranged stacked on a stone base. Such a system may have an outlet control rise with orifice holes and an overflow weir. Such a system may have various weirs located in the system to control flow in the system for accumulation of water.
FIGS. 2B , 2 C, 3 B, 3 C, 4 B, 4 C, 5 B, 5 C, 6 B, 6 C, 7 B, 7 C, 8 B, 8 C, 11 B, 11 C, 12 B, 12 C, 13 B, 13 C, 14 B and 14 C allow show modules that may be stackable or are adapted to be stackable. These modules have indentations shown in the top right and top left of each module that are adapted to receive the legs of a corresponding module. This allows the modules to be stacked upon one another. Modules, thus, have a lateral friction element that prevents the modules from moving.
In certain embodiments, stackable systems may also involve a top level not have a floor (floorless) and the bottom level not have a ceiling (ceilingless), creating a height volume area of twice the size of a module. Certain embodiments also are directed to mixed systems with a mixture of double-stack and single-stack systems. Such systems have a mixture of volume heights, as modules of smaller and greater sizes may be used in such systems.
FIGS. 23-28 show examples of stackable modules. FIG. 23 shows a type of stackable module that may be used is a multilayer or stacked system. Module 2300 is shown as being made of two modules, a lower module and an upper module. The lower module has four legs 2320 , 2325 , 2330 and 2335 . The four legs 2320 , 2325 , 2330 and 2335 support the upper module. Each of the four legs 2320 , 2325 , 2330 and 2335 has a bottom edge. The upper module also has four legs 2320 A, 2325 A, 2330 A, and 2335 A. Each of the four legs 2320 A, 2325 , 2330 A and 2335 A has a bottom edge. The four legs 2320 A, 2325 A, 2330 A and 2335 A support a horizontal deck 2310 A. Legs 2320 and 2325 are connected together by a beam 2340 . Window 2345 is shown above beam 2340 . Legs 2320 and 2335 are connected via beam 2360 with window 2365 shown above beam 2360 .
Channel 2355 is shown between leg 2330 and 2335 ; channel 2345 A is shown between leg 2320 A and 2325 A; channel 2375 A is shown between leg 2325 A and 2330 A; channel 2355 A is shown between let 2330 A and 2335 A; and channel 2365 A is shown between leg 2320 A and 2335 A. The lower module has opening 2310 in its ceiling instead of having a horizontal deck.
FIG. 24 shows a type of stackable module that may be used is a multilayer or stacked system. Module 2400 is shown as being made of two modules, a lower module and an upper module. The lower module has four legs 2420 , 2425 , 2430 and 2345 . The four legs 2420 , 2425 , 2430 and 2435 support the upper module. Each of the four legs 2420 , 2425 , 2430 and 2435 has a bottom edge. The upper module also has four legs 2420 A, 2425 A, 2430 A, and 2435 A. Each of the four legs 2420 A, 2425 , 2430 A and 2435 A has a bottom edge. The four legs 2420 A, 2425 A, 2430 A and 2435 A support a horizontal deck 2410 A.
Legs 2420 and 2435 are connected together by a beam 2460 . Window 2465 is shown above beam 2460 . Legs 2420 A and 2435 A are connected via beam 2460 A with window 2465 A shown above beam 2460 A. Legs 2425 and 2430 are connected together via beam 2470 . Window 2475 is shown above beam 2470 . Legs 2425 A and 2430 A are connected together via beam 2470 A. Window 2475 A is shown above beam 2470 A. Channel 2455 is shown between leg 2430 and 2435 ; channel 2455 A is shown between leg 2430 A and 2435 A; channel 2445 is shown between leg 2420 and 2425 ; and channel 2445 A is shown between leg 2320 A and 2325 A. The lower module has opening 2410 in its ceiling instead of having a horizontal deck.
FIG. 25 shows a type of stackable module that may be used is a multilayer or stacked system. Module 2500 is shown as being made of two modules, a lower module and an upper module. The lower module has four legs 2520 , 2525 , 2530 and 2545 . The four legs 2520 , 2525 , 2530 and 2535 support the upper module. Each of the four legs 2520 , 2525 , 2530 and 2535 has a bottom edge. The upper module also has four legs 2520 A, 2525 A, 2530 A, and 2535 A. Each of the four legs 2520 A, 2525 , 2530 A and 2535 A has a bottom edge. The four legs 2520 A, 2525 A, 2530 A and 2535 A support a horizontal deck 2510 A.
Legs 2520 and 2535 are connected together by a beam 2560 . Window 2565 is shown above beam 2560 . Legs 2520 A and 2535 A are connected via beam 2560 A with window 2565 A shown above beam 2560 A. Legs 2525 and 2530 are connected together via wall 2570 . Legs 2525 A and 2530 A are connected together via wall 2570 A. Perforations 2580 are shown in wall 2570 and wall 2570 A. Channel 2555 is shown between leg 2530 and 2455 ; channel 2555 A is shown between leg 2530 A and 2535 A; channel 2545 is shown between leg 2520 and 2525 ; and channel 2545 A is shown between leg 2520 A and 2525 A. The lower module has opening 2510 in its ceiling instead of having a horizontal deck.
FIG. 26 shows a type of stackable module that may be used is a multilayer or stacked system. Module 2600 is shown as being made of two modules, a lower module and an upper module. The lower module has four legs 2620 , 2625 , 2630 and 2645 . The four legs 2620 , 2625 , 2630 and 2635 support the upper module. Each of the four legs 2620 , 2625 , 2630 and 2635 has a bottom edge. The upper module also has four legs 2620 A, 2625 A, 2630 A, and 2635 A. Each of the four legs 2620 A, 2625 , 2630 A and 2635 A has a bottom edge. The four legs 2620 A, 2625 A, 2630 A and 2635 A support a horizontal deck 2610 A.
Legs 2620 and 2635 are connected together by a beam 2660 . Window 2665 is shown above beam 2660 . Legs 2620 A and 2635 A are connected together by a beam 2660 A. Window 2665 A is shown above beam 2660 A. Legs 2625 and 2630 are connected together via wall 2670 . Legs 2625 A and 2630 A are connected together via wall 2670 A. Legs 2630 and 2635 are connected together via wall 2650 . Legs 2630 A and 2635 A are connected together via wall 2650 A. Perforations 2680 are shown in wall 2670 , wall 2670 A, wall 2650 and wall 2650 A. Channel 2645 is shown between leg 2620 and 2625 ; and channel 2645 A is shown between leg 2620 A and 2625 A. The lower module has opening 2610 in its ceiling instead of having a horizontal deck.
FIG. 27 shows a type of stackable module that may be used is a multilayer or stacked system. Module 2700 is shown as being made of two modules, a lower module and an upper module. The lower module has four legs 2720 , 2725 , 2730 and 2745 . The four legs 2720 , 2725 , 2730 and 2735 support the upper module. Each of the four legs 2720 , 2725 , 2730 and 2735 has a bottom edge. The upper module also has four legs 2720 A, 2725 A, 2730 A, and 2735 A. Each of the four legs 2720 A, 2725 , 2730 A and 2735 A has a bottom edge. The four legs 2720 A, 2725 A, 2730 A and 2735 A support a horizontal deck 2710 A.
Legs 2720 and 2735 are connected together by a beam 2760 . Window 2765 is shown above beam 2760 . Legs 2720 A and 2735 A are connected together by a beam 2760 A. Window 2765 A is shown above beam 2760 A. Legs 2725 and 2730 are connected together via wall 2770 . Legs 2725 A and 2730 A are connected together via wall 2770 A. Legs 2730 and 2735 are connected together via wall 2750 . Legs 2730 A and 2735 A are connected together via wall 2750 A. Perforations 2780 are shown in wall 2770 , wall 2770 A, wall 2750 and wall 2750 A. Wall 2750 A also has opening 2718 and output pipe 2715 A. Channel 2745 is shown between leg 2720 and 2725 ; and channel 2745 A is shown between leg 2720 A and 2625 A. The lower module has floor 2710 A.
FIG. 28 shows a type of stackable module that may be used is a multilayer or stacked system. Module 2800 is shown as being made of two modules, a lower module and an upper module. The lower module has four legs 2820 , 2825 , 2830 and 2845 . The four legs 2820 , 2825 , 2830 and 2835 support the upper module. Each of the four legs 2820 , 2825 , 2830 and 2835 has a bottom edge. The upper module also has four legs 2820 A, 2825 A, 2830 A, and 2835 A. Each of the four legs 2820 A, 2825 , 2830 A and 2835 A has a bottom edge. The four legs 2820 A, 2825 A, 2830 A and 2835 A support a horizontal deck 2810 A.
Legs 2820 and 2835 are connected together by a beam 2860 . Window 2865 is shown above beam 2860 . Legs 2820 A and 2835 A are connected together by a beam 2860 A. Window 2865 A is shown above beam 2860 A. Legs 2825 and 2830 are connected together via wall 2870 . Legs 2825 A and 2830 A are connected together via wall 2870 A. Legs 2820 and 2825 are connected together via wall 2640 . Legs 2820 A and 2825 A are connected together via wall 2840 A. Perforations 2680 are shown in wall 2870 , wall 2870 A, wall 2840 and wall 2840 A. Channel 2855 is shown between leg 2830 and 2835 ; and channel 2855 A is shown between leg 2830 A and 2835 A. The lower module has opening 2810 in its ceiling instead of having a horizontal deck. Wall 2840 A has an opening 2890 A.
Dimensions of the modules shown in FIGS. 23-28 may be shown has having 12 inch beams (12 inches being the beam height); however, beams with other heights may be used, such as having beams that have a height of greater than 12 inches. The modules shown in FIGS. 23-28 are typically are approximately 8 feet wide and 8 feet deep and have a lower module height of 3 feet 8 inches and an upper modules height of 4 feet 8 inches when employing 12 inch beams. However, the modules shown in these figures can have a greater and smaller size. The modules can range in height, so as to allow a man to enter the module to service it.
Furthermore, modules typically have the ability to support 10,000 to 14,000 pounds of weight. However, modules may support additional weight based on materials used, such as having a steel frame internal to the concrete outer shell. Modules may be made of other materials known in the art, and may be made of materials that are more expensive and have greater load bearing capabilities, if desired.
Embodiments of the present invention have various advantages for the environment and have additional “green advantages” that have a positive impact on the environment. Notably, the present invention has a smaller environmental footprint, has more optimal use of area via geometry, and has less stone hauling and less material use than existing systems.
Embodiments of the present invention may do multiple processes, such as treatment, in a single module, and use less material and impact less surface area than existing systems. Embodiments of the present invention have stackability of the modules and/or may be a multilayered system, which reduces the environmental footprint of the systems.
Embodiments of the present invention have flow control to reduce erosion in receiving water, have water quality control treatment processes, have water reuse processing and storage, and also have irrigation runoff usage. Embodiments of the present invention have wastewater secondary grey water systems for use for irrigation, have non-sanitary water use and savings, treatment and storage.
Embodiments of the present invention may have water reuse for fire protection, temperature control of warmed parking lot runoff, wastewater detention relieving undersized public utilities loading, combine sewer storage and treatment, and surge flow protection. Embodiments of the present invention have ground water recharge, and may be used in conjunction with bio retention systems.
Embodiments of the present invention may support elements of green designs by virtue of the application. The material on construction is green by being a natural product. Embodiments of the present invention support fuel and energy reduction by a multi-use concept. Embodiments of the present invention support water reuse for secondary functions and water flow control to reduce the environmental impacts for receiving water, such as counterbalancing increased flows due to increase in hard surfaces.
While the invention has been specifically described in connection with certain specific embodiments thereof, it is to be understood that this is by way of illustration and not of limitation and that various changes and modifications in form and details may be made thereto, and the scope of the appended claims should be construed as broadly as the prior art will permit.
The description of the invention is merely exemplary in nature, and thus, variations that do not depart from the gist of the invention are intended to be within the scope of the invention. Such variations are not to be regarded as a departure from the spirit and scope of the invention.
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Modular storage and controlled outflow systems for controlling a flow of water and methods of assembly of modular storage and controlled outflow systems having indirect flow of water through the system. Modular systems for controlling a flow of water having beams extending across the modules to direct the flow of water in an indirect manner or a serpentine or semi-serpentine manner. Modular storage and controlled outflow systems for treatment and filtration of water.
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BACKGROUND OF THE INVENTION
The present invention relates generally to pump jacks and more specifically to hydraulic pump jacks for oil wells and other applications.
Oil well pump jacks have traditionally consisted of complex mechanical devices with linkage units for transforming rotary motion from motors into the reciprocating motion needed for pumping. Conventional pump jacks generally require a relatively large amount of space in order to provide adequate clearance for the various moving parts and have necessarily been positioned aboveground. These pump jacks also require firmly anchored base supports or support pads in order to properly align the drive unit of the apparatus with the sucker rod of the oil well. The size and clearance requirements associated with traditional oil well pump jacks have proven to be a problem in agricultural areas utilizing center pivot irrigation systems and other large farm machinery. In addition, above ground pump jacks tend to be noisy and unsightly, thereby making oil wells aesthetically undesirable in populated or scenic areas. A further disadvantage of conventional pump jacks is the tendency of systems having multiple moving parts to break down at frequent intervals. If the number of moving parts in such systems are reduced, then desirable pumping characteristics having to do with pump stroke length and speed are generally sacrificed.
A need exists for an oil well pump jack which is reliable and which can also operate in a confined space. The pump jack should be capable of adaptation to different types of oil wells and should be capable of providing desirable pump stroke performance.
SUMMARY OF THE INVENTION
The present invention is a hydraulic pump jack which is constructed in a compact unit that may be directly attached to the head casing of an oil well.
Accordingly, it is a primary object of the present invention to furnish a hydraulic pump jack in a self-contained unit.
It is a further object of the present invention to provide a pump jack that may be attached directly to the head of an oil well casing.
It is a further object of the present invention to provide a pump jack that may be mounted below the ground surface.
It is a further object of the present invention to provide a pump jack that has a hydraulic valve system which allows a hydraulic cylinder to be operated at a preselected speed.
It is a further object of the present invention to provide a pump jack that has a hollow piston shaft for connection with an oil well sucker rod.
It is a further object of the present invention to provide a pump jack that may be powered by an electric or fossil fuel pump motor.
It is a further object of the present invention to provide a pump jack that has an adjustable stroke length.
It is a further object of the present invention to provide a pump jack that has a cooling chamber for hydraulic fluid.
It is a further object of the present invention to provide a pump jack that has relatively few moving parts.
It is a further object of the present invention to provide a pump jack that is compact in size.
It is a further object of the present invention to provide a pump jack that may be placed in a manhole type vault.
It is a further object of the present invention to provide a pump jack which may be easily removed from an oil well for repairs with a boom truck.
It is a further object of the present invention to provide a pump jack with a piston which does not produce a side thrust on the sucker rod.
It is a further object of the present invention to provide a pump jack which will not slip on a mounting pad.
It is a further object of the present invention to provide a pump jack which will be nearly maintenance free.
It is a further object of the present invention to provide a pump jack which may be built in a variety of sizes.
It is a further object of the present invention to provide a pump jack which eliminates the need for a pitman and mechanical gears.
It is a further object of the present invention to provide a pump jack which is contained in a cylindrical housing.
It is a further object of the present invention to provide a pump jack which is equipped with a shear pin at the connection with the sucker rod.
It is a further object of the present invention to provide a pump jack which may utilize counterweights.
It is a further object of the present invention to provide a pump jack which has an integrated hydraulic pump and control assembly contained in a sub unit mounted on the pump jack housing.
It is a further object of the present invention to provide a pump jack which is aesthetically pleasing in appearance.
It is a further object of the present invention to provide a pump jack that is safe to operate.
It is a further object of the present invention to provide a pump jack that is relatively inexpensive to construct and maintain.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a perspective view of a hydraulic pump jack.
FIG. 2 is a cross-sectional view of a hydraulic pump jack showing the piston in its up stroke motion.
FIG. 3 is a cross-sectional view of a hydraulic pump jack with the piston at the beginning of its down stroke.
FIG. 4 is a cross-sectional view of a hydraulic pump jack with the piston at the beginning of its up stroke.
FIG. 5 is a cross-sectional view of a hydraulic pump jack mounted in an underground operating vault.
FIG. 6 is a cross-sectional view of a hydraulic pump jack with counter weights.
FIG. 7 is a side view showing removal of a hydraulic pump jack from an operating vault.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
As shown by FIG. 1, the hydraulic pump jack 10 of the present invention has a generally cylindrical shape. The cylinder body 11 is mounted vertically on an oil well casing 12 by means of a collar arrangement 14 and mounting bolts 15. The collar arrangement 14 allows the pump jack 10 to be securely affixed to the oil well casing 12 and yet, allows the pump jack 10 to be easily removed for repairs or routine maintenance. A blind end cap 17 positioned at the top of the cylinder body 11 is also provided with a collar arrangement 16 which allows the cap 17 to be removed; thus, providing access to the piston 40 for maintenance purposes. As shown by FIG. 2, a piston 40 provided with piston seals or rings 41 is slideably mounted within the pump jack cylinder body 11. A piston rod 42, coaxial with the longitudinal axis of the cylinder 11, is secured to the piston 40 by means of a bolt 47, or other conventional attachment means well known in the art. A rod end cap 44 is welded, or otherwise rigidly attached to the interior wall of the cylinder 11, and is provided with a rod bearing 45 and rod packing 46 for accepting a piston rod 42 in sliding and sealing contact. The piston rod 42 is tubular and adapted to accept an oil well sucker rod 13 in a telescoping relationship, as shown in FIG. 2. A piston rod collar 43 allows the piston rod 42 to be attached to the sucker rod 13 at a pre-selected position. It will be seen that this telescoping arrangement provides for straight line pumping and prevents side thrust on the sucker rod 13.
As shown in FIGS. 1 and 2, a valve unit 20 is positioned on the side of the pump jack cylinder 11 and communicates with the upper portion of the cylinder 11 cavity through an orifice 48. The valve unit 20 is preferably bolted, or otherwise removably mounted on the cylinder 11, to facilitate removal for maintenance purposes. A hydraulic pump unit 21 is mounted adjacent to the valve unit 20 and provides hydraulic fluid under pressure to the valve unit 20. A fluid reservoir 22 is attached to the cylinder 11 directly above the valve unit 20 and pump unit 21. A hydraulic unit supply line 25 places the reservoir 22 in fluid communication with the pump unit 21 and a hydraulic fluid return line 26 provides fluid communication between the reservoir 22 and the valve unit 20. In the preferred embodiments, the hydraulic pump unit 21 contains an electric motor (not shown) which is energized by means of a power supply line 23. However, fossil fuel motors (not shown) could also be used and may be required in many remote areas. The particular configuration of the valve unit 20, pump unit 21 and return reservoir unit 22, as shown in the preferred embodiments, could, of course, be modified for various circumstances. For example, it might be desirable to maintain the reservoir unit 22 and pump unit 21 separate from the pump jack cylinder 11. These units 22, 21 would then be connected to the valve unit 20 with appropriate hydraulic fluid lines. This second type of arrangement might be particularly desirable when the pump jack 10 is mounted below ground, as shown in FIG. 5, or when the hydraulic fluid pump motor (not shown) is a fossil fuel type, which is more conveniently maintained at ground level.
As shown in FIG. 2, a valve actuator rod 28 projects downward from the valve unit 20 and is pivotally connected to one end of a pivot bar 31. A pivot bar opening 32 in the wall of the cylinder 11 below the rod end cap 44 allows the pivot bar 31 to enter the lower portion of the cylinder 11 cavity. The pivot bar 31 is pivotally mounted on a pivot bar shaft 34 which is welded or otherwise conventionally attached to the interior walls of the cylinder 11 below the rod end cap 44. The end of the pivot bar 31 positioned inside the cylinder 11 is pivotally attached to a pump stroke adjuster bar 36. The lower end of the adjuster bar 36 is slideably mounted within an adjuster bar guide 39, which is in turn welded or otherwise conventionally attached to the lower end of the piston rod 42. Adjuster stops 38 are slideably bolted to the adjuster bar 36 and may be moved up or down to produce a desired pump stroke length as will be more fully described below.
The operation of the pump jack will now be described. An inflow of hydraulic fluid through the orifice 48 causes the piston 40 to rise in the cylinder 11, thereby raising the sucker rod 13 of the oil well. When fluid pressure is released, the force of gravity on the sucker rod 13 and piston 40 causes the piston 40 to descend until fluid pressure is again applied for the upward pump stroke or until the piston 40 contacts the rod end cap 44. In the preferred embodiments, the inflow and exhaust of hydraulic fluid from the cylinder 11 is controlled by a conventional three-way spool valve (not shown). In the preferred embodiments, the valve unit 20 is actuated by a valve actuator rod 28 which may be positioned either "up" or "down". When the actuator rod 28 is in the "down" position, as shown in FIG. 3, hydraulic fluid within the cylinder 11 is allowed to pass out through the orifice 48 and through the valve unit 20 and exhaust line 26 into the hydraulic fluid reservoir 22. When the actuator rod 28 is in the "up" position, as shown in FIG. 3, hydraulic fluid is pumped from the reservoir 22 through the hydraulic fluid supply line 25, pumping unit 21, and valve unit 20, and orifice 48 into the pump jack cylinder 11. It may be seen from FIGS. 3 and 4 that the actuator rod 28 is placed in either the "up" or the "down" position by the relative motion of the adjuster bar guide 39, with respect to the adjuster stops 38. When the piston rod 42 has risen to a sufficient height, the adjuster bar guide 39 contacts the upper adjuster stop 38, causing a rotational movement of the pivot bar 31 and thence a downward movement of the valve actuator rod 28. A downward movement of the actuator rod 28 changes the porting arrangement within the valve unit 20 releasing the fluid pressure within the cylinder 11, thereby causing the piston rod 42 to begin its downward stroke. The actuator rod 28 remains on the "down" position until the piston rod 42 has descended sufficiently far to cause the adjuster bar guide 39 to contact the lower adjuster stop 28. The downward movement thus produced in the adjuster bar 36 causes an upward displacement of the actuator rod 28, which again changes the porting arrangement within the valve unit 20, causing the hydraulic fluid to flow into the cylinder 11, thereby beginning the upward piston 40 stroke, as shown in FIG. 4. It will be seen from the above, that by placing the adjuster stops 38 farther apart, the pump stroke is lengthened and conversely by moving the adjuster stops 38 closer together, the pump stroke is stortened. Pressure control units, or other control means (not shown) well known in the hydraulic arts, may be used to control or vary the speed of the punp stroke as may be desired for particular applications. In pump jacks 10 used on large wells and heavy pumping equipment, it is often necessary to provide counterweights in order to eliminate the need to overcome the gravitational force on the pump apparatus during each upward stroke. As shown in FIG. 6, this result may be accomplished by mounting pulleys 56 within the cylinder 11 immediately below the rod end cap 44. The pulleys 56 may be suspended from the rod end cap 44 or otherwise attached by conventional mounting means well known in the art. Cables 57 may then be attached to the lower end of the piston rod 42 and threaded over the pulleys 56. Weights 58, sufficient to offset the weight of the pumping apparatus 10, the sucker rod 13 and part of the load of fluid being pumped are then attached to the free end of the cable 57.
The compact nature of the hydraulic pump jack 10 of the present invention allows it to be conveniently mounted underground, as shown in FIGS. 5 and 7 in a manhole type vault arrangement. A manhole cover 50 may be provided to keep out moisture. The underground arrangement prevents freezing and other undesirable conditions associated with the weather experience in surface mounting, making the pumpjack 10 operational in a number of adverse weather environments where a surface pump might be unfeasible. The underground mounting is also desirable for a variety of land utilization purposes. As shown by FIG. 3, a metal loop 18 may be provided at the top of the pump jack 10 to facilitate placement and removal of the pump jack by means of a boom truck 51, or other hoisting device.
Thus, it can be seen that a hydraulic pump jack 10 has been provided which is compact in size, transportable, easily maintainable, and extremely reliable. Obviously, many modifications and variations of the described invention are possible. For example, a double acting cylinder might be employed rather than the single acting cylinder which was specifically described in the preferred embodiment. It is, therefore, understood within the scope of the inventor's claim that the invention may be practiced otherwise than as specifically described.
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A hydraulic pump jack is disclosed which utilizes a hydraulic cylinder to provide pumping force to an oil well sucker rod. The hydraulic pump jack may be directly mounted on an oil well casing either above or below ground. A tubular piston rod which may be connected to a sucker rod in telescoping relation for transmitting vertical force without side loading is also disclosed. Apparatus for mounting the piston rod within a cylindrical housing is described. The use of a counter weight system for balancing the pump load is also described.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application claims priority to patent application Ser. No. 12/196,469, filed Aug. 22, 2008, now U.S. Pat. No. 7,837,524, which itself claimed priority to provisional application Ser. No. 60/957,206, filed Aug. 22, 2007.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to devices and methods for marine propulsion and liquid pumping, and, more particularly, to such devices and methods for improving a performance of marine propulsion and pumping systems.
2. Description of Related Art
A cutlass bearing (common usage) is a special type of bearing used extensively in marine and industrial applications for bearings operating under water or in other liquids. Cutlass bearings have no moving parts, and the bearing material is usually composed of a type of synthetic rubber and/or polymer, which supports the propeller shaft. Cutlass bearings are designed to utilize the lubricating properties of a hydraulic film of the surrounding water/fluid in which the bearing is operating. For this reason channels are designed within the bearing surface to promote the flow of liquids through the bearing, assuring proper lubrication while cooling the bearing and shaft surfaces at the same time.
A common problem in propeller-driven vessels is fouling of the propeller and shaft with lines, rope, netting, plastic bags, etc. When propeller shafts are fouled, often the fouling material is wound around the shaft in the section between the cutlass bearing and propeller hub. When this happens, the flow of water through the cutlass bearing is restricted and, in some cases, is cut off entirely. A vessel operator is sometimes made aware of a fouling condition because of vibration in the propulsion gear and diminished performance. If he is aware of the fouling, the operator will usually attempt to clear it by reversing the propulsion gear in an attempt to release the wound-up fouling, or, when that is not successful, someone may go overboard to clear the fouled propulsion gear. Even a small amount of fouling right next to the cutlass bearing will severely impede the flow of lubricating water because the cross-sectional area of the water channels in the bearing is relatively small. Small amounts of fouling around a propeller shaft, however, often goes unnoticed for extended periods. In this situation, the cutlass bearing suffers premature wear because of starvation of lubricating water. Furthermore, it is fairly common to have the aft ends of bearings and bearing housings physically damaged and abraded when fouling materials are tightly wrapped around the propeller shaft for an extended period.
Several devices have been designed and marketed for the purpose of preventing propeller and shaft fouling. They are generally based on rotary cutters that are attached to the shaft and act to cut the fouling materials as they begin to wrap around the shaft. Although some of these devices work well under the ideal conditions for which they were designed, they are not as effective in extreme conditions. These cutting devices generally require frequent repair and replacement in heavy use applications such as those experienced by vessels operating in the commercial sector. These devices also are not specifically designed to increase the flow of water through the cutlass bearing.
Therefore, it would be beneficial to provide a simple, robust, and dependable device and method of manufacture and use for substantially preventing fouling of propellers, shafts, and cutlass bearings in marine vehicles.
SUMMARY OF THE INVENTION
The present invention is directed to a device that is mountable on a propeller shaft abaft (in back of) a cutlass bearing for improving a performance of a propeller-driven propulsion apparatus. The device comprises an annular collar affixable for rotation with and dimensioned for positioning about a shaft of a propeller in a longitudinal space between a propeller hub and a cutlass bearing. A plurality of impeller blades are affixed to and extend radially out from the collar in spaced-apart relation. Each impeller blade has a length sufficient to nearly span the longitudinal space between the propeller hub and the cutlass bearing, leaving a gap between forward ends of the blades and the cutlass bearing.
An annular ring is affixed in spanning relation to the forward ends of the impeller blades. A bridging element extends from one of the annular ring and the cutlass bearing, and is positioned to longitudinally bridge the gap between the blades forward ends and the cutlass bearing, thereby substantially enclosing the gap.
In use, the impeller blades rotate in conjunction with the propeller shaft, and in doing so they create a centrifugal flow of water outward from the shaft, which in turn creates suction along the shaft surface and abaft the cutlass bearing. The suction draws water through the water channels in the bearing surface. The pumping action of the impeller blades, along with the greatly increased discharge area for water around the periphery of the device, greatly decreases the likelihood that fouling around the propeller shaft can restrict the flow through the cutlass bearing. Additionally, the outside edges of the impeller blades help cut through and shear away the rotating fouling materials over time, making it much more likely that the fouling material eventually be cut and thrown off than it would when wound up on a relatively smooth shaft surface.
The device can be easily attached to the existing propulsion gear of a vessel in order to improve the dependability and performance, and reduce the maintenance cost, of the propulsion gear. The invention can relate to that sector of vessels that utilize a propulsion system composed of an inboard engine that turns a drive shaft exiting through the hull to turn a propeller. This type of propulsion apparatus normally uses one or more cutlass bearings to support the shaft in its underwater section.
The device of the present invention increases water flow through normal cutlass bearings and decreases the likelihood that the water flow be severely impeded by propeller and shaft fouling. The device, even with fouling around the propeller shaft, lessens the likelihood of bearing damage owing to lack of water circulation. In order to achieve this, the device has multiple radially mounted blades that extend from the shaft surface outward. These blades act as an impeller to create centrifugal pumping action in the water when the shaft is rotated. The periphery of the device also creates a large area for fluid discharge, which makes severely flow restriction by fouling less likely.
The present device, when mounted abaft a cutlass bearing, shields the bearing from physical damage and erosion from fouling materials that may become wrapped around the propeller shaft. The blades of the device mounted immediately abaft the bearing prevent fouling materials from reaching the after end of the bearing and bearing housing, thereby protecting the bearing and housing from direct abrasion.
The present device is robust and durable, and is able to remain effective under extreme conditions and extended use. The device can be constructed of, for example, stainless steel or other corrosion-resistant metal alloys with welded or cast components and does not depend on sharp edges or close tolerances to remain effective.
The features that characterize the invention, both as to organization and method of operation, together with further objects and advantages thereof, will be better understood from the following description used in conjunction with the accompanying drawing. It is to be expressly understood that the drawing is for the purpose of illustration and description and is not intended as a definition of the limits of the invention. These and other objects attained, and advantages offered, by the present invention will become more fully apparent as the description that now follows is read in conjunction with the accompanying drawing.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 (prior art) is a cross-sectional side view a propulsion setup for inboard engine vessel.
FIG. 2 (prior art) cross-sectional end view of a propeller shaft, cutlass bearing, bearing housing, and water channel grooves.
FIG. 3 is a cross-sectional side view of a device of the present invention mounted on a propeller shaft.
FIG. 4 is an end view of the device of FIG. 3 , illustrating a plurality of impeller blades equally spaced around the periphery.
FIGS. 5A-5D depict various impeller blade embodiments: FIG. 5A , a flat plate blade of rectangular cross section with square outside edge; FIG. 5B , a flat blade design with pointed ends; FIG. 5C , a flat blade design with serrated edge; FIG. 5D , a curved blade.
FIGS. 6 A, 6 B are end views of two impeller blade placement embodiments:
FIG. 6A , a blade placed with its radial axis collinear with a radial axis of the shaft; FIG. 6B , an impeller blade with a radial axis at an angle with respect to the shaft radial axis.
FIGS. 7 A, 7 B, 7 C illustrate three embodiments varying in longitudinal placement of the impeller blades: FIG. 7A , the longitudinal axis of the impeller blades parallel with the shaft longitudinal axis; FIG. 7B , the longitudinal axis of the impeller blades at an angle with the shaft longitudinal axis; FIG. 7C , the longitudinal axis of the impeller blades is curved downward in a forward direction.
FIG. 8 illustrates another embodiment of the invention that includes a fairing and a different impeller profile.
FIG. 9 illustrates an embodiment designed for intermediate shaft bearings.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
A description of the preferred embodiments of the present invention will now be presented with reference to FIGS. 1-9 .
In FIGS. 1 and 2 are shown a typical marine vehicle arrangement of a propeller hub 101 , drive shaft 102 , cutlass bearings 103 , bearing housing 104 , water inlet 105 , and bearing-to-propeller dimension 106 . S 1 and S 2 are an aft strut and intermediate strut, respectively, which support the bearing housings 104 . Vessels with relatively short shafts generally use only one bearing S 1 . Intermediate struts S 2 and bearings 103 are typically used on vessels with longer shafts. FIG. 2 further includes an illustration of the water channel grooves 107 in the cutlass bearing 103 .
FIG. 3 shows a cross-sectional side view of a propulsion setup with an embodiment of a device 10 of the present invention mounted in the space 106 abaft the cutlass bearing 103 and before the propeller 100 . For this type of application the device 10 is manufactured to fit the available space 106 , with sufficient clearance to provide for some lateral and longitudinal movement of the shaft. A substantially annular collar 108 is dimensioned for placement over the propeller shaft 102 and extends approximately half the distance of the total length of the distance 106 . Multiple setscrews 109 in the collar 108 can be used to lock the device to the shaft 102 . An annular back-plate 110 is welded to the collar 108 and fits flush against the propeller hub 101 in this embodiment. As an alternative affixing means of locking the device to the shaft 102 , the device may be attached with multiple cap screws fastening the back-plate 110 to tapped holes in the propeller hub 101 .
Multiple equally spaced impeller blades 111 are disposed radially around the device 10 and are welded to the collar 108 and back-plate 110 . A length 114 of the impeller blades 111 plus a width 115 of the backplate 110 nearly spans the distance 106 , leaving a gap 118 to allow for sufficient clearance between the impeller blades and bearing housing 104 . Forward ends 116 of the impeller blades 111 are welded to an annular ring 112 , which holds the forward ends 116 of the impeller blades 111 in place. The annular ring 112 extends a short distance 119 over an outside 117 of the bearing housing 104 , thereby covering the gap 118 between the impeller blades 111 and bearing housing 104 .
FIG. 4 shows an end view of the device 10 , with a plurality of impeller blades 111 substantially equally spaced around the shaft 102 .
FIGS. 5A-5D depict various impeller blade cross-section embodiments that have been contemplated for use in the invention, although these are not intended as limitations. A simple design 111 a ( FIG. 5A ) comprises a flat plate blade of rectangular cross section with square outside edge 120 a . FIG. 5B illustrates a flat blade design 111 b with pointed outside edges 120 b . FIG. 5C illustrates a flat blade design 111 c with serrated outside edges 120 c . FIG. 5D illustrates a curved blade 111 d with a pointed outside edge 120 d.
FIGS. 6 A, 6 B depict end views of two impeller blade placement embodiments 10 a , 10 b , with the embodiment 10 a of FIG. 6A having a blade 111 placed with a radial axis 121 collinear with a radius 122 extending from the shaft axis 123 . In the embodiment 10 b of FIG. 6B , an impeller blade 111 ′ is placed with its radial axis 121 ′ at an angle 126 with respect to the radius 122 extending from the shaft axis 123 . The angle 126 can be in a range of 0 to 45 degrees, for example.
FIGS. 7A-7C depict embodiments 10 c , 10 d in longitudinal placements of the impeller blades 111 ″, 111 ′″. The longitudinal axis 124 ″ of the impeller blades 111 ″ can be parallel to the collar axis 127 , which in use is collinear with the shaft axis 123 , as depicted in FIG. 7A , or the longitudinal axis 124 ″ can be placed at an angle 125 with respect to the collar axis 127 , as depicted in FIG. 7B . Alternatively, the impeller blades 111 ″″ can be downwardly curved in a forward direction with respect to the shaft axis 123 , as depicted in FIG. 7C . The longitudinal blade angle 125 can range between 0 and 30 degrees, for example.
All the variations in blade cross section and placement depicted in FIGS. 5A-7C are capable of successfully achieving the objects of this invention. It is evident that the options in blade cross-section design and placement will only serve to enhance the performance of the invention and provide more options for particular applications. For example, it would seem reasonable that blades and annular rings with sharp and/or serrated edges will cut through fouling better, while curved blade sections will be better at creating pumping action. It is also evident that placing the blades at an angle to the longitudinal axis of the shaft, or having helical blades, may be used to create positive thrust with the device. The performance benefits of a certain blade design and placement scheme for a device can be weighed against the cost of its manufacture, durability, and maintenance.
Also contemplated in the design of the device are various shaped fairings that may be fixed to the existing bearing housing forward of the device. The benefits of such fairings include that they (1) provide a better hydrodynamic profile, and lower resistance of the device, (2) improve the pumping ability of the invented device by serving as a volute of a pump, (3) help prevent fouling materials from jamming the device.
FIG. 8 shows another embodiment 10 e of the invention that includes a fairing and alternative impeller profile. The annular fairing ring 113 can be mounted to the bearing housing 104 with tapped screws. Forward annular ring 112 e and impeller blades 111 e are designed to fit the sleeker profile, as compared with the embodiment 10 of FIG. 3 , with the annular ring 112 e in this embodiment 10 e not extending over the bearing housing 104 .
For intermediate bearings S 2 , where there is no propeller behind the bearing S 2 , the device 10 f can have a different profile. FIG. 9 depicts one embodiment 10 f of the invention designed for intermediate shaft bearings S 2 . A redesigned impeller profile 111 f and the absence of a back plate present a more hydrodynamic profile, while other elements such as 112 f , 113 f , and 109 remain similar to the embodiments shown above. The collar 108 f can have a rounded rear edge 127 for improved hydrodynamic performance.
It will be understood by one of skill in the art that the embodiment 10 f of FIG. 9 could also be used in concert with any type of shaft-borne bearing, for example, in a pump, for enhancing the lubrication thereof. The structure for this type of device would be substantially the same as that depicted in FIG. 9 .
Design Theory
The cross-sectional area of the water flow channels in traditional cutlass bearings is relatively small. For example, the height of the water channels in cutlass bearings measured from the shaft surface is less than one-half inch for shafts up to 4 in. thick. Therefore, when propeller shafts become fouled with lines, ropes, or other material behind the cutlass bearing, the water flow through the bearing is quickly blocked. Without a steady flow of water, the bearing and shaft surfaces are starved for lubrication, causing overheating and premature wear in the bearing and shaft surfaces.
Conventional cutlass bearings depend only on the hydrodynamic force of the water flowing past them to provide water flow through the bearing. Many cutlass bearing housings have an inlet scoop designed on the forward end to promote positive water pressure on the forward side of the bearing. The amount of pressure developed at the forward end of the bearing is proportional to the speed of the water moving past the bearing. A slow-moving vessel, or one that is not moving, will therefore have much less water flowing through the bearing that would a vessel moving at high speed.
With the use of the instant invention several key improvements are realized.
1. The aft end of the bearing is shielded from external fouling by the placement of the impeller blades, which extend radially from the surface of the propeller shaft in the device. Restriction of water flow is therefore less likely and also direct wear damage to the bearing is less likely from fouling materials.
2. The use of the device prevents bearing damage from water starvation even with fouling around the shaft and/or the device. This because the effective discharge area for water coming through the bearing and out of the invented device is about 100 times greater than it is without the device.
3. The shaft-mounted impeller blades of the invented device cause centrifugal pumping action, which greatly increases the hydraulic force acting on the water that is fed through the cutlass bearing. That centrifugal force creates suction on the aft side of the bearing. The amount of hydraulic pressure imparted by the centrifugal action of the impeller blades is strictly dependent on shaft speed and not vessel speed. Therefore, the benefits of the invention for slower-moving vessels is even more significant.
4. The sharp edges of rotating impeller blades make a much more hostile environment for fouling material that winds around the shaft than are the relatively smooth surfaces of the shaft and bearing housings found in traditional propulsion systems without the present device. Therefore, fouling is ripped apart by the rotating blades and does not remain in place as long when the device of the present invention is mounted to the propulsion gear.
Finally, another potential advantage of the device is that the design of cutlass bearings can be improved because engineer-designers will have a new option of having forced water flow available instead of depending only on passive water flow as with conventional bearing designs.
In the foregoing description, certain terms have been used for brevity, clarity, and understanding, but no unnecessary limitations are to be implied therefrom beyond the requirements of the prior art, because such words are used for description purposes herein and are intended to be broadly construed. Moreover, the embodiments of the apparatus illustrated and described herein are by way of example, and the scope of the invention is not limited to the exact details of construction.
Having now described the invention, the construction, the operation and use of preferred embodiments thereof, and the advantageous new and useful results obtained thereby, the new and useful constructions, and reasonable mechanical equivalents thereof obvious to those skilled in the art, are set forth in the appended claims.
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A device that when fitted to a motor vessel's existing propulsion gear improves the performance and reduces potential damage and wear of underwater propeller shaft bearings, commonly referred to as “cutlass bearings” that are used on boats, ships, etc. Designed with radially mounted impeller blades around the periphery of the propeller shaft, the device creates a forced flow of water by centrifugal pumping action, which creates suction along the shaft abaft the cutlass bearing, thereby increasing the flow of water through the cutlass bearing. The device also greatly diminishes the probability that fouling around a propeller shaft will severely restrict water flow through the cutlass bearing.
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FIELD OF INVENTION
[0001] The invention relates to active food packaging whereby a low bioburden biodegradable and/or compostable absorbent nonwoven medium which does not support bacterial growth is employed in conjunction with at least one antimicrobial agent such as silver-based and/or silver ion-based active ingredients in the absorbent media or other packaging material. The food packaging material of the present invention functions to destroy microbes within the packaging environment and as they come into contact with the food packaging material thereby preserving food integrity while introducing mechanical protection to the food (e.g., fruit/produce) within the package by, e.g., reduction of bruising and physical damage. Active ingredients that are part of the food packaging of the present invention can function in the condensed phase and the biodegradable nonwoven pad incorporated in a package can function as a carrier and/or a release vehicle for one or more antimicrobial and/or antifungal chemicals or other actives.
BACKGROUND OF THE INVENTION
[0002] Active food packaging is a critically important area that provides the foundation for keeping packaged food fresh while reducing microbe load, inhibiting microbe growth and/or keeping the product substantially microbe-free so that the nutritional value of the food can be maintained and loss from spoilage minimized. Consequently, because of advances in food packaging technology, more people have access to fresh food. Food producers, packers and sellers can also provide a higher quality product while sustaining less economic loss due to product spoilage.
[0003] Active packaging, i.e., packaging that incorporates methods and/or compositions for the inhibition of microbial growth, covers many areas, but can be broadly defined in the art as the use of chemical or biochemical systems, including the use of antimicrobial and/or antifungal agents, that preserve the freshness and extend the shelf life of a food product by interacting with the food or the atmosphere surrounding the food either constantly or via controlled release. One prior art method of controlling the package atmosphere is the use of what is termed in the food packaging industry as Modified Atmosphere Packaging (MAP) where, generally, the relative concentrations of oxygen, carbon dioxide and nitrogen are adjusted relative to each other to preserve the integrity and freshness of the particular packaged item. A good review of Modified Atmosphere Packaging is provided in the art by Church and Parsons (Church, I. J. & Parsons, A. L.: (1995) Modified Atmosphere Packaging Technology: A Review , Journal Science Food Agriculture, 67, 143-152), as well as Beaudry (Beaudry, R., MAP as a Basis for Active Packaging, in Intelligent and Active Packaging for Fruits and Vegetables , C. L. Wilson, Ed. CRC Press, 2007. pp. 31-55).
[0004] The term “antimicrobial” with respect to food packaging is known in the art to include any composition and/or method to reduce or inhibit microbial growth (including bacteria and fungi) and, therefore, has wide breadth in the art. For example, as explained in López-Rubio (López-Rubio, A., et. al., (2004). Overview of Active Polymer - Based Packing Technologies for Food Applications . Food Rev. Int., 20(4): 357-87, p. 366), carbon dioxide often exerts a microbiological inhibitory effect in meats, cheeses and baked goods, but excess carbon dioxide may also adversely affect the taste or texture of the food product as well. Still, use of carbon dioxide is considered by those of skill in the art to be an antimicrobial agent. To the extent that there are gases like carbon dioxide, and others as detailed below, that provide an antimicrobial effect, we classify their use together in food packaging as a type of antimicrobial packaging. Exemplary representation of the current state of the food packaging art is provided below.
[0005] 1. Description of Related Art—Food Packaging Pads
[0006] In food packaging, an absorbent pad can be used for a variety of reasons, but is typically used to protect food articles from damage and to absorb moisture or biofluids that would otherwise compromise the freshness, integrity and appearance of the packaged food. Typically, a superabsorbent polymer, or SAP, is employed in granular or fiber form along with a nonwoven pad comprised of spunbond or meltblown synthetic fibers or paper pulp fibers, to absorb fluid. The pad typically can employ a film-based top and bottom layer with perforations that allow the fluid to reach the nonwoven absorbent layer but protect the food product from stray fibers.
[0007] U.S. Pat. No. 6,270,873, assigned to Sealed Air Corporation, teaches a food pad that comprises a top sheet and a bottom sheet with an absorbent nonwoven layer in between. According to the disclosure, the absorbent layer can be situated in the construction in a variety of ways. The top layer and bottom layer are sealed to confine the absorbent layer and microperforations are used in the various layers to allow fluid to permeate the sheet layers and reach the absorbent. However, such multilayer construction can be expensive and microperforations may become plugged by particulates. The patent does not have any teaching on biodegradable thermoplastic polymers and nor on the actual specific manufacturing process with regard to the involvement of antimicrobial and antifungal agents.
[0008] U.S. Pat. No. 7,732,036, assigned to Paper-Pak Industries, describes a shaped absorbent pad system whereby the pad system is sealed ultrasonically such that it prevents the pad from bursting due to fluid absorption, specifically with the usage of side panels and hinge connects. It also provides for multiple layers and also, among other features, allows that no perforations be used for fluid to flow into the absorbent pad. It also provides examples of using active agents to preserve packaged food freshness. However, this pad design is also relatively costly to manufacture and the envisioned active ingredients may not be optimal for longer term food preservation. Further, the pad design is not biodegradable and does not provide controlled release of an antimicrobial agent. And, finally, the pad system does not utilize biodegradable thermoplastic non-woven fibers that are specifically oriented and constructed to allow fluid absorption in manner that allows the adequate expansion of the pad.
[0009] U.S. Pat. No. 5,444,113, assigned to Ecopol, LLC, discloses products made of degradable materials that include a hydrolytically degradable polymer. Poly(lactic) acid is specifically mentioned, which is also called polylactide, which the authors further cite as a polydioxanedione. The authors list numerous forms of the biodegradable polymers such as laminates, foams, powders and adhesives, and they list ways to modify the polymers to enhance biodegradability. They specifically state that the materials in their invention degrade in a time period of a few months to a few years. However, they do not teach how antimicrobials may be incorporated into the degradable polymers of their disclosure nor how controlled release of the antimicrobial agent may be achieved. Further, they do not disclose how specific meltblown non-woven layer materials with enhanced mechanical and performance properties can be constructed and manufactured.
[0010] 2. Description of Related Art—Antimicrobial, Biocidal, Antifungal Food Packaging Aspects
[0011] U.S. Pat. No. 7,585,530, assigned to Paper-Pak Industries, discloses a multi-phase food pad absorbent system that absorbs fluids and inhibits bacterial growth by incorporating bacteriostatic and/or bactericidal ingredients and, optionally, the ability to modify the atmosphere inside the package, with other options that include reaction promoters in the food pad to maintain the integrity and safety of the packaged article. It is also important to note that in U.S. Pat. No. 7,585,530, no mention of biodegradability is made. U.S. Pat. No. 7,585,530 focuses on absorbency and the use of superabsorbent materials specifically in related to meat products within the context of using an organic acid bacterial inhibitor. U.S. Pat. No. 7,585,530 also discloses atmosphere modification within the package by CO 2 /O 2 modification, and discloses the use of enzymes to modify the atmosphere, specifically to reduce the oxygen content. Although this prior art claims antimicrobial materials in an absorbent medium, along with methods to modify the atmosphere inside the package, the art does not teach methods of controlled release of the antimicrobial agent(s) that would prolong the shelf life of the packaged food products.
[0012] U.S. Pat. No. 7,799,361, assigned to Paper-Pak Industries, similarly to U.S. Pat. No. 7,585,530, demonstrates an absorbent food pad constructed from tissue layers and is specifically related to absorbing liquid purge emanating from meat and poultry produce and using bacterial inhibitors to inhibit the growth of bacteria in the liquid purge itself. Also disclosed is a carbon dioxide generating system. There is no mention of the usage of antimicrobial agents in a controlled release manner and no discussion of a food pad that is biodegradable and no teaching of all aspects of the food pad non-woven construction including the calendaring of a non-woven biodegradable thermoplastic polymer.
SUMMARY OF THE INVENTION
[0013] The examples of the prior art provided above encompass packaging for both meat and produce. The advances in food packaging provided by the present invention, as detailed below, can apply to packaging for meat and produce and other foods, including, but not limited to, juices and liquids, amorphous solids and semi-solids, cheeses, seafood, and so on.
[0014] This invention utilizes, but is not limited to, antimicrobial action generated in situ upon contact of the pathogen with the antimicrobial agent, as opposed to conventional modified atmosphere packaging where the gaseous environment surrounding the packaged food product is altered during the packaging process, and changes due to respiration of the food product or other reactive chemistry. The in situ, contact-based action of the present invention can be controlled via reaction chemistry or a triggering event, such as contact with moisture, or it can be constantly released thereby providing antimicrobial and/or antifungal protection throughout the packaging life cycle. It is contemplated that the antimicrobial agent(s) is specifically integrated to the thermoplastic fibers and released when moisture (liquid or gaseous), humidity or free water content in the food package makes contact with the pad and pad fibers and/or during the biodegradation of the fibers.
[0015] The scope of this invention encompasses those aspects of food packaging that destroy or prevent microbial growth in and on a packaged product by the use of an antimicrobial agent. The antimicrobial agents of the present invention can function in the condensed phase, where condensed phase means a liquid or solid, or in a gaseous phase and said antimicrobial agents can be generated in situ via a chemical reaction, or used as-is, or released in a controlled fashion.
[0016] The invention also includes, but is not limited to, the antimicrobial chemistries described herein used in conjunction with biodegradable nonwoven fibers and non-biodegradable nonwoven fibers, the fibers having antimicrobial activity and/or very low bioburden. Such biodegradable and low bioburden fibers include those based on poly(lactic) acid, also known as polylactide, and its various L, D and meso configurations, including mixed L, D, and meso compositions, their various crystallinities, molecular weights, and various co-polymers. In this work poly(lactic) acid it is understood to be synonymous with poly(lactide) and both terms encompass all the optically active variations of the polymer. Other examples of antimicrobial, low bioburden polymers are known to those in the art as shown in a review by Kenway, et. al., (Kenway, E. R., Worley, S. D., Broughton, R. (2007), The chemistry and applications of antimicrobial polymers. A state-of-the-art review; Biomacromolecules, 8 vol, number 5 1359-1384).
[0017] The current invention advances the art of food packaging and active food packaging on two fronts. In an embodiment, the invention contemplates absorbent media which is specifically integrated to a biodegradable thermoplastic polymer non-woven layer concurrently with the creation of a unique apertured biodegradable thermoplastic polymer film. The nature, construction and advantages of said absorbent media, together with the biodegradable thermoplastic polymer, are unique and non-obvious. Second, the absorbent media is combined with silver and/or silver-based antimicrobial and/or antifungal chemistry in a specific fashion that allows for a long-lasting, robust and cost-effective antimicrobial action. Preferred embodiments of the antimicrobial and/or antifungal chemistry are novel in their own right, but the major advance is demonstrated in the concomitant use of both concepts: novel and non-obvious absorbent media architecture utilizing the biodegradable polymer with a surface to the food pad being apertured (i.e., porous or having porosity or having perforations or “pinpricks”) and/or non-apertured (i.e., non-porous or essentially non-porous, not having perforations or “pin pricks”; allowing no more than a trivial amount of liquid and or gas to pass though the film) in combination with the novel and non-obvious silver and/or silver-based antimicrobial and/or antifungal chemistry. The apertures of the present invention can be created through the calendaring process or created by other means known to those of skill in the art at the time of the invention. Even without apertures, the film may still have limited porosity much as fabric may allow limited amounts of liquid or gas to traverse the material.
[0018] Both aspects of this invention, the absorbent media and details of food preservation via controlled release silver and/or silver ion-based antimicrobial and/or antifungal chemistry should be understood in order to clearly delineate the advancement of the art.
[0019] A preferred antimicrobial agent is ionic silver, being released from a nonwoven pad made preferably from poly(lactic) acid fibers incorporating, in one aspect, absorbent media and superabsorbent media.
[0020] Examples of suitable silver and silver ion-based agents include, but are not limited to, silver halides, nitrates, nitrites, selenites, selenides, sulphites, sulphates, sulphadiazine, silver polysaccharides where such polysaccharides include simple sugars to polymeric and fibrous polysaccharides, silver zirconium complexes, forms including organic-silver complexes such as silver trapped in or by synthetic, natural or naturally-derived polymers, including cyclodextrins; all compounds, inorganic or organic, that contain silver as part of the structure, where such structures can exist as a gas, solid, or liquid, as intact salts, dissolved salts, dissociated species in protic or aprotic solvents and silver species which contain the molecular morphology or macroscopic properties of materials in contact with silver whereby such materials, either organic, inorganic, and/or of biological nature, are found in various morphologies, such as crystalline or amorphous forms, or optical activities, such as d, I or meso forms, or tacticities such as isotactic, atactic, or syndiotactic, or mixtures thereof of any of the above.
[0021] Silver ion-based agents include and are defined as, for example, compounds that contain silver as part of the structure that can be covalently bound, ionically bound, or bound by other mechanisms known as “charge-transfer” complexes, including clathrate compounds that involve silver or silver species as part of the structure. Silver ion-based agents also include silver or silver containing species that exist as a result of the process of sorption, either chemical or physical sorption, meaning absorption or adsorption, where the sorptive surface can be a molecule, polymer, organic or inorganic entity such as, but not limited to, synthetic oligomers or polymers (either thermoplastic or thermoforming), natural or naturally-derived polymers (either thermoplastic or thermoforming), biodegradable and non-biodegradable polymers (either thermoplastic or thermoforming), and inorganic or organic species whose surface area provides for some sorptive effect including, but not limited to, charcoal, zeolites of all chemical structures, silica, diatoms, and other high-surface area materials, also including silver or silver species in all its known valence states, either organically or inorganically bound, and includes organic or inorganic materials, either gas, liquid, or solid, where the silver or silver species can “exchange” or transfer by mechanisms such as, but not limited to, ion-exchange, diffusion, replacement, dissolution, and the like, including silver glass, silver zeolite, silver-acrlyic and nano-silver structures. Zeolite carrier based (the silver ions exchange with other positive ions (often sodium) from the moisture in the environment, effecting a release of silver “on demand” from the zeolite crystals) and glass based silver chemistries (soluble glass containing antimicrobial metal ions wherein with the presence of water or moisture, the glass will release the metal ions gradually to function as antimicrobial agents), are non-limiting examples of silver-ion-based agents suitable for use in the present invention.
[0022] Any combination of the above exemplary silver and silver ion-based agents is also contemplated for use in the food pads of the present invention.
[0023] In a preferred embodiment of the present invention, the antimicrobial and antifungal agents are incorporated into the actual fibers of the food pad. In this embodiment, the agents are added to the polymer prior to the formation of the polymer into fibers. In this embodiment, the agents are released as the fibers breakdown and thereby provide antimicrobial and antifungal affects to the package environment, including the food product, in which the food pad is placed. In this embodiment, the antimicrobial and antifungal agents are released, at least in great part, as the fibers in the non-woven pad degrade in the package environment. In another embodiment, the antimicrobial and antifungal agents are interspersed between the fibers of the food pad. In this embodiment, the agents are added to the fiber composition after the polymer is formed into fibers. In this embodiment, the antimicrobial and antifungal agents are released, at least in part, as the fibers in the non-woven pad degrade in the package environment. In yet another embodiment the antimicrobial and antifungal agents are both incorporated into the actual fibers and interspersed between the fibers.
[0024] In other embodiments, non-silver and non-silver ion-based antimicrobial and antifungal agents are contemplated for use with the food pads of the present invention. These non-silver and non-silver ion-based agents may be used in conjunction with the silver and silver ion-based agents of the present invention. One of ordinary skill in the art, based on the teachings of the present specification, can determine suitable combinations of agents depending on the fiber composition of the food pad, the size of the food package, the type of food being packaged, etc. Suitable non-silver and non-silver ion-based agents are, but are not limited to, compounds containing zinc, copper, titanium, magnesium, quaternary ammonium, silane (alkyltrialkoxysilanes) quaternary ammonium cadmium, mercury, biguanides, amines, glucoprotamine, chitosan, trichlocarban, triclosan (diphenyl ether (bis-phenyl) derivative known as either 2,4,4′-trichloro-2′ hydroxy dipenyl ether or 5-chloro-2-(2,4-dichloro phenoxyl)phenol), aldehydes, halogens, isothiazones, peroxo compounds, n-halamines, cyclodextrines, nanoparticles of noble metals and metal oxides, chloroxynol, tributyltins, triphenyltins, fluconazole, nystatin, amphotericin B, chlorhexidine, alkylated polethylenimine, lactoferrin, tetracycline, gatifloxacin, sodium hypophosphite monohydrate, sodium hypochlorite, phenolic, glutaraldehyde, hypochlorite, ortho-phthalaldehyde, peracetic acid, chlorhexidine gluconate, hexachlorophene, alcohols, iodophores, acetic acid, citric acid, lactic acid, allyl isothiocyanate, alkylresorcinols, pyrimethanil, potassium sorbate, pectin, nisin, lauric arginate, cumin oil, oregano oil, pimento oil, tartaric acid, thyme oil, garlic oil (composed of sulfur compounds such as allicin, diallyl disulfide and dyallyl trisulfide), grapefruit seed extract, ascorbic acid, sorbic acid, calcium compounds, phytoalexins, methylparaben, sodium benzoate, linalool, methyl chavicol, lysozyme, ethylenediamine tetracetic acid, pediocin, sodium lactate, phytic acid, benzoic anhydride, carvacrol, eugenol, geraniol, terpineol, thymol, imazalil, lauric acid, palmitoleic acid, phenolic compounds, propionic acid, sorbic acid anhydride, propylparaben, sorbic acid harpin-protein, ipradion, 1-methylcyclopropene, polygalacturonase, benzoic acid, hexanal, 1-hexanol, 2-hexen-1-ol, 6-nonenal, 3-nonen-2-one, methyl salicylate, sodium bicarbonate and potassium dioxide.
[0025] Thus, in an embodiment of the present invention, the invention comprises an absorbent, biodegradable food pad, comprising: at least one layer (i.e., a core) of non-woven fibers comprising one or more biodegradable thermoplastic polymers and one or more silver-based or silver ion-based antimicrobial agents. The silver-based or silver ion-based antimicrobial agents can be are incorporated into the non-woven fibers or interspersed between the non-woven fibers. The fibers of the food pad are, in an embodiment, oriented to provide compression resistance and maintain paths for liquid-flow and air-flow, preferentially in a direction transverse or essentially traverse to an exterior surface. See, for example, FIG. 11 . Further, the fibers of the present invention may be vertically lapped or spirally wound. “Vertically lapped” is defined herein as meaning that the ends of one set of fibers overlap vertically with the ends of another set of fibers, i.e., the fibers of the first set of fibers and the fibers of the second set of fibers are oriented substantially in the same direction and are overlapping to some degree. “Spirally wound” is defined herein as meaning that the fibers form substantially a helix.
[0026] In our current invention, although we can utilize synthetic fibers such as polypropylene and polyethylene, or paper such as recycled paper, we preferentially employ natural plant-based materials, such as natural polymers or naturally-derived meltblown nonwoven polymer fibers or filaments. One example is poly(lactic) acid (PLA), as defined above. The PLA is degradable and renewable, and has a low bioburden as opposed to, for example, recycled wood pulp. From an end-use standpoint and a processing and manufacturing standpoint, the low bioburden profile achieved with the nonwoven process precludes any heat drying that is required to destroy microbes present in a wood or tissue-based product; allowing a “cleaner” and safer system when compared to traditional alternatives such as wood pulp.
[0027] Another differentiating feature of PLA is that PLA is completely compostable, resorbable and safe in terms of cytotoxity, versus recycled pulp or synthetic fibers. One of the degradation products of poly(lactic) acid is lactic acid, which is produced in the human body.
[0028] Another feature differentiating the present invention from prior art technology is that most food pads are currently comprised of cellulose-based compositions as the absorbent medium, necessitating the use of a protective layer between the food and absorbent material. When a protective layer is needed to isolate the food from the pad a layer of thin PE film is generally used. This is glued onto the pad and a perimeter of film-to-film gluing is required to prevent edge leakage of fluid. Our selection of PLA (or other suitable thermoplastic fibers) eliminates the need for glue via the ability of thermoplastic materials ability to thermal bond and seal. This feature allows for more advantageous internal and perimeter bonding of the fibers compared to the current technique of pattern bonding or “stitching.” Stitching is a process wherein the pulp fibers are mechanically forced via a calendar roll to weakly interlock. The present invention of thermal bonding the poly(lactic) acid fibers provides more mechanical strength. In many applications, a “four-side sealed” pad is preferred as this prevents the absorbent contents from escaping. Current practice requires the interior pad, or core, be smaller than the overall pad to allow the upper and lower film layers direct contact for sealing. With the biodegradable thermoplastic core structure of the present invention, the entire pad, outer film layers plus core, can be thermally bonded, thereby allowing a streamlined and lower cost manufacturing process and added design capabilities as the pad can easily be fabricated in complex shapes to fit a complex tray or containment device. Another advantage of poly(lactic) acid food pads of the present invention over the prior art is the ability of the food pad to be thermal bonded directly to package trays and incorporated into three-dimensional structures, whereas most pads today are glued to a tray.
[0029] In another feature differentiating the present invention from the prior art, as compared to the limited prior art wherein poly(lactic) acid is employed as a food pad, is that the PLA of the present invention can be specifically engineered to be fully degradable as well as function in a dual-use as a carrier or active component in an antimicrobial and/or antifungal release system.
[0030] Another feature differentiating the present invention from the prior art is that in the present invention the method of meltblowing the PLA fibers into continuous filaments is novel and non-obvious and imparts unique characteristics to the food pad of the present invention. The unique characteristics allow, for example, for the incorporation multiple layers of fibers and filaments that serve specific functions including, but not limited to, three-dimensional pads, or molded or formed pad systems using pattern forming techniques. The multiple layering is also useful to provide specific absorbency without the need to perform separate lamination operations, as is typically done in the prior art. Separate lamination operations encompasses a sequence of discrete process steps wherein sheets and webs are created on separate forming stations or machines and then utilizing a bonding system, the individuals webs are thermally or adhesively or ultrasonically fused together.
[0031] In one embodiment of the present invention, the fibers form a non-woven core that forms the absorbent portion of the food pad. The core may be covered with a surface film as described and exemplified in detail below. The core, the core in combination with the film and/or the film may be present in multiplicities (i.e., pluralities)—in other words, there may be one or more layers of core and surface film in any order or combination as is necessary for suitable fluid retention, for protection and antimicrobial/antifungal action for the food product being packaged. The surface film may comprise, but is not limited to, a biodegradable thermoplastic polymer hydrophobic film is comprised from one or more of polylactic acid, polylactide, polyglycolide, poly-L-lactide, poly-DL-lactide or copolymers thereof.
[0032] In another embodiment of the present invention, the fibers of the core of the food pad are oriented to provide compression resistance and maintain paths for liquid-flow and air-flow. In one embodiment, the fibers are oriented in a direction substantially traverse to the exterior surface. In other words, when formed in to a non-woven sheet, the fibers run substantially parallel to the surface of the sheet.
[0033] The food pad of the present invention is capable of expanding up to 5, up to 10, up to 15, up to 20 and up to about 25 times of the original thickness when liquid is absorbed by the food pad. The expansion can be without the rupturing of any surface film or the sealed edges of any surface film that envelopes or encases the non-woven core(s) of the food pad.
[0034] The food pad of the present invention is capable of holding up to 5, up to 10, up to 20, up to 30, up to 40, up to 50, up to 60, up to 70, up to 80, up to 90 and up to about 100 times of the original weight of the food pad when liquid is absorbed by the food pad. The expansion can be without the rupturing of any surface film or the sealed edges of any surface film that envelopes the non-woven core(s) of the food pad.
[0035] In another embodiment of the present invention, the PLA fibers of the present invention can be used in combination with other fibers such as spunbond polypropylene or polyethylene, but the fibers used with the PLA fibers of the present invention are not limited to those two materials. For example, the PLA fiber or fibers can be employed as an outer surface of a multi-layer construction to provide a barrier against the food. Additionally, hydrophilic or hydrophobic layers in a single layer or multilayer construction are possible where either the PLA or the other polymer, or both, are treated with materials to render the nonwoven filaments hydrophilic or hydrophobic, depending on the end use and purpose. The hydrophilic and hydrophobic materials can be introduced in the fiber prior to extrusion via masterbatching or via a subsequent process such as coating, spraying or dipping. The introduction of hydrophilic and hydrophobic materials to the fibers is not limited to the techniques mentioned here but can be accomplished by any technique available to those of ordinary skill in the art.
[0036] PLA polymer is suitable at the 100% level in this application, however, with the inclusion of additives such as co-polymers, masterbatch additives and/or plasticizers, other additional advantages are observed. The term “additives,” as defined herein, are compounds that affect the manufacture and/or physical characteristic of the fibers and food pads of the present invention (i.e., also referred to as processing agents). As an example, when polycaprolactone, a degradable polymer often used in medical implants, is incorporated at up to 50% of the blend with PLA it imparts flexibility and softness to counteract the brittle nature of the PLA. Other additives function as plasticizers, lubricants and processing aids in the fiber spinning process. Examples of such methods and suitable agents are known to those of skill in the art as is shown by and outlined in, for example, “Processing and Mechanical characterization of plasticized Poly (lactide acid) films for food packaging V. P. Martino, R. A. Ruseckaite, A. Jiménez, Proceeding of the 8 th Polymers for Advanced Technologies International Symposium Budapest, Hungary, 13-16 Sep. 2005”, and “Poly(lactic acid): plasticization and properties of biodegradable multiphase systems Polymer, Volume 42 , Issue 14 , June 2001 , Pages 6209-6219, O Martin, L Avérous”, and “European Patent EP19990300874, assigned to KABUSHIKI KAISHA KOBE SEIKO SHO also known as Kobe Steel Ltd. (3-18, Wakinohama-cho 1 chome, Chuo-ku, Kobe, 651-0072, JP)” and “Study of Effects of Processing Aids on Properties of Poly(lactic acid)/Soy Protein Blends, Bo Liu, Long Jiang and Jinwen Zhang, Journal of Polymers and the Environment Volume 19, Number 1, 239-247.”
[0037] Suitable examples of plasticizers, lubricants and processing aids are CP-L01 from Polyvel (Hammonton, N.J.) which is a PLA plasticizer specifically targeted to improving the toughness, impact and processing capabilities of PLA. Another product by Polyvel is CT-L01, a lubricant, which improves slip characteristics while retaining other properties; it decreases PLA's high coefficient of friction and therefore reduces or eliminates adhesion between other film or metal surfaces during production. Additionally, Polyvel CT-L03 is a processing aid which raises intrinsic viscosity of PLA providing increased molecular weight and improved melt strength. Many other similar products are present in the commercial polymer additive and modifier marketplace.
[0038] In our invention the PLA can be thermally glazed (also known as “calendaring”). This is a distinct advantage over conventional food pad materials. Heat with calendaring and even exposure to blasts of hot air can render the nonwoven filaments with a smooth film-like surface, yet still have porosity to fluids and moisture. With regard to the present invention, the calendaring process and the effect it has on the surface of the non-woven thermoplastic core of the food pad of the present invention may be considered to be a surface film. Porosity can be controlled by controlling the heat used to calendar the material, and by the usage of an engraving roll that can place apertures on the film. Glazing can be an overall surface treatment or a variable/zone application. For purposes of visual comparison only, and not for comparison to mechanical or end-use properties, the smooth glazed PLA fibrous surface resembles in looks only the commercial product Tyvek®. The purpose of the fiber glazing (calendaring) process is to eliminate the need for a separate film, and it provides a unique and advantageous method to control fluid flow in the food package with a minimum of lamination and processing effort while increasing the utility of the food pad. Non-limiting examples of the range of porosity that can be achieved by the calendaring process of the present invention are shown in Tables 3 and 4a, below. One of ordinary skill in the art would be able, with guidance from the teachings of the present invention, to extrapolate times and temperatures necessary for a desired porosity.
[0039] In a further embodiment of the present invention, food pads can be constructed eliminating the need for glues and adhesive bonding by utilizing the calendaring process and, at the same time provide, if warranted, perforations (apertures) that allow the biological food fluids to flow into the absorbent core. The current art, in reference to a food pad with an absorbent core, may have perforations in the protective layer that is in contact with food. Such layers are typically polyethylene, but they are not limited to polyethylene. The present invention also provides for a construction whereby a protective film, typically polyethylene or polypropylene, but not limited to those materials, and in present invention successfully done with polylactic acid (e.g., comprised from one or more of polylactic acid, polylactide, polyglycolide, poly-L-lactide, poly-DL-lactide or copolymers thereof), can be thermally bonded to the PLA absorbent core, if desired. The present invention utilizes thermal bonding which can bond similar and dissimilar materials including but not limited to film to film, film to fiber and fiber to fiber, generally employing thermoplastic materials including, but not limited to, thermoplastic materials of natural, naturally-derived or synthetic origin, both organic and inorganic in nature, as exemplified elsewhere in this specification.
[0040] In a further embodiment of the present invention, construction of the food absorbent pad can incorporate superabsorbent technology. The usage of the one or more superabsorbent agents allows the food pad to absorb the free fluid (e.g., water, biofluids, etc.) that is frequently present in food packaging (e.g., fresh produce packaging) to improve the visual appearance of the food to the consumer. Superabsorbents are generally insoluble crosslinked polyacrylamide polymers in granular form that absorb water and fluid, but the field of superabsorbent polymers is not limited to polyacrylamide chemistry, as is known by those of ordinary skill in the art. Superabsorbents, abbreviated SAP, provide an economical means to increase fluid-holding capacity. U.S. Pat. Nos. 7,732,036 and 7,799,361 (both of which are incorporated herein by reference in their entirety) teach the use of SAP technology in a food pad. Further, SAPs are available commercially. However, conventional use of SAP's do not preclude the escape of the particles from the absorbent food pad area into the food package thereby allowing the SAP to possibly come in contact with the food.
[0041] In a further embodiment of the present invention, the SAP particles are secured to either the nonwoven pad or the previously described films that contact the food surface (e.g., on the inner surface of the films facing the absorbent pad). First, for example, SAP's can be delivered to the fibrous web and to positioned between layers. They can be held in place mechanically by the fibrous web. Second, for example, any granular SAP's used in the present invention can be secured between two layers of the fibrous web and thermal calendared so as to create a compressed and mechanically bonded pad. Third, for example, any granular SAP's used in the present invention can be secured with an aqueous polyacrylic acid solution polymer and an appropriate crosslinker. Such a polyacrylic acid solution polymer is described in U.S. Pat. No. 7,135,135 (incorporated herein by reference in its entirety), assigned to H.B. Fuller Licensing and Financing, Inc., under the trade name FULATEX PD8081H. The crosslinking agent can be an aqueous zirconium reagent or any other appropriate crosslinker described in the patent or known in the art. U.S. Pat. No. 7,135,135 further describes a spray-able material that is superabsorbent. The present invention may employ the FULATEX PD8081H as a means to secure granular superabsorbent powder dispersed in the nonwoven absorbent web, where the nonwoven preferentially comprises totally or partially a fibrous poly(lactic) acid filament. The present invention does not preclude the use of FULATEX PD8081H on other natural, naturally-derived or synthetic nonwoven materials or with other granular materials, especially, but not limited to, various antimicrobial and/or antifungal agents. Further, with regard to the present invention, FULATEX PD8081H can in itself be and function as part of a multi-component active ingredient release system (i.e., a controlled release system such as that taught by the present invention).
[0042] In a further embodiment of the present invention, antibacterial agents can be added into the polymer that is then meltspun into fibers. In other words, the antimicrobial agents are incorporated into the polymer fibers of the present invention. This provides protection and encapsulation of the antimicrobial agents and provides controlled release of the agents as the polymers of the present invention degrade as they are designed. Antibacterial, antimicrobial and antifungal agents can also be incorporated into the food packaging materials of the present invention in a variety of ways.
[0043] In an embodiment of the present invention, the antimicrobial action is incorporated into the polymer fiber structure of the present invention. There is no antimicrobial action imparted on (e.g., applied to) the food packaging (i.e., the food wrapping, barrier layer or film, clamshell or other outer wrap, for example) or the food itself. The presence of the antimicrobial agent(s) in the non-woven material prevents the food pad discoloring due to speckling caused by, for example, of the presence of mold. It also prohibits the spread of pathogens on the food pad itself, which would nominally acquire moisture during use (and hence, a possible location for pathogen propagation) in, for example, the fresh produce food packaging.
[0044] One improvement of the present invention over the related prior art is that the present invention integrates the antimicrobial compound as a masterbatch directly into the thermoplastic (e.g., polylactic acid) fibers as part of the meltblown fiber manufacturing process with specifically tuned process variables (as exemplified below) which results in the non-woven material used in the food pad core. Additionally, an improvement of the present invention is to be able to specifically calendar (as a function of speed, pressure and temperature) the polylactic acid polymer non-woven material with the antimicrobial formulation in order to allow it to function as a food pad insert or food pad film.
[0045] One novel and unique improvement of the present invention over the related prior art is the construction of the pad from polylactic acid in a novel fashion that allows multiple layers of non-woven polylactic acid fibers to manufactured with multiple layers of superabsorbent captured in those layers without the use of adhesive, by utilizing the calendaring process directly in the meltblown processing line for the multiple layers. This allows for manufacturing flexibility and optimization while ensuring the robustness of the non-woven material layer(s) in order it to function as a food pad insert.
[0046] Another improvement of the present invention over the related prior art is the construction of the pad from the polylactic acid with the integrated superabsorbent polymer in a unique fashion using the calendaring of the PLA non-woven materials such that it allows the pad to absorb up to 50 grams of water per 3″×3″ pad or up to approximately 7 gms per square inch (i.e., up to 100 times its dry weight) without rupturing and the PLA layers adequately stretching and keeping pad integrity intact. Thus, the food pad of the present invention has the unique property of absorbing and retaining high volumes of liquid thereby keeping the food product fresh. This novel advancement makes the functionality of the food pad to act as a food or fruit purge absorption pad possible.
DESCRIPTION OF THE FIGURES
[0047] FIG. 1 shows a schematic diagram of an embodiment of the production method of the present invention.
[0048] FIG. 2 shows a schematic diagram of an embodiment of the calendaring method of the present invention.
[0049] FIG. 3 shows a schematic diagram representing an embodiment of the food pad of the present invention.
[0050] FIG. 4 shows effectiveness of an embodiment of the food pad of the present invention with regard to bacterial kill.
[0051] FIG. 5 shows antimicrobial efficacy of the absorbent core of an embodiment of the food pad of the present invention.
[0052] FIG. 6 shows performance of the silver-ion treated apertured film of the present invention.
[0053] FIG. 7 shows E. coli CFU reduction as log count on an apertured film of the present invention.
[0054] FIG. 8 shows E. coli CFU reduction as percent on an apertured film of the present invention.
[0055] FIG. 9 shows effect of nozzle-size changes on the production of the polymer fiber of the present invention.
[0056] FIG. 10 shows a micrograph of the polymer fiber of the present invention.
[0057] FIG. 11 shows a magnified photograph of 0.015 inch fibers of the PLA insert in a cross-section of the non-woven pad construction with fiber direction being transverse to an exterior surface. FIG. 11 shows the pad insert orientation wherein the top surface is the horizontal surface on the photograph and the side of the insert is the vertical surface.
[0058] FIGS. 12 and 13 show the partially vertical surface is the side of the insert at higher magnification.
[0059] FIG. 14 shows a schematic representation of a layered configuration of two calendared non-woven food pad cores surrounded with outer layer surface films.
[0060] FIG. 15 shows a schematic of a second layered configuration of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0061] As used herein, the term “polymer” refers to thermoplastic, natural, naturally-derived, synthetic, biopolymers and oligomeric species thereof. As used herein, the term “oligomer” refers to a low molecular weight polymer of two or more repeating monomeric repeating units. Polymers specifically include, but are not limited to, PolyLactic Acid (PLA); PolyCaproLactone (PCL) and PolyHydroxyAlkanoate (PHA) alone or in blends/alloys or as copolymers.
[0062] Wherein the disclosed methods are given, these are only exemplary and one of skill in the art will understand that, based on the teachings provided herein, modifications of these procedures are within the metes and bounds of the present invention.
[0063] NatureWorks (Minnetonka, Minn.) produces several grades of PLA in pellet form that can be melt processed into film or fibers and are useful in this invention. Many grades are useful however grade 6202D as a high melt-point version with the optional use of grade 6251D as a low-melt binder fiber have proven to process well in the present invention. Perstorp (Toledo, Ohio) produces PCL and, although several grades are suitable for use in the present invention, grade Capa 6800 processes well. Mirel PHA from Metabolix (Cambridge, Mass.) is also compatible with the present invention.
[0064] When processing PLA, to maintain maximum chain length, it is important to dry the polymer is a commercial desiccant dryer such as a Conair (Cranberry Township, Pa.) “W” series machine to a moisture level below 200 ppm. This is critical as PLA polymer is extremely hydroscopic and will acquire moisture from the air rapidly. This moisture hydrolytically degrades the polymer chains resulting in a reduced viscosity and thus product strength. If moisture levels are too high, the additional problem of steam generation and uncontrolled pressures within the extrusion system are observed.
[0065] For exemplification, for production, a Davis-Standard (Pawcatuck, Conn.) single screw 30:1 2.5″ extruder (or equivalent) with melt temperatures of 350 to 425° F. and pressures of 500 to 2000 psi are achieved at the outlet. The polymer passes thru filtration to remove particulate debris and enters a pressure control zone achieved via a positive displacement Zenith (Monroe, N.C.) gear pump. Molten pressurized polymer is delivered to a melt-spinning die produced by BIAX (Greenville, Wis.). Several arrangements of nozzles, diameters, and total nozzle count can be varied to suit the polymer and final production needs. A typical spinning die contains 4000-8000 nozzles/meter of width with an internal diameter of 0.25-0.50 mm may be utilized efficiently. It must be noted that melt spinning dies produced by other suppliers such as Hills (W. Melbourne, Fla.) or Reifenhauser (Danvers, Mass.) may be used.
[0066] Heated and high velocity air is introduced into the die and both polymer and air streams are released in close proximity allowing the air to attenuate the polymer streams as they exit the die. Air temperatures of about 230-290° C. with pressures at the die at about 0.6 to about 4.0 atmospheres may be used. Following extrusion and attenuation, cool and/or moist air may be used to quench the fibers rapidly. At this point, liquids or mists can be applied to coat the surface. Surfactants, antimicrobials, fertilizers or adhesives can be beneficially adhered to the fibers.
[0067] The fibers may be collected on a single belt or drum or a multiple belt or drum collector. Air is drawn from below the belt(s) or drum(s) and fibers collect in a web or matt on the surface. There are many adjustments in the entire system, temperatures, pressures, quench conditions, extrusion air velocity, suction air velocity, etc. With these adjustment points, a matt that is, for example, stiff and thin or flexible and fluffy is possible. For this invention, a low-density structure with fine-diameter fibers is beneficial although one of skill in the art will realize that other densities and diameters are suitable for use in the present invention. The low density improves fluid acquisition and the small diameter maximizes surface area, which is important for the release of “actives” from the fibers.
[0068] Fiber diameters can range from approximately 1 to 30 microns (μm) however it is possible to produce nano or sub-micron fibers via increased hot air attenuation and/or low polymer throughputs. The cost of production increases as a result however the overall surface area of the fibers increases. Likewise, larger fibers are easily produced when attenuation air is reduced or eliminated and/or melt pressures are increased. A compromise of cost and performance is seen in, approximately, the 5-25 micron range. Within the large number of consecutive fibers being spun, it can be important to allow a range of diameters as this has been observed to increase the loft or thickness of the structure and this provides for improved shock absorbing and cushioning properties. Different diameters can be achieved by adjusting the internal nozzle diameters and/or air velocity at certain nozzles or by directing external cooling air toward certain fiber streams.
[0069] The invention described herein involves numerous embodiments around the production and use of biodegrable thermoplastic polymer fiber layers with super absorbent polymer (SAP) granules captured within the layers together with an antimicrobial, antifungal and biocidel agent in a food package that also provides for a natural or naturally-derived material, such as a nonwoven fibrous pad, where the agent is designed to prohibit, mitigate, prevent or inhibit microbe growth or kill microbes on the pad structure itself.
[0070] It is preferred to place “actives” in the polymer (as described and exemplified throughout the present specification) and, thus, in each fiber and/or interspersed between fibers. Traditionally, actives have been defined as chemical or physical agents that impart specific performance characteristics (as opposed to merely physical characteristics) to polymers. For example, it is current state of art to incorporate in to deodorant and cosmetic products actives using specialized pharmaceuticals and natural and botanical ingredients to provide odor control and wrinkle reduction for the user. For example, actives can be drug agents used for delivery of targeted therapeutics as outlined in “Polylactic acid as a biodegradable carrier for contraceptive steroids, Theodore M Jackanicz, Ph.D, et al., Contraception, Volume 8, Issue 3, September 1973, Pages 227-234.” In our invention, actives are defined, at least in part, as antimicrobial ingredients which mitigate and control the propagation of pathogen in and on the polymer fibers and in the food package environment. A good overview of antimicrobial actives for textile application can be seen in “Recent Advances in Antimicrobial Treatments of Textiles, Yuan Gao and Robin Cranston, Textile Research Journal 2008; 78; 60” or the use of antimicrobial actives as agents in polymers in “U.S. Pat. No. 5,906,825, Polymers containing antimicrobial agents and methods for making and using same,” both of which are indicative of what is known by one of ordinary skill in the art are incorporated herein by reference.
[0071] However, many materials will not tolerate the heat and pressure of extrusion. For example, halogens (iodine, chlorine, bromine) and chlorides (PVC) can release corrosive gas that can rapidly attack the machinery and require expensive alloys for protection; however, silver does not present these problems. As an alternative to a polymer-additive, after the polymer fibers are formed, the poly(lactic) acid can be treated by coating, immersion, spraying, printing or any other technique capable of transferring an ingredient or ingredients onto the fibers. The purpose of such treatment could be to promote release of the antimicrobial agent and could include, but is not limited to, water, lactic acid, lactide, organic and inorganic acids and bases, and catalysts.
[0072] If the product does not require the application of any absorbent or superabsorbent (SAP) granules or other powder “actives,” the web can proceed into winding and die cutting to final size/shape.
[0073] If granules are utilized (SAP, for example) a powder spreader is positioned to introduce powder directly into the path of the molten fibers as they are collected above a vacuum source. This vacuum source is a part of a flat belt collector, a dual drum collector or 3-D pocket former for the formation of dimensional and discrete parts. More than one spinning head can be utilized to allow the granules to be positioned generally in the center of the structure. It has been found that several mechanical arrangements are possible and that very high performing structures are possible with a fiber-supported interconnecting structure with SAP. Up to 85% SAP by weight has been tested with the present invention. The SAP can be calendared into/onto the non-woven fiber cores of the present invention.
EXEMPLIFICATION
Example 1
Creation of the PLA Non-Woven Food Pad Insert
[0074] Grade 6202D PLA polymer pellets from NatureWorks (Minnetonka, Minn.) were utilized from a fresh unopened bag and introduced into the mouth of a 2.5″ 30:1 40-hp extruder and exposed to mechanical shear and heat ranging from approximately 325 to 425° F. as it travels through the system. Filtration followed by a gear pump pushed the molten polymer thru a heated transfer line into a BIAX meltblown system at approximately 800 to 2000 psi. Compressed air was heated to approximately 475-525° F. and introduced into the die at approximately 10-18 psi and used to attenuate the PLA fibers thru nozzles with an internal diameter of about 0.012 inches. A filtered water mist quench was produced using a high-pressure piston pump and a fluid-misting system. This quench was operated at approximately 500-1800 psi and the mist impinges the fibers as they exit the die zone and serves to cool them. An air quench system introduced cool outside air to the fibers before they were deposited on a flat belt with a vacuum source below. The speed of this belt determined the weight of the web. For most food packaging applications a food pad insert from about 10 to about 80 grams per square meter (gsm) is required. The vacuum level additionally served to compress the web, or allow it to remain fluffy and at a low density. Calendar or thermal point bonding served to strengthen the food pad insert and impart strength. An alternative was to place a lightweight (about 14-about 20 gsm) spunbond nonwoven fabric under the web of fibers to impart strength. Once the food pad was calendared it was directed to a windup station for final packaging and assembly. Refer to FIG. 1 for a schematic view of the process.
[0075] Following collection on the belt, the web was wound into a roll and delivered to a roll wind up station. In some embodiments, depending on the requirements of the application, this web can be unwound from the station, and passed through a series of rollers and lamination stations, to get conjoined with an equivalent web, to yield a food pad with increased compressibility and mechanical characteristics. Such a web, either one layer or more layers, was cut to fit into clamshell or flexible pouch style containers.
[0076] As a reference for mechanical properties, the tensile strength of one 33 gsm PLA layer was measured to be 0.765 in/lbs using a Twing-Albert (West Berlin, N.J.) Tensile Tester using ASTM D5035 protocols (as is known to those of ordinary skill in the art). A 66 gsm PLA layer was measured to be 3.884 in/lbs using a Twing-Albert Tensile Tester using ASTM D5035 protocols.
Example 2
Inclusion of SAP in Fibrous Active Structure with Adhesive in PLA Food Pad Insert
[0077] In this example, superabsorbent polymer (SAP) was added (crosslinked polyacrylic acid grade Favor®Pac 530 from Emerging Technologies/Stockhausen (Greensboro, N.C.); approved by the FDA) as an indirect food additive. The SAP was granular and was dispensed uniformly via a powder spreader produced by Christy Machine Co. (Fremont, Ohio). The granules were dispersed directly into the fiber stream or simply between layers of fibers that have already been formed. It can be advantageous to utilize a pressure sensitive adhesive to construct a more robust structure and contain the SAP to prevent particles from dislodging and possibly contaminating the food. In this example an ITW Dynatec (Hendersonville, Tenn.) UFD fiber spray system was used to spray adhesive fibers between the meltblown webs and SAP granules followed by a nip roll to insure good contact with the adhesive. Many adhesives can be used including. In the present example HL 2110 from HB Fuller (St. Paul, Minn.) was used at an application rate of approximately 2-20 gsm. The meltblown/SAP structure then was laminated with exterior films and/or nonwovens as described in Example 1 and then processed into die cutting and used as an absorbent core.
[0078] Note that other absorbents can be used also including starch-based superabsorbents as offered by ADM (Decatur, Ill.; formerly Lysac), under several brand names and chemical configurations. An advantage of this brand is that is it made from a 100% natural raw material source which is synergistic with the natural polymers used to form fibers and structures of the present invention.
[0079] In terms of the water absorption data, please see Table 1, below. One can observe that the control paper (cellulose-based absorbent pad, similar to products manufactured by Dade Paper (Miami, Fla.), Buckeye Paper Mills (Canton, Ohio), Bartec Paper and Packaging (Cheshire, UK) and others) was saturated essentially by Day 3; however, the Modified (PLA, 2 layers of 33 gsm) pad (starting weight is 16.8 g average) kept on absorbing the excess water throughout the duration of the entire test
[0000]
TABLE 1
Day
Day
Day
Day
Day
Day
Day
Day
Day
Day
Day
Day
1
3
6
8
10
13
15
17
22
24
27
29
Control
11.0
12.0
12.0
12.0
12.5
12.0
12.0
12.0
14.0
13.0
14.0
14.5
pad (total
wet
weight,
grams)
Modified
22.5
22.0
24.5
27.0
27.5
31.0
28.0
31.5
34.5
32.5
pad (total
wet
weight,
grams)
Example 3
Inclusion of SAP in Fibrous Active Structure without Adhesive in PLA Food Pad Insert
[0080] We also utilized the dispersion and capture of the SAP between the layers of fibers by calendaring the two film layers. We used a BF Perkins (division of Standex Engraving, LLC, Sandston, Va.) Calendar Station which contained two heated rolls and two hydraulic rams. Each heated roll was filled with high temperature oil, which was heated by a separate machine. A hot oil machine controlled the temperature and the flow of oil through each zone of the Calendar Station. The temperature can range from 110 to 550° F. The hot oil was circulated at 30 psi through 2 inch iron pipes into a rotary valve for each zone.
[0081] The Calendar Station was opened and closed by a control station which also regulated the amount of pressure used to move the hydraulic rams. This pressure can range from 1 psi to 3,000 psi and maintained the amount of force with which the Drive Roll was supported. A variable spacer between the Sunday Roll (also called an Engraved Roll) and the Drive Roll maintained the distance of one roll to the other. The spacer allowed for the thickness of the PLA and the hydraulic rams maintain that distance. See, FIG. 2 for a schematic representation of the process. Non-limiting specifications are given below. One of ordinary skill in the art will be able to modify these specifications based on the guidance provided by this specification.
i. Top roll, labeled Sunday Roll, was an engraved roll; 7⅜″ diameter by 20″ length. ii. Bottom Roll, labeled Drive Roll, was a smooth roll; 10″ diameter by 19½″ length. iii. The temperature was variable on product density and speed of the process line. The speed can range, for example, from 1 to 200 FPM (feet per minute) with a temperature of 175 to 350° F. iv. The distance between the rolls was a variable controlling product thickness which can range from 0.5 to 0.001 inch.
Example 4
Creation of PLA Food Pad with Film and PLA Food Pad Insert
[0086] The PLA food pad insert was laminated to an olefin perforated or apertured film (the term “aperture” and “aperture film” and similar, refer to film having various degrees of porosity suitable for use with the present invention), 40-Hex pattern, from Tredegar (Richmond, Va.) and cut to a convenient size to fit into a 1-lb clamshell-style container designed for strawberries. The aperture film was placed upward against the food product and the pad/film structure provided mechanical cushioning and antimicrobial action. The silver in the PLA acted as a biocidal agent and slowed the growth of bacteria and fungi on the pad itself. See, FIG. 3 for a schematic representation of an embodiment of the food pad of the present invention.
Example 5
Creation of PLA Food Pad with PLA Film and PLA Food Pad Insert
[0087] The PLA food pad insert was laminated to a PLA perforated or apertured film created by uniquely calendaring the PLA fibers. The apertured film was placed upward against the food product and the pad/film structure provided mechanical cushioning and antimicrobial action. The silver in the PLA acted as a biocidal agent and slowed the growth of bacteria and fungi on the pad itself.
[0088] 1 GLP-1 and 2GLP-1 were sample identifiers for manufactured PLA food pad with PLA film. 1 GLP-1 was two layers of 50 gsm melt spun PLA integrated with a formulation of silver Zeolite grade AC-10D from AgION (Wakefield, Mass.; see, for example, U.S. Pat. No. 6,866,859, incorporated herein by reference), coupled with silver glass grade WPA from Marubeni/Ishizuka (Santa Clara, Calif.) with 30 gsm of SAP. 2GLP-1 was two layers of 33 gsm melt spun PLA integrated with a formulation of silver Zeolite grade AC-10D from AgION coupled with silver glass grade WPA from Marubeni/Ishizuka with 2 gsm of SAP, each were calendared to bond the SAP between the two layers of PLA melt spun. With regard to the edge sealing, the edges were heat sealed on all four edges of the pad/film structure. See, Table 2, below.
[0000]
TABLE 2
Line
Tensile
Speed
Temper-
Calendar
Strength
(feet per
ature
Gap
Thickness
ASTM
minute)
(° F.)
(inches)
(inches)
D5035
1GLP-1
20 FPM
240° F.
0.015
0.019″
10.724 in/lbs
W/O Edge
Sealing
1GLP-1 W/
20 FPM
240° F.
0.015
0.019″
10.470 in/lbs
Edge
Sealing
2GLP-1
120 FPM
280° F.
0.009
0.016″
3.684 in/lbs
W/O Edge
Sealing
2GLP-1 W/
120 FPM
280° F.
0.009
0.016″
3.808 in/lbs
Edge
Sealing
[0089] Different variations of PLA calendared film, inclusive of apertures, can be manufactured with different mechanical properties based on the teachings of the present specification. For example, PLA Film 1 was calendared 33 gsm PLA integrated with a formulation of silver Zeolite grade AC-10D from AgION coupled with silver glass grade WPA from Marubeni/Ishizuka at 240° F., 40 fpm, at 0.001 inch gap under 900 psi. PLA Film 2 was calendared 66 gsm melt spun PLA integrated with a formulation of silver Zeolite grade AC-10D from AgION coupled with silver glass grade WPA from Marubeni/Ishizuka at 280° F., at 10 fpm, at 0.005 inch gap, under 1,000 psi. Corresponding test data is shown below in Table 3.
[0000]
TABLE 3
If the corresponding PLA Film 1 and PLA Film 2 were
uncalendared, the data is as follows (which clearly
shows the effects of calendaring):
Permeation
Tensile Strength
Apparent
(ASTM E96)
(ASTM D5030)
elongation (%)
(g/hm 2 )
PLA Film 1
2.999 in/lbs
6.884%
80.2337
PLA Film 2
5.579 in/lbs
5.064%
67.7960
Permeation
Tensile Strength
Apparent
(ASTM E96)
(ASTM D5030)
elongation (%)
(g/hm 2
PLA Film 1 -
0.765 in/lbs
5.886%
67.4622
uncalendared
PLA Film 2 -
3.784 in/lbs
3.814%
64.9974
uncalendared
g/hm 2 = grams per hour times meter squared
[0090] As a reference for mechanical properties, the determination of permeation is conducted according to ASTM E96/E96M-10, Water Vapor Transmission of Materials Test methodology using permeation cups by BYK-Gardner (Columbia, Md.) and weigh scale by Mettler Toledo (Columbus, Ohio).
[0091] The size of the apertures for PLA Film 1 and PLA Film 2 were measured to be 0.022 inches in diameter. The apertures can be of a given shape (circular, diamond, etc.) as determined by the design of the engraved roll (Sunday roll).
[0092] Additional permeation characteristics can be designed with various constructions as exemplified in the Tables 4a and 4b below.
[0000]
TABLE 4a
Permeation
((ASTM E96)
Construction
(g/hm 2 )
Two layers of 50 gsm uncalendared PLA integrated
156.7750
with a formulation of silver Zeolite grade AC-10D
from AgION coupled with silver glass grade WPA
from Marubeni/Ishizuka with 50 gsm of SAP in
between the said PLA insert layers
Two layers of 50 gsm uncalendared PLA integrated
171.6458
with a formulation of silver Zeolite grade AC-10D
from AgION coupled with silver glass grade WPA
from Marubeni/Ishizuka without any SAP in between
the said PLA insert layers
Two layers of 66 gsm calendared PLA integrated
145.0521
with a formulation of silver Zeolite grade AC-10D
from AgION coupled with silver glass grade WPA
from Marubeni/Ishizuka with two layers of 50 gsm
calendared PLA insert which has 50 gsm of SAP in
between the PLA insert layers
Two layers of 66 gsm calendared PLA integrated
148.0729
with a formulation of silver Zeolite grade AC-10D
from AgION coupled with silver glass grade WPA
from Marubeni/Ishizuka with two layers of 50 gsm
calendared PLA insert which has no SAP in
between the PLA insert layers
Two layers of 66 gsm calendared PLA integrated
155.8896
with a formulation of silver Zeolite grade AC-10D
from AgION coupled with silver glass grade WPA
from Marubeni/Ishizuka with two layers of 33 gsm
calendared PLA insert which has 2 gsm of SAP in
between the PLA insert layers
Two layers of 66 gsm calendared PLA integrated
157.4042
with a formulation of silver Zeolite grade AC-10D
from AgION coupled with silver glass grade WPA
from Marubeni/Ishizuka with two layers of 33 gsm
calendared PLA insert which has no SAP in
between the PLA insert layers
[0093] Shown here are results wherein PLA calendared film was calendared to each other with or without heat sealing to create a stronger and/or more absorbent structure. Additionally, the PLA calendared films can be calendared to the PLA food insert pad and heat sealed. Below is a table (Table 4b) which demonstrates some of the combinations of structures and the corresponding mechanical properties of embodiments of the present invention.
[0000]
TABLE 4b
Tensile
Thickness
Strength
(in)
(in/lbs)
Two layers of Film1 without
0.006
6.379
insert sealed together.
Two layers of Film1 without
0.006
7.652
insert calendared together.
Two layers of Film2 without
0.018
8.276
insert sealed together.
Two layers of Film2 without
0.019
10.631
insert calendared together.
Two layers of Film1 and one
0.018
10.092
layer 1GLP-1 sealed together.
Two layers of Film1 and one
0.028
>11
layer 1GLP-1 calendared
together.
Two layers of Film2 and one
0.034
10.664
layer 1GLP-1 sealed together.
Two layers of Film2 and one
0.019
>11
layer 1GLP-1 calendared
together.
Two layers of Film1 and one
0.026
>11
layer 2GLP-1 sealed together.
Two layers of Film1 and one
0.019
>11
layer 2GLP-1 calendared
together.
Two layers of Film2 and one
0.042
>11
layer 2GLP-1 sealed together.
Two layers of Film2 and one
0.028
>11
layer 2GLP-1 calendared
together.
Example 6
Active Structure with Polymer Additives for Lubrication for PLA
[0094] This example is similar to Example 1, above, however a polymer additive or masterbatch in dry form was added into the PLA to impart lubricity. When added to the PLA at a 3.0% level higher volumetric throughput rate was observed (higher density; i.e., gsm attainment) while maintaining the same operating pressures, indicating a lower resistance to pumping. The higher volumetric throughput rate was observed by the increased rpm on the melt-pump and extruder motor. The melt additive used was CP-L01 from Polyvel Inc. (Hammonton, N.J.), a multipurpose plasticizer additive. When CT-L01 was substituted, also from Polyvel, at 3% level, lubricant or processing aid for “slip,” the same throughput rate at lower extruder and meltpump speeds was observed.
[0095] The data below (Table 5) shows the change in density (gsm) for different runs of PLA integrated with a formulation of silver Zeolite grade AC-10D from AgION coupled with silver glass grade WPA from Marubeni/Ishizuka with different process settings and with different levels of additives.
[0000]
TABLE 5
Density, extruder speed (rpm)
and meltpump speed (rpm)
PLA non-woven
63 gsm, Extruder RPM 12%,
food pad insert
Melt Pump RPM 19%
97% PLA with 3% CP-L01
65 gsm, Extruder RPM 13.5%,
food pad insert
Melt Pump RPM 21%
97% PLA with 3% CT-L01
55 gsm, Extruder RPM 11%,
food pad insert
Melt Pump RPM 18%
94% PLA with 3% CP-L01 and
63 gsm, Extruder RPM 11%,
3% CT-L01 food pad insert
Melt Pump RPM 18%
[0096] Similar results (not shown) as above were obtained with polypropylene based on the guidance provided by the present specification for those of ordinary skill in the art.
Example 7
Active Structure with Topical Hydrophilic Treatment Added for PLA
[0097] This is similar to Example 1 except the hydrophilic additive was in liquid form mixed into the water quench system and sprayed directly on the fibers while hot. Many surfactants are candidates; however polyethylene glycol (PEG) 200-900 mw is preferred. The concentration used was based on the weight of the fibers strayed and a range of 0.05% to 2.0% has proved beneficial in promoting rapid fiber wet-out. Additionally, the resultant fibrous web demonstrates a more rapid fluid acquisition speed was observed. This enhanced hydrophilicity was advantageous when an absorbent article with rapid fluid uptake was desired. The liquid additive used was Lurol PP-2213 from Goulston Technologies, Inc. (Monroe, N.C.), which is marketed as a single-use surface hydrophilic agent into the hygiene and diaper industry. The results were dramatic as almost immediate wet-out occurs. A similar product also useful in the present invention, Lurol PS-9725-NAD from Goulston, provides immediate wet-out also and is marketed as offering semi-durable performance. Another product, Triton X-100 (Dow Chemical, Midland, Mich.) was also tried successfully. It was applied to a 3×3 inch, 33 gsm PLA food insert pad comprising a formulation of silver Zeolite grade AC-10D from AgION coupled with silver glass grade WPA from Marubeni/Ishizuka, with a water mixture, at 1% and 0.5%. Each sample was fully submerged into a volume of water and then weighed with these results (Table 6).
[0000]
TABLE 6
Dry Weight (g)
Wet Weight (g)
0% Triton X-100
0.19
0.45
0.5% Triton X-100
0.19
1.66
1% Triton X-100
0.19
1.72
[0098] Repeated insult performance is important in food packaging applications, especially for pallet shipments and shipping case quantities where fluid levels may vary. The above samples were re-tested for repeated insult performance by saturating and drying each sample five times to determine if the hydrophilic properties were consistent after multiple uses. The positive results are presented below (Table 7).
[0000]
TABLE 7
Dry Weight after 5
Wet Weight after 5
insults (g)
insults (g)
0% Triton X-100
0.19
0.75
0.5% Triton X-100
0.19
1.86
1% Triton X-100
0.19
1.93
[0099] Similar results as above were obtained with polypropylene based on the guidance provided by the present specification for those of ordinary skill in the art.
[0100] A 33 gsm polypropylene material was created with 3% TMP12713, a modifier manufactured by Techmere (Clinton, Tenn.); a 3″ by 3″ sample was cut and submerged into a volume of water and then weighed. The sample was re-tested, saturated and dried multiple times with these results (Table 8):
[0000]
TABLE 8
Dry Weight (g)
Wet Weight (g)
1 st insult
0.19
1.85
5 th insult
0.19
1.94
Example 8
Active Structure with Nonwoven Support Structure Added
[0101] This example is similar to Example 1 except a supporting nonwoven pad was positioned above the vacuum conveyor and below the matt of fibers being extruded. This additional layer provided additional strength to the very weak web of fibers allowing the formation of the web to be very loose, fluffy and low density. A low-density web offers greater impact and cushion protection for food, thus lower bruising and spoilage related to bruising. Many suitable spunbond webs are suitable for use in the present invention in view of the teaching provided in the present specification (e.g., PP, PET or PLA polymers with hydrophilic or hydrophobic finishes). For this trial, a 15-gsm SMS web (spunbond/meltblown/spunbond) from BBA Nonwovens (Simpsonville, S.C.) was selected. This is a commodity product used in infant disposable diapers and has a hydrophilic finish with FDA food approval. It is very strong and uniform of its lightweight and does not hinder the formation of a meltblown web on its surface when included in the meltblown process. Depending on the application it can be removed before the finished final product is assembled.
Example 9
Active Structure with Ionic Silver Controlled-Release Antimicrobial Feature
[0102] This example is similar to Exhibit 1 except a custom masterbatch containing a slow-release silver ion compound was incorporated to provide broad antimicrobial and antifungal performance. Several silver-releasing materials have been evaluated including, silver Zeolite grade AC-10D from AgION, silver glass grade WPA from Marubeni/Ishizuka, silver zirconium, Alphasan from Milliken (Spartanburg, S.C.). In each case, a 20-30% loading in a carrier polymer was prepared and used to uniformly deliver the silver additive into the mix. One preferred silver agent was the silver zeolite grade AC-10D from AgION which also contained copper elements as an anti-fungal agent. Another preferred silver was the WPA silver glass powder from Marubeni/Ishizuka. Particle size of less-than 5 microns was specified with an average of 2-3 microns to preclude spinneret nozzle clogging. The final concentration of silver in the meltblown fibers was dependent on the quantity of masterbatch used. In trials, up to 20% masterbatch has been processed to demonstrate an extreme loading, up to 5% silver by weight. For the performance required of food packaging, we have found 20 to 1000 ppm loading of actual silver, as a portion of the silver-based additive use with the pad, to be effective. In a food packaging application silver was highly effective as its slow release and long-term bacterial control properties match the end-use requirements. The silver was be placed in a masterbatch with PLA, or an olefin carrier. For PLA fibers, the PLA carrier is preferred to maintain the degradability performance.
[0103] To determine the efficacy of antimicrobial formulation, product 3GLP-1 was tested. 3GLP-1 was two layers of about 33 gsm melt spun PLA food pad insert with about 20 gsm of SAP, with the SAP captured between the two layers of PLA with adhesive (as in Example 2) and topical treatment (as in Example 7), and hex-40 film comprising the other film layer (as in Example 4) utilizing the nonwoven support structure (as in Example 8) which was removed prior to the heat sealing of the edges.
[0104] 26 boxes of lettuce were shipped overnight from California, received in Biovation (Boothbay, Me.) facilities. 13 boxes were “Control” (existing bag packaging in the box, cellulose paper between layers of lettuce and at bottom of package) and 13 were “Modified” (existing bag packaging with Biovation's 3GLP-1 pad at bottom of package, with SAP manufacturing as in Example 2, and the antimicrobial formulation of Example 9). One box (all boxes were stored in 3° C. walk-in cooler) of each type was opened on every testing day (Mondays, Wednesdays and Fridays, starting with a Wednesday). The packaging materials were tested for aerobic bacteria. Also packaging materials were inoculated with E. coli for an antimicrobial challenge test.
[0105] When nutrients are present and temp/humidity conditions are acceptable;
[0106] bacteria will rapidly populate to a level of 10 6 to 10 8 cfu/gram. Generally, it is considered that a level of 10 5 indicates spoilage. Fresh produce with moisture and an environment conducive to growth certainly will support bacterial growth. Many bacteria are “safe” and although the produce may become slimy, there is no health risk and many bacteria are considered as “probiotic.” The risks increase with certain strains including, but not limited to, E. coli, Listeria and/or Salmonella.
[0107] In a natural environment, a broad range of organisms thrive and constantly compete for available resources; nutrients, moisture, etc. It is unusual for one organism to dominate the others and even if this occurs, the lives of bacterial organisms is so short, the dominant situation rapidly reverts back to a complex bacterial flora, all in competition for resources. Many bacteria reproduce on a 20-min cycle which leads to an explosive logarithmic growth phase. This phase ends when nutrients are limited or toxins develop from dead bacteria.
[0108] Aside from testing to determine the type of bacteria present, basic microbiological testing is often conducted to determine population counts and population reduction ability of the packaging or processing technique. Microbiological testing of food products is well established and many protocols are available to those of ordinary skill in the art, especially for antimicrobial and “active” materials.
[0109] Bacterial populations (colony forming units, cfu) were determined with standard methods. When required, recovered samples were incubated at 37° F. for 24-hrs. Serial dilution, each step was 1-log, were conducted using Butterfield's solution as the diluent. One ml samples were taken using an electronic pipette and non-selective 3M #4604 Aerobic Bacteria Petrifilm™ plates (3M, St. Paul, Minn.). Following a 36-48-hr incubated growth phase, manual readings of the plates were taken and recorded. Populations of bacteria were recorded as CFU/ml of fluid. Bacterial count tests were also performed using 3M #6417 plates with 5-day incubation periods. Duplicate testing was performed for added accuracy. The two readings were averaged for reporting.
[0110] As can be seen in FIG. 4 , high levels of aerobic bacterial activity in Day 15 and Day 29 were observed for the Control Paper. The materials of the present invention did not indicate the presence of any aerobic bacterial colonies. This was expected as the materials were formulated with Biovation's FDA approved food grade antimicrobial and antifungal agent(s). The agent used in the Example performed as expected and prevented the growth of bacteria. Note the low bacterial counts on the “Modified” material on Day-1. The antimicrobial used in the present invention is a long-duration type antimicrobial agent with a safe but slow activation period. This system generally takes 24-hrs to show strong performance.
[0111] For the antimicrobial challenge test sample sizes were generally 2 inch square or 1″×4″ rectangular. For thin materials, like the “control” cellulose paper, a flat test method using a sterile cover sheet was found to be suitable. This test was essentially the same as the JIS Z 2801 protocol, also known as ISO 22196, a global standard. The absorbent pad was tested with a widely accepted textile standard AATCC-100 which determines antimicrobial effectiveness in fibrous materials. It was also acceptable (equivalent) to use a spray technique to deliver a uniform level of bacteria as compared to flooding the sample, as with AATCC-100. Everything else remained equivalent the only difference being that the bacteria were delivered differently.
[0112] Pure certified strains of bacteria were purchase from ATCC and were received lyophilized or freeze dried. For this study we selected E. coli because it is an organism of most concern for the produce industry. E. coli #8739 is routinely used in antimicrobial testing and all labs carry it. It is considered as BioHazard Level 2 organisms and is regulated and requires moderately advanced lab conditions and safety procedures. Biovation performed these tests internally in their facility.
[0113] The bacteria were maintained in a liquid sample that allowed it to grow. To be able to count the population, the concentration of bacteria was diluted as levels of 1,000,000 colonies and higher per ml were very common in the experiments described here. Highly accurate electronic pipettes and premeasured dilution bottles were used. Serial dilutions of 9:1 were performed. The petri film, plate or dishes were read following 48-hrs of incubation. The technician visually determined which plates could be read and calculated the concentration after considering the dilution factor.
[0000] Test protocols that were followed herein are outlined below:
Grow a pure strain of the organism of choice in nutrient broth or agar. Most organisms will grow to a population density of 10 6 to 10 8 cfu/gram; CFU=colony forming units. Adjust the population density to a known value so a “starting point” is determined. Introduce or inoculate a small quantity of the test bacteria on the product to be tested. A food source is provided along with ideal growing conditions in an incubator. Note that actual “real life” conditions can also be utilized, such as chilled temperatures or temperature cycling. Place a known quantity of bacteria and fluid on a known sample size of the pad or film. Generally duplicate or triplicate samples are used for accuracy. Allow the inoculated bacteria to grow (or be killed by the “active”) over a fixed period, generally 18-hrs to 48-hrs. A negative control is included in the testing as this establishes the baseline for comparison. Following the incubation phase in which the food or packaging material is exposed to the bacteria, extract the bacteria for population determination. This extraction can be via simple fluid collection if a film or pad surface is involved. Vortexing or can be used to assist in collection. The goal is to recover remaining live bacteria for counting. Immediately following this collection step, the “active” or antimicrobial must be neutralized to prevent further activity. A neutralizer solution is used, one specific to the antimicrobial used (e.g., BD Diagnostic Systems, Dey/Engley D/E Neutralizing Broth). Care must be taken to not harm the bacteria or slow their growth while stopping the antimicrobial activity and a “neutralization verification” protocol is run to determine this. Following neutralization, the population of remaining bacteria is counted. This is done visually on agar plates or films. The agar is chosen to provide a suitable growth media for the organism used. A wide variety of suitable agars and nutrient plates are available commercially. Because cfu, or colony forming units, are counted the concentration must be adjusted to provide a density that can be accurately counted. Too high and a lawn of bacteria is observed and cannot be counted. A known quantity of fluid containing the neutralized and recovered bacteria is in placed on the agar plates and diluted in serial steps, each step being 1-log or 10× population reduction. Generally 5 or 6 dilution steps are required. These agar plates, each with a known dilution, are placed into an incubator to provide ideal growth conditions, generally for 48-hrs. Visually look at the plates and determine which dilution step has a “countable” number of cfu's. Count the bacteria and determine the population density of live bacteria. Also count the “control” sample. The performance of the “active” or antimicrobial packaging is determined by the population reduction of cfu's or log reduction reported in percent reduction.
[0126] Refer to Table 9, below, and FIG. 5 . From the starting point, the untreated samples (which can also be considered equivalent to the Control paper) allowed dramatic microbial growth while the treated sample reduced the population dramatically.
[0000]
TABLE 9
Population
Reduction (%)
Log Reduction
Treated vs. Startin Pop
99.44086%
3.083E+04
Treated vs. Control
99.99996%
3.933E+08
[0127] These data indicate an unexpectedly strong performance as a contact antimicrobial for the 3GLP-1 test sample. Bacteria absorbed into the core were effectively killed; a 4-log kill (99.99996%) kill rate is considered by those of skill in the art to be the required and effective range of industrial performance benchmarking.
[0128] Finally, a detailed visual inspection was carried out on 3GLP-1 and there was absolutely no discoloration or speckling (which was present on the control cellulose paper), demonstrating the positive benefits of the antimicrobial agents in the non-woven material.
Example 10
Active Structure Made with Polypropylene Polymer
[0129] This is similar to all above examples with the exception of polypropylene polymer (PP) is substituted for the PLA. The advantage of PP is a higher processing and throughput speed. PP has all the required health and safety and low-bioburden properties food packaging require. It is also receptive to hydrophilic additives in a masterbatch or surface treatment to impart rapid fluid wet-out. Additives can easily be included in masterbatch form. A PP meltblown web can also be thermally point bonded or placed on a spunbond carrier for additional strength and can be processed in a secondary treatment step to impart an silver-containing treatment.
[0130] In this example we used ExxonMobil (Houston, Tex.) Achieve 6936G ultra-high melt flow rate polypropylene at the 100% level and with additives. One distinct advantage was lower melt processing conditions when compared to PLA. Extruder and spinning temperatures in the 275 to 350° F. range were sufficient and this product and this allowed polymer additives that were heat-intolerant to be utilized.
[0131] The below table (Table 10) shows the particulars of a 3GLP-1 all PP sample manufactured on the meltblown line. 3GLP-1 consists of two 50 gsm PP melt spun layers and 25 gsm of SAP, calendared to bond the SAP between the two layers of PP.
[0000]
TABLE 10
Tensile
Strength
Line
Calendar
(ASTM
Speed
Temperature
Gap
Thickness
D5035)
3GLP-1
10 FPM
250 F.
0.005
0.019
5.65
W/O Edge
Sealing
3GLP-1 W/
10 FPM
250 F.
0.005
0.019
3.951
Edge
Sealing
[0132] Melt spun PP of various densities and thicknesses were calendared at a close nip under high pressure to produce a film structure. See test data below (Table 11) to see the various structures created and the performance difference between “calendared” and “uncalendared.”
[0133] The 33 gsm melt spun PP was calendared at 210° F., at 10 fpm (feet per minute), at 0.001″ gap, under 1000 psi, to create “PP Film 1”.
[0000]
TABLE 11
Tensile Strength
(ASTM D5035)
Apparent Elongation
PP Film 1 - Un-Calendared
1.253 in/lbs
29.302%
PP Film 1 - Calendared
2.294 in/lbs
15.78%
[0134] A 48 gsm melt spun PP was calendared at 250 F, at 10 fpm, at 0.005″ gap, under 1,000 psi, to create “PP Film 2,” see, Table 12.
[0000]
TABLE 12
Tensile Strength
(ASTM D5035)
Apparent Elongation
PP Film 2 - Un-Calendared
1.788 in/lbs
23.398%
PP Film 2 - Calendared
3.789 in/lbs
8.475%
Example 11
Creation of a PP Food Pad with PP Food Pad Insert with PLA Fill
[0135] Similar to Example 5, a polypropylene food pad can be constructed with polypropylene food pad inserts as demonstrated in Example 11, with PLA film on the top and bottom outer layers. The polypropylene food pad inserts can be calendared, or uncalendared, wherein the PLA film can be of the calendared type also described in Example 5. The PLA film would be heat sealed on all four edges with the PP food pad insert captured in the center of the total substrate.
Example 12
Creation of a PLA Food Pad with PLA Food Pad Insert with PP Film
[0136] Similar to Example 5, a PLA food pad can be constructed with PLA food pad inserts as mentioned in Example 1, 2, 3, 4 and 5, with PP film on the top and bottom outer layers. The polypropylene film would be calendared with the hydrophilic additive as mentioned in Example 7. The PP film would be heat sealed on all four edges with the PLA food pad insert captured in the center of the total substrate.
Example 13
Active Structure Made with Polycaprolactone Polymer
[0137] This is similar to Example 1, above, with the exception that Polycaprolactone (PCL) is added to the PLA in a blend at various levels from 5% to over 70%. PCL is a naturally derived polymer with a very low melt point. When used at low levels, generally 30% and lower, it functions as a plasticizer for the PLA, a brittle polymer, and imparts lubricity and softness to the fibers that functions to reduce breakage. This dramatic improvement was apparent even at a 2% add-on level and increases with concentration. The PLA/PCL blend incorporated masterbatch additives or surface finishes to modify the hydrophilicity and fluid wet-out speed. Silver was also incorporated. The lower processing temperature of the PCL allows the use of low-temp additives but also limits the effective storage and use temperatures of the finished product.
[0138] Below, Tables 13 and 14 show the physical property of various PLA/PCL structures that were manufactured with different mechanical properties. For example, PLA/PCL Structure UC-1 was non-calendared 600 gsm 93% PLA with 3% CP-L01 and 3% CT-L01 and 1% PCL run at 400 F, 3 fpm and 1100 psi. Corresponding test data is shown below for various combinations and permutations wherein the speed, pressure and temperature were changed.
[0000] TABLE 13 Tensile Strength Apparent (ASTM elongation Break Time D5035) (%) (sec) PLA/PCL Structure UC1 0.732 28.996 4.375 PLA/PCL Structure UC2 0.937 14.131 2.141 PLA/PCL Structure UC3 1.109 16.356 2.547 PLA/PCL Structure UC4 1.837 12.024 1.843 PLA/PCL Structure UC5 1.731 21.465 3.313 PLA/PCL Structure UC6 1.347 22.304 3.391 PLA/PCL Structure UC7 1.840 23.915 3.609 PLA/PCL Structure UC8 1.360 10.460 1.594 PLA/PCL Structure UC9 1.375 18.804 2.844 PLA/PCL Structure UC10 1.767 17.139 2.734 PLA/PCL Structure UC11 1.730 25.954 4.000 PLA/PCL Structure UC12 1.316 21.022 3.250 PLA/PCL Structure UC13 0.797 22.914 3.469 PLA/PCL Structure UC14 1.176 15.248 2.312 PLA/PCL Structure UC15 0.755 27.581 4.157 PLA/PCL Structure UC16 0.851 19.247 2.906 PLA/PCL Structure UC17 1.205 20.022 3.094 PLA/PCL Structure UC18 1.118 23.247 3.562
The mean is 1.277 lbs for tensile strength, 20.046% for apparent elongation and 3.063 sec for break time.
[0000] TABLE14 By calendaring various samples, the following data was obtained: Tensile Strength Apparent (ASTM elongation Break Time D5035) (%) (sec) PLA/PCL Structure 1 1.957 18.478 2.797 PLA/PCL Structure 2 1.636 15.690 2.468 PLA/PCL Structure 3 1.702 16.475 2.500 PLA/PCL Structure 4 1.621 14.251 2.157 PLA/PCL Structure 5 1.357 12.808 1.937 PLA/PCL Structure 6 2.032 12.911 1.953 PLA/PCL Structure 7 1.117 23.799 3.593 PLA/PCL Structure 8 1.481 10.696 1.704 PLA/PCL Structure 9 2.268 19.359 3.000 PLA/PCL Structure 10 2.221 17.755 2.750 PLA/PCL Structure 11 2.185 22.342 3.375
The mean is 1.780 lbs for tensile strength, 16.779% for apparent elongation and 2.567 sec for break time
Example 14
Apertured Film and/or Structure with “Actives” and Coloration
[0139] This is identical to Example 4 and 5 except the apertured film was pigmented to match the color of the food or berry or the exudate of the food. The color of the film can also be white or another contrasting color to enhance the visual appearance of the package. This was simply to present a pleasing consumer package. The final construction of the absorbent pad utilized film on two sides, top and bottom.
[0140] In a similar design, one or both of the films was spunbond or SMS layered on the calender bonded surface of the PLA or PP fibers themselves. There are many options. In this example, two layers of white pigmented 40-Hex Tredegar apertured film, including 5% masterbatch with WPA silver glass antimicrobial, were utilized and the edges were thermally sealed with heat/pressure. This film offers a one-way flow feature and the flow is inward, into the absorbent pad.
[0141] The testing conditions and protocol denoted in detail in Example 7 was also used to test the performance of the film (which though is 40-hex Tredegar film in the test, can be manufactured from PLA as mentioned in Example 5).
[0142] We measured the bacterial count translated to 449,460,000 (4.5×10 8 ) total colonies per box, on average. This was a large number but there is a very large surface area of lettuce and the concentrate per leaf is really quite low. The risk however, was the potential for explosive growth with a strain that is pathogenic and can cause illness, or death. With certain bacteria, it can reportedly (and is known to those of ordinary skill in the art) take as few as 100 colonies to cause illness in humans.
[0143] With this as a starting point, we made several assumptions.
1. That the 500 g of lettuce sampled from the top layer is representative of the entire box. 2. That a “worst case” is for 100% of those bacterial colonies to become exposed to the packaging materials. 3. That the E. coli strain selected, ATCC #8739, is representative of bacterial contamination found on the lettuce leaves. 4. That the distribution of colonies is uniform and not highly concentrated.
[0148] A known number of colonies and a certain area were used in the “treated” materials with which to control these colonies; 0.495 square meters of film with all layers combined, and, 0.090 square meters of pad surface. It is unlikely that the vast majority of these bacteria will never contact the packaging materials; however, if all did, that would become a “worst case” scenario.
[0149] In the lettuce box, the absorbent pad was observed to increase in weight as it picked up free moisture. Experience gained in other food packaging investigations using chicken, beef and fish indicates that in food packaging, this free fluid is often laden with bacteria. This leads to the last assumption.
5. That 80% of the bacteria are mobile in the free fluid and this fluid ends up being contained in the absorbent pad and 20% are exposed to the apertured film layers.
[0151] With these assumptions it was concluded that to simulate the “worst case” bacterial exposure, the apertured film surface should be inoculated with 1.81×10 8 colonies per square meter. The test protocol was carefully calibrated to deliver these levels.
[0152] To expand this range and gain a better understanding of the performance of these materials, several other concentrations were used in addition, both higher and lower concentrations.
[0000]
TABLE15
Target Loading On the Film
Level
(CFU/sq meter)
Plus 1-log
1.81 × 10 9
Target Bacterial Exposure
1.81 × 10 8
Minus 1-log
1.81 × 10 7
Minus 2-log
1.81 × 10 6
Minus 3-log
1.81 × 10 5
[0153] Please recognize that this was a unique customized protocol in which a challenge test was performed by loading or inoculating materials with a carefully controlled bacterial loading of different concentrations.
[0154] Controlled atomization was used for the apertured film and a traditional direct fluid inoculation was used for the absorbent pad. All materials were provided with additional moisture in the form of a sterile buffered misting. All samples were of a known size for ease of calculation. This size was a circle of exactly 1/100 of a square meter. A James H. Heal (Halifax, UK) model 230 circular sample cutter delivered very precise samples.
[0155] All inoculated samples were placed in sterile glass jars, with a lid, and incubated for 24-hrs at 37° C., a standard setting. Following incubation, sterile D/E Neutralizing Broth was used to deactivate the antimicrobial system but not hinder the growth of bacteria. Serial dilutions were made using serial Butterfield's Buffer and 3M Petrifilm Plates (3M, St. Paul, Minn.) were used to culture the viable colonies. Following a 48-hr incubation period, colonies were counted.
[0156] These data were from the apertured film (see, FIG. 6 ) that is used as the outer layer of the food absorbent pad. There was a controlled release silver-ion system embedded in the film, as described above.
[0157] The blue line (diamonds) was the population of the E. coli inoculum as diluted to the five different concentrations. The colony count was very linear and as-planned.
[0158] The red line (squares) was the Time-Zero (T-0) measurement. This was a measurement made to determine the logical base-line of performance. To obtain this, immediately after inoculating the film, the D/E Neutralization step was conducted and the broth was plated and incubated. This accurately determined the number of colonies placed on the sample. Notice how closely it matches the blue line.
[0159] The green line (triangles) was the count of colonies recovered following a 24-hr exposure to the antimicrobial film. There are several Zero readings which did not plot. Note the concentration was plotted using a logarithmic scale so each horizontal line indicates a 10× change in colony count. The film indicates strong antimicrobial properties against E. coli.
[0160] There are two other ways to view these same data, the log reduction (see, FIG. 7 ) and the percent reduction (see, FIG. 8 ). The antimicrobial performance of the apertured film was impressive and unexpected with an average of 99.93% reduction in bacteria.
Example 15
Fiber Diameter Influence on Performance
[0161] By varying the thru put rate of the molten polymer and the air used for attenuation, the fiber diameter and degree of polymer orientation within the fiber may be modified. Additionally, the internal diameter of the polymer nozzles, in the die or spinneret plate can be modified. In this example the polymer and thru put rate was held constant while spinneret plates with different diameters were utilized and the effect of fiber diameters was measured. Extruder zone temperatures, die-head temperatures and pressures, collector belt speed and quench air settings were optimized. Diameters ranging from 0.011 to 0.023 were evaluated and resultant changes in fluid management and physical cushioning were observed. An experimental trial matrix and performance data follow in Table 16 and FIG. 9 .
[0000]
TABLE 16
Thru put
g/hole/hour
13.2
19.2
42.6
Fiber Diameter
pm
10
15
20
Nozzle ID
inches
0.011
0.015
0.023
[0162] FIG. 10 shows a magnified photograph of fibers from 0.015 inch nozzle. FIG. 11 , FIG. 12 and FIG. 13 show a magnified photograph of 0.015 inch fibers of the PLA insert in a cross-section of the non-woven pad construction with fiber direction being transverse to an exterior surface. FIG. 11 shows the pad insert orientation wherein the top surface is the horizontal surface on the photograph, and the side of the insert is the vertical surface. In FIGS. 12 and 13 , the partially vertical surface is the side of the insert, in an even more magnified photograph.
Example 16
Substrate Construction Methodology Influence on Air Permeation
[0163] For all the examples mentioned above, it is important to note that the method of construction of the food pad inserts and films themselves, and in concert with being calendared and assembled with one another has a direct influence on the air permeation value. And hence, this affects the ability of the complete food pad to either absorb moisture and/or water and also concurrently to “breathe” so as to not trap any air under it. The table above shows the different levels of air permeation for the various food pad inserts and films that have been manufactured.
Example 17
Layered Pad 1
[0164] This pad is constructed with two outer layers of PLA film and two insert layers of PLA and SAP. The film layers are 66 gsm PLA with a 2% CP-L01 (Polyvel) additive, calendared at 280° F. at 10 fpm. See, FIG. 16 . This outer layer of film adds strength and contains any SAP that would otherwise spill out of the insert layer. The tensile strength of the film is 5.579 in/lbs and is perforated during calendaring with an engraved roll (Sunday roll); the aperture size is “diamond shaped” and is approximately 0.022 inches in diameter. Triton X-100 (Dow) was applied as surfactant to each outside surface of the outer film before edge sealing to impart hydrophilic characteristics to the PLA.
[0165] Each of the two insert layers were constructed of two layers of 50 gsm PLA. A power spreader (Christy Machine Co, Freemont, Ohio), at 50% motor rpm, was used to apply 50 gsm of SAP between the two layers. This was then calendared at 240° F. at 30 fpm to bond the two layers together with the SAP in between. This insert roll was then cut into the size needed for the product application, and lightly misted with the surfactant. Two inserts for each pad were used to increase the total capacity of the absorbent pad.
[0166] All the PLA layers were comprised PLA fibers incorporating a formulation of silver Zeolite grade AC-10D from AgION coupled with silver glass grade WPA from Marubeni/Ishizuka.
[0167] The film layers were edge sealed on a single side using a ¼″ band, impulse foot sealer (American International Electric, Whittier, Calif.) at the “4” dial setting. Two insert layers were placed at the edge of the seal and then the remaining three sides were sealed. In this application the insert layers were cut to 3″ by 3″ and the film was cut at 3½ by 3½.
[0168] The absorbent capacity of this pad is 45-50 g of water completely saturated. Each pad weighs an average of 2.3 g and was then submerged in water for 60 sec. After a drip time of two minutes the pad weighed 34 g. The pad was then submerged again for sixty minutes, allowed a three minute drip time and re-weighed. The end result of 47 g full saturated. Up to the point of full absorption (defined as the point of absorption where there is a visual rupture in the edge seal of the food pad), the food pad thickness went from 0.068 inches (dry) to 0.65 inches (wet).
Example 18
Layered Pad 2
[0169] Two 33 gsm PLA film layers, integrated with a formulation of silver Zeolite grade AC-10D from AgION coupled with silver glass grade WPA from Marubeni/Ishizuka were calendared together, at 240° F., 50 fpm, at 0.001″ gap under 1000 psi to create a single outer film layer. See, FIG. 17 .
[0170] A similar single outer film layer can also be made from 50 gsm PLA with a 2% CP-L01 (Polyvel) additive, calendared at 220° F. at 20 fpm.
[0171] An inner insert layer was constructed in the following fashion: Two 33 gsm PLA non-woven uncalendared layers, integrated with a formulation of silver Zeolite grade AC-10D from AgION coupled with silver glass grade WPA from Marubeni/Ishizuka, were calendared (230° F., 50 fpm, at 0.001″ gap under 1000 psi) with 25 gsm SAP (using a powder spreader, Christy Machine, Freemont, Ohio, at 20% motor rpm) captured in between the layers. Then, another 33 gsm PLA non-woven uncalendared layer, integrated with a formulation of silver Zeolite grade AC-10D from AgION coupled with silver glass grade WPA from Marubeni/Ishizuka, was calendared (250° F., 50 fpm, at 0.001″ gap under 1000 psi) to the aforementioned pre-calendared two layers, with 25 gsm SAP (using a powder spreader, Christy Machine, Freemont, Ohio, at 20% motor rpm) captured in between the layers, to form a single three 33 gsm PLA calendared layers with two layers of SAP captured in between the layers. Two of these insert layers were placed between the outer layers and the four edges of the outside layers were heat sealed together to form the complete food pad.
[0172] The tensile strength of the outer film is 6.822 in/lbs and is perforated during calendaring with an engraved roll (Sunday roll); the aperture size is “diamond shaped” and is approximately 0.022 inches in diameter. Metolat 700 (Munzing, Bloomfield, N.J.) was applied to each outside surface of the outer film, before edge sealing, as a surfactant to impact hydrophilicity to the PLA.
[0173] The outer film layers were edge sealed on one side using a ¼″ band, impulse foot sealer (American International Electric, Whittier, Calif.) at the “4” dial setting. Two insert layers were placed at the edge of the seal and then the remaining three sides were sealed. In this application the insert layers were cut to 2.5″ by 2.5″ and the film was cut at 3.5″ by 3.5″.
[0174] A simple water absorption test was carried out. The dry weight of the pad was 2.5 grams and was then submerged in water for 60 sec. After a drip time of two minutes the pad weighed 39 g. The pad was then submerged again for sixty minutes, allowed a three minute drip time and re-weighed. The end result was 57 g fully saturated with the pad reaching its full absorption capability, defined as the point of absorption where there is a visual rupture in the edge seal of the food pad. Up to the point of full absorption, the food pad thickness went from 0.068 inches (dry) to 0.65 inches (wet).
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Disclosed are food packaging materials and processes that are useful for commercial products to extend the freshness and preserve the integrity and shelf-life of packaged foods. Said food packaging materials utilize a low bioburden, biodegradable and/or compostable shock absorbing/cushioning nonwoven structure and some form or forms of an antimicrobial and/or antifungal agent consisting of silver or silver-based species that destroy microbes which would otherwise spoil the food. The shelf-life extension process involves silver-based antimicrobial agents that function to mitigate the spread of food spoilage pathogens when they come in contact with the said food packaging materials. Fluid absorbing or superabsorbent, capabilities may be incorporated in the structure to control excess fluids.
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CROSS-REFERENCE TO RELATED APPLICATIONS
This application is a continuation of U.S. patent application Ser. No. 14/680,745, filed Apr. 7, 2015, which is a continuation of U.S. patent application Ser. No. 13/619,160, filed Sep. 14, 2012, now U.S. Pat. No. 9,006,260, which is a continuation of Ser. No. 12/143,427, filed Jun. 20, 2008, now U.S. Pat. No. 8,278,318, which claims the benefit of U.S. Ser. No. 60/945,487, filed Jun. 21, 2007. The entire disclosure of each of the related applications is incorporated herein by reference in its entirety.
FIELD OF THE INVENTION
The present invention relates to certain spirocyclic compounds that are inhibitors of 11-β hydroxyl steroid dehydrogenase type 1 (11βHSD1), compositions containing the same, and methods of using the same for the treatment of diabetes, obesity and other diseases.
BACKGROUND OF THE INVENTION
The importance of the hypothalamic-pituitary-adrenal (HPA) axis in controlling glucocorticoid excursions is evident from the fact that disruption of homeostasis in the HPA axis by either excess or deficient secretion or action results in Cushing's syndrome or Addison's disease, respectively (Miller and Chrousos (2001) Endocrinology and Metabolism, eds. Felig and Frohman (McGraw-Hill, New York), 4 th Ed.: 387-524). Patients with Cushing's syndrome (a rare disease characterized by systemic glucocorticoid excess originating from the adrenal or pituitary tumors) or receiving glucocorticoid therapy develop reversible visceral fat obesity. Interestingly, the phenotype of Cushing's syndrome patients closely resembles that of Reaven's metabolic syndrome (also known as Syndrome X or insulin resistance syndrome) the symptoms of which include visceral obesity, glucose intolerance, insulin resistance, hypertension, type 2 diabetes and hyperlipidemia (Reaven (1993) Ann. Rev. Med. 44: 121-131). However, the role of glucocorticoids in prevalent forms of human obesity has remained obscure because circulating glucocorticoid concentrations are not elevated in the majority of metabolic syndrome patients. In fact, glucocorticoid action on target tissue depends not only on circulating levels but also on intracellular concentration, locally enhanced action of glucocorticoids in adipose tissue and skeletal muscle has been demonstrated in metabolic syndrome. Evidence has accumulated that enzyme activity of 11βHSD1, which regenerates active glucocorticoids from inactive forms and plays a central role in regulating intracellular glucocorticoid concentration, is commonly elevated in fat depots from obese individuals. This suggests a role for local glucocorticoid reactivation in obesity and metabolic syndrome.
Given the ability of 11βHSD1 to regenerate cortisol from inert circulating cortisone, considerable attention has been given to its role in the amplification of glucocorticoid function. 11βHSD1 is expressed in many key GR-rich tissues, including tissues of considerable metabolic importance such as liver, adipose, and skeletal muscle, and, as such, has been postulated to aid in the tissue-specific potentiation of glucocorticoid-mediated antagonism of insulin function. Considering a) the phenotypic similarity between glucocorticoid excess (Cushing's syndrome) and the metabolic syndrome with normal circulating glucocorticoids in the latter, as well as b) the ability of 11βHSD1 to generate active cortisol from inactive cortisone in a tissue-specific manner, it has been suggested that central obesity and the associated metabolic complications in syndrome X result from increased activity of 11βHSD1 within adipose tissue, resulting in ‘Cushing's disease of the omentum’ (Bujalska et al. (1997) Lancet 349: 1210-1213). Indeed, 11βHSD1 has been shown to be upregulated in adipose tissue of obese rodents and humans (Livingstone et al. (2000) Endocrinology 131: 560-563; Rask et al. (2001) J. Clin. Endocrinol. Metab. 86: 1418-1421; Lindsay et al. (2003) J. Clin. Endocrinol. Metab. 88: 2738-2744; Wake et al. (2003) J. Clin. Endocrinol. Metab. 88: 3983-3988).
Additional support for this notion has come from studies in mouse transgenic models. Adipose-specific overexpression of 11βHSD1 under the control of the aP2 promoter in mouse produces a phenotype remarkably reminiscent of human metabolic syndrome (Masuzaki et al. (2001) Science 294: 2166-2170; Masuzaki et al. (2003) J. Clinical Invest. 112: 83-90). Importantly, this phenotype occurs without an increase in total circulating corticosterone, but rather is driven by a local production of corticosterone within the adipose depots. The increased activity of 11βHSD1 in these mice (2-3 fold) is very similar to that observed in human obesity (Rask et al. (2001) J. Clin. Endocrinol. Metab. 86: 1418-1421). This suggests that local 11βHSD1-mediated conversion of inert glucocorticoid to active glucocorticoid can have profound influences whole body insulin sensitivity.
Based on this data, it would be predicted that the loss of 11βHSD1 would lead to an increase in insulin sensitivity and glucose tolerance due to a tissue-specific deficiency in active glucocorticoid levels. This is, in fact, the case as shown in studies with 11βHSD1-deficient mice produced by homologous recombination (Kotelevstev et al. (1997) Proc. Natl. Acad. Sci. 94: 14924-14929; Morton et al. (2001) J. Biol. Chem. 276: 41293-41300; Morton et al. (2004) Diabetes 53: 931-938). These mice are completely devoid of 11-keto reductase activity, confirming that 11βHSD1 encodes the only activity capable of generating active corticosterone from inert 11-dehydrocorticosterone. 11βHSD1-deficient mice are resistant to diet- and stress-induced hyperglycemia, exhibit attenuated induction of hepatic gluconeogenic enzymes (PEPCK, G6P), show increased insulin sensitivity within adipose, and have an improved lipid profile (decreased triglycerides and increased cardio-protective HDL). Additionally, these animals show resistance to high fat diet-induced obesity. Taken together, these transgenic mouse studies confirm a role for local reactivation of glucocorticoids in controlling hepatic and peripheral insulin sensitivity, and suggest that inhibition of 11βHSD1 activity may prove beneficial in treating a number of glucocorticoid-related disorders, including obesity, insulin resistance, hyperglycemia, and hyperlipidemia.
Data in support of this hypothesis has been published. Recently, it was reported that 11βHSD1 plays a role in the pathogenesis of central obesity and the appearance of the metabolic syndrome in humans. Increased expression of the 11βHSD1 gene is associated with metabolic abnormalities in obese women and that increased expression of this gene is suspected to contribute to the increased local conversion of cortisone to cortisol in adipose tissue of obese individuals (Engeli, et al., (2004) Obes. Res. 12: 9-17).
A new class of 11βHSD1 inhibitors, the arylsulfonamidothiazoles, was shown to improve hepatic insulin sensitivity and reduce blood glucose levels in hyperglycemic strains of mice (Barf et al. (2002) J. Med. Chem. 45: 3813-3815; Alberts et al. Endocrinology (2003) 144: 4755-4762). Furthermore, it was recently reported that selective inhibitors of 11βHSD1 can ameliorate severe hyperglycemia in genetically diabetic obese mice. Thus, 11βHSD1 is a promising pharmaceutical target for the treatment of the Metabolic Syndrome (Masuzaki, et al., (2003) Curr. Drug Targets Immune Endocr. Metabol. Disord. 3: 255-62).
A. Obesity and Metabolic Syndrome
As described above, multiple lines of evidence suggest that inhibition of 11βHSD1 activity can be effective in combating obesity and/or aspects of the metabolic syndrome cluster, including glucose intolerance, insulin resistance, hyperglycemia, hypertension, and/or hyperlipidemia. Glucocorticoids are known antagonists of insulin action, and reductions in local glucocorticoid levels by inhibition of intracellular cortisone to cortisol conversion should increase hepatic and/or peripheral insulin sensitivity and potentially reduce visceral adiposity. As described above, 11βHSD1 knockout mice are resistant to hyperglycemia, exhibit attenuated induction of key hepatic gluconeogenic enzymes, show markedly increased insulin sensitivity within adipose, and have an improved lipid profile. Additionally, these animals show resistance to high fat diet-induced obesity (Kotelevstev et al. (1997) Proc. Natl. Acad. Sci. 94: 14924-14929; Morton et al. (2001) J. Biol. Chem. 276: 41293-41300; Morton et al. (2004) Diabetes 53: 931-938). Thus, inhibition of 11βHSD1 is predicted to have multiple beneficial effects in the liver, adipose, and/or skeletal muscle, particularly related to alleviation of component(s) of the metabolic syndrome and/or obesity.
B. Pancreatic Function
Glucocorticoids are known to inhibit the glucose-stimulated secretion of insulin from pancreatic beta-cells (Billaudel and Sutter (1979) Horm. Metab. Res. 11: 555-560). In both Cushing's syndrome and diabetic Zucker fa/fa rats, glucose-stimulated insulin secretion is markedly reduced (Ogawa et al. (1992) J. Clin. Invest. 90: 497-504). 11βHSD1 mRNA and activity has been reported in the pancreatic islet cells of ob/ob mice and inhibition of this activity with carbenoxolone, an 11βHSD1 inhibitor, improves glucose-stimulated insulin release (Davani et al. (2000) J. Biol. Chem. 275: 34841-34844). Thus, inhibition of 11βHSD1 is predicted to have beneficial effects on the pancreas, including the enhancement of glucose-stimulated insulin release.
C. Cognition and Dementia
Mild cognitive impairment is a common feature of aging that may be ultimately related to the progression of dementia. In both aged animals and humans, inter-individual differences in general cognitive function have been linked to variability in the long-term exposure to glucocorticoids (Lupien et al. (1998) Nat. Neurosci. 1: 69-73). Further, dysregulation of the HPA axis resulting in chronic exposure to glucocorticoid excess in certain brain subregions has been proposed to contribute to the decline of cognitive function (McEwen and Sapolsky (1995) Curr. Opin. Neurobiol. 5: 205-216). 11βHSD1 is abundant in the brain, and is expressed in multiple subregions including the hippocampus, frontal cortex, and cerebellum (Sandeep et al. (2004) Proc. Natl. Acad. Sci. Early Edition: 1-6). Treatment of primary hippocampal cells with the 11βHSD1 inhibitor carbenoxolone protects the cells from glucocorticoid-mediated exacerbation of excitatory amino acid neurotoxicity (Rajan et al. (1996) J. Neurosci. 16: 65-70). Additionally, 11βHSD1-deficient mice are protected from glucocorticoid-associated hippocampal dysfunction that is associated with aging (Yau et al. (2001) Proc. Natl. Acad. Sci. 98: 4716-4721). In two randomized, double-blind, placebo-controlled crossover studies, administration of carbenoxolone improved verbal fluency and verbal memory (Sandeep et al. (2004) Proc. Natl. Acad. Sci. Early Edition: 1-6). Thus, inhibition of 11βHSD1 is predicted to reduce exposure to glucocorticoids in the brain and protect against deleterious glucocorticoid effects on neuronal function, including cognitive impairment, dementia, and/or depression.
D. Intra-Ocular Pressure
Glucocorticoids can be used topically and systemically for a wide range of conditions in clinical ophthalmology. One particular complication with these treatment regimens is corticosteroid-induced glaucoma. This pathology is characterized by a significant increase in intra-ocular pressure (IOP). In its most advanced and untreated form, IOP can lead to partial visual field loss and eventually blindness. IOP is produced by the relationship between aqueous humour production and drainage. Aqueous humour production occurs in the non-pigmented epithelial cells (NPE) and its drainage is through the cells of the trabecular meshwork. 11βHSD1 has been localized to NPE cells (Stokes et al. (2000) Invest. Ophthalmol. Vis. Sci. 41: 1629-1683; Rauz et al. (2001) Invest. Ophthalmol. Vis. Sci. 42: 2037-2042) and its function is likely relevant to the amplification of glucocorticoid activity within these cells. This notion has been confirmed by the observation that free cortisol concentration greatly exceeds that of cortisone in the aqueous humour (14:1 ratio). The functional significance of 11βHSD1 in the eye has been evaluated using the inhibitor carbenoxolone in healthy volunteers (Rauz et al. (2001) Invest. Ophthalmol. Vis. Sci. 42: 2037-2042). After seven days of carbenoxolone treatment, IOP was reduced by 18%. Thus, inhibition of 11βHSD1 in the eye is predicted to reduce local glucocorticoid concentrations and IOP, producing beneficial effects in the management of glaucoma and other visual disorders.
E. Hypertension
Adipocyte-derived hypertensive substances such as leptin and angiotensinogen have been proposed to be involved in the pathogenesis of obesity-related hypertension (Matsuzawa et al. (1999) Ann. N.Y. Acad. Sci. 892: 146-154; Wajchenberg (2000) Endocr. Rev. 21: 697-738). Leptin, which is secreted in excess in aP2-11βHSD1 transgenic mice (Masuzaki et al. (2003) J. Clinical Invest. 112: 83-90), can activate various sympathetic nervous system pathways, including those that regulate blood pressure (Matsuzawa et al. (1999) Ann. N.Y. Acad. Sci. 892: 146-154). Additionally, the renin-angiotensin system (RAS) has been shown to be a major determinant of blood pressure (Walker et al. (1979) Hypertension 1: 287-291). Angiotensinogen, which is produced in liver and adipose tissue, is the key substrate for renin and drives RAS activation. Plasma angiotensinogen levels are markedly elevated in aP2-11βHSD1 transgenic mice, as are angiotensin II and aldosterone (Masuzaki et al. (2003) J. Clinical Invest. 112: 83-90). These forces likely drive the elevated blood pressure observed in aP2-11βHSD1 transgenic mice. Treatment of these mice with low doses of an angiotensin II receptor antagonist abolishes this hypertension (Masuzaki et al. (2003) J. Clinical Invest. 112: 83-90). This data illustrates the importance of local glucocorticoid reactivation in adipose tissue and liver, and suggests that hypertension may be caused or exacerbated by 11βHSD1 activity. Thus, inhibition of 11βHSD1 and reduction in adipose and/or hepatic glucocorticoid levels is predicted to have beneficial effects on hypertension and hypertension-related cardiovascular disorders.
F. Bone Disease
Glucocorticoids can have adverse effects on skeletal tissues. Continued exposure to even moderate glucocorticoid doses can result in osteoporosis (Cannalis (1996) J. Clin. Endocrinol. Metab. 81: 3441-3447) and increased risk for fractures. Experiments in vitro confirm the deleterious effects of glucocorticoids on both bone-resorbing cells (also known as osteoclasts) and bone forming cells (osteoblasts). 11βHSD1 has been shown to be present in cultures of human primary osteoblasts as well as cells from adult bone, likely a mixture of osteoclasts and osteoblasts (Cooper et al. (2000) Bone 27: 375-381), and the 11βHSD1 inhibitor carbenoxolone has been shown to attenuate the negative effects of glucocorticoids on bone nodule formation (Bellows et al. (1998) Bone 23: 119-125). Thus, inhibition of 11βHSD1 is predicted to decrease the local glucocorticoid concentration within osteoblasts and osteoclasts, producing beneficial effects in various forms of bone disease, including osteoporosis.
Small molecule inhibitors of 11βHSD1 are currently being developed to treat or prevent 11βHSD1-related diseases such as those described above. For example, certain amide-based inhibitors are reported in WO 2004/089470, WO 2004/089896, WO 2004/056745, and WO 2004/065351. Additional small molecule inhibitors of 11βHSD1 are reported in US 2005/0282858, US 2006/0009471, US 2005/0288338, US 2006/0009491, US 2006/0004049, US 2005/0288317, US 2005/0288329, US 2006/0122197, US 2006/0116382, and US 2006/0122210.
11) INCY0035 (US 2007/0066584)
Antagonists of 11βHSD1 have been evaluated in human clinical trials (Kurukulasuriya, et al., (2003) Curr. Med. Chem. 10: 123-53).
In light of the experimental data indicating a role for 11βHSD1 in glucocorticoid-related disorders, metabolic syndrome, hypertension, obesity, insulin resistance, hyperglycemia, hyperlipidemia, type 2 diabetes, androgen excess (hirsutism, menstrual irregularity, hyperandrogenism) and polycystic ovary syndrome (PCOS), therapeutic agents aimed at augmentation or suppression of these metabolic pathways, by modulating glucocorticoid signal transduction at the level of 11βHSD1 are desirable.
As evidenced herein, there is a continuing need for new and improved drugs that target 11βHSD1. The compounds, compositions and methods described herein help meet this and other needs.
SUMMARY OF THE INVENTION
The present invention provides, inter alia, inhibitors of 11βHSD1 having Formula I:
or pharmaceutically acceptable salts thereof, wherein the variables are defined below.
The present invention further provides compositions comprising a compound of Formula I, or a pharmaceutically acceptable salt thereof, and at least one pharmaceutically acceptable carrier.
The present invention further provides methods of inhibiting 11βHSD1 by contacting the 11βHSD1 with a compound of Formula I, or a pharmaceutically acceptable salt thereof.
The present invention further provides methods of inhibiting activity of 11βHSD1 comprising contacting the 11βHSD1 with a compound of Formula I, or a pharmaceutically acceptable salt thereof.
The present invention further provides methods of inhibiting the conversion of cortisone to cortisol in a cell comprising contacting the cell with a compound of Formula I, or a pharmaceutically acceptable salt thereof.
The present invention further provides methods of inhibiting the production of cortisol in a cell comprising contacting the cell with a compound of Formula I, or a pharmaceutically acceptable salt thereof.
The present invention further provides methods of treating various diseases including any one of the following disorders, or any combination of two or more of the following disorders: obesity; diabetes; glucose intolerance; insulin resistance; hyperglycemia; hypertension; hyperlipidemia; cognitive impairment; depression; dementia; glaucoma; cardiovascular disorders; osteoporosis; inflammation; metabolic syndrome; androgen excess; or polycystic ovary syndrome (PCOS) in a patient comprising administering to the patient a therapeutically effective amount of a compound of Formula I, or a pharmaceutically acceptable salt thereof.
DETAILED DESCRIPTION
The present invention provides, inter alia, inhibitors of 11βHSD1 having Formula I:
or pharmaceutically acceptable salts thereof, wherein:
R 1 is F, Cl, Br, or I; and
R 2 and R 3 are independently selected from H, C 1-6 alkyl, and C 3-6 cycloalkyl.
In some embodiments:
R 1 is F and Cl; and R 2 and R 3 are independently selected from H and C 1-4 alkyl.
In some embodiments, R 1 is F or Cl.
In some embodiments, R 1 is F.
In some embodiments, R 1 is Cl.
In some embodiments, R 2 and R 3 are independently selected from H, methyl, and ethyl.
In some embodiments, at least one of R 2 and R 3 is other than H.
In some embodiments, the compounds of the invention have Formula II:
At various places in the present specification, substituents of compounds of the invention are disclosed in groups or in ranges. It is specifically intended that the invention include each and every individual subcombination of the members of such groups and ranges. For example, the term “C 1-6 alkyl” is specifically intended to individually disclose methyl, ethyl, C 3 alkyl, C 4 alkyl, C 5 alkyl, and C 6 alkyl.
It is further appreciated that certain features of the invention, which are, for clarity, described in the context of separate embodiments, can also be provided in combination in a single embodiment. Conversely, various features of the invention which are, for brevity, described in the context of a single embodiment, can also be provided separately or in any suitable subcombination.
As used herein, the term “alkyl” is meant to refer to a saturated hydrocarbon group which is straight-chained or branched. Example alkyl groups include methyl (Me), ethyl (Et), propyl (e.g., n-propyl and isopropyl), butyl (e.g., n-butyl, isobutyl, t-butyl), pentyl (e.g., n-pentyl, isopentyl, neopentyl), and the like.
As used herein, “cycloalkyl” refers to non-aromatic 3-7 membered carbocycles including, for example, cyclopropyl, cyclobutyl, cyclopentyl, and cyclohexyl.
The compounds described herein are asymmetric (e.g., having one or more stereocenters). All stereoisomers, such as enantiomers, are intended unless otherwise indicated. Compounds of the present invention that contain asymmetrically substituted carbon atoms can be isolated in optically active or racemic forms. Methods on how to prepare optically active forms from optically active starting materials are known in the art, such as by resolution of racemic mixtures or by stereoselective synthesis. Cis and trans isomers of the compounds of the present invention are described and may be isolated as a mixture of isomers or as separated isomeric forms.
Compounds of the invention can also include tautomeric forms. Tautomeric forms result from the swapping of a single bond with an adjacent double bond together with the concomitant migration of a proton. Tautomeric forms include prototropic tautomers which are isomeric protonation states having the same empirical formula and total charge. Example prototropic tautomers include ketone—enol pairs, amide—imidic acid pairs, lactam—lactim pairs, amide—imidic acid pairs, enamine—imine pairs, and annular forms where a proton can occupy two or more positions of a heterocyclic system, for example, 1H- and 3H-imidazole, 1H-, 2H- and 4H-1,2,4-triazole, 1H- and 2H-isoindole, and 1H- and 2H-pyrazole. Tautomeric forms can be in equilibrium or sterically locked into one form by appropriate substitution.
Compounds of the invention can also include all isotopes of atoms occurring in the intermediates or final compounds. Isotopes include those atoms having the same atomic number but different mass numbers. For example, isotopes of hydrogen include tritium and deuterium.
All compounds, and pharmaceutically acceptable salts thereof, may be obtained in various solid forms, including solvated or hydrated forms. In some embodiments, the solid form is a crystalline form. Methods for preparing and discovering different solid forms are routine in the art and include, for example, X-ray powder diffraction, differential scanning calorimetry, thermogravimetric analysis, dynamic vapor sorption, FT-IR, Raman scattering methods, solid state NMR, Karl-Fischer titration, etc.
In some embodiments, the compounds of the invention, and salts thereof, are substantially isolated. By “substantially isolated” is meant that the compound is at least partially or substantially separated from the environment in which it was formed or detected. Partial separation can include, for example, a composition enriched in the compound of the invention. Substantial separation can include compositions containing at least about 50%, at least about 60%, at least about 70%, at least about 80%, at least about 90%, at least about 95%, at least about 97%, or at least about 99% by weight of the compound of the invention, or salt thereof. Methods for isolating compounds and their salts are routine in the art.
The present invention also includes pharmaceutically acceptable salts of the compounds described herein. As used herein, “pharmaceutically acceptable salts” refers to derivatives of the disclosed compounds wherein the parent compound is modified by converting an existing acid or base moiety to its salt form. Examples of pharmaceutically acceptable salts include, but are not limited to, mineral or organic acid salts of basic residues such as amines; alkali or organic salts of acidic residues such as carboxylic acids; and the like. The pharmaceutically acceptable salts of the present invention include the conventional non-toxic salts of the parent compound formed, for example, from non-toxic inorganic or organic acids. The pharmaceutically acceptable salts of the present invention can be synthesized from the parent compound which contains a basic or acidic moiety by conventional chemical methods. Generally, such salts can be prepared by reacting the free acid or base forms of these compounds with a stoichiometric amount of the appropriate base or acid in water or in an organic solvent, or in a mixture of the two; generally, nonaqueous media like ether, ethyl acetate, ethanol, isopropanol, or acetonitrile are preferred. Lists of suitable salts are found in Remington's Pharmaceutical Sciences, 17th ed., Mack Publishing Company, Easton, Pa., 1985, p. 1418 and Journal of Pharmaceutical Science, 66, 2 (1977), each of which is incorporated herein by reference in its entirety.
The phrase “pharmaceutically acceptable” is employed herein to refer to those compounds, materials, compositions, and/or dosage forms which are, within the scope of sound medical judgment, suitable for use in contact with the tissues of human beings and animals without excessive toxicity, irritation, allergic response, or other problem or complication, commensurate with a reasonable benefit/risk ratio.
Compounds of the invention can modulate activity of 11βHSD1. The term “modulate” is meant to refer to an ability to increase or decrease activity of an enzyme or receptor. Accordingly, compounds of the invention can be used in methods of modulating 11βHSD1 by contacting the enzyme or receptor with any one or more of the compounds or compositions described herein. In some embodiments, compounds of the present invention can act as inhibitors of 11βHSD1. In further embodiments, the compounds of the invention can be used to modulate activity of 11βHSD1 in an individual in need of modulation of the enzyme or receptor by administering a modulating amount of a compound of the invention.
The present invention further provides methods of inhibiting the conversion of cortisone to cortisol in a cell, or inhibiting the production of cortisol in a cell, where conversion to or production of cortisol is mediated, at least in part, by 11βHSD1 activity. Methods of measuring conversion rates of cortisone to cortisol and vice versa, as well as methods for measuring levels of cortisone and cortisol in cells, are routine in the art.
The present invention further provides methods of increasing insulin sensitivity of a cell by contacting the cell with a compound of the invention. Methods of measuring insulin sensitivity are routine in the art.
The present invention further provides methods of treating disease associated with activity or expression, including abnormal activity and overexpression, of 11βHSD1 in an individual (e.g., patient) by administering to the individual in need of such treatment a therapeutically effective amount or dose of a compound of the present invention, or pharmaceutically acceptable salt thereof, or a pharmaceutical composition thereof. Example diseases can include any disease, disorder or condition that is directly or indirectly linked to expression or activity of the enzyme. An 11βHSD1-associated disease can also include any disease, disorder or condition that can be prevented, ameliorated, or cured by modulating enzyme activity.
Examples of 11βHSD1-associated diseases include obesity, diabetes, glucose intolerance, insulin resistance, hyperglycemia, hypertension, hyperlipidemia, cognitive impairment, dementia, depression (e.g., psychotic depression), glaucoma, cardiovascular disorders, osteoporosis, and inflammation. Further examples of 11βHSD1-associated diseases include metabolic syndrome, type 2 diabetes, androgen excess (hirsutism, menstrual irregularity, hyperandrogenism) and polycystic ovary syndrome (PCOS).
As used herein, the term “cell” is meant to refer to a cell that is in vitro, ex vivo or in vivo. In some embodiments, an ex vivo cell can be part of a tissue sample excised from an organism such as a mammal. In some embodiments, an in vitro cell can be a cell in a cell culture. In some embodiments, an in vivo cell is a cell living in an organism such as a mammal. In some embodiments, the cell is an adipocyte, a pancreatic cell, a hepatocyte, neuron, or cell comprising the eye (ocular cell).
As used herein, the term “contacting” refers to the bringing together of indicated moieties in an in vitro system or an in vivo system. For example, “contacting” the 11βHSD1 enzyme with a compound of the invention includes the administration of a compound of the present invention to an individual or patient, such as a human, having 11βHSD1, as well as, for example, introducing a compound of the invention into a sample containing a cellular or purified preparation containing the 11βHSD1 enzyme.
As used herein, the term “individual” or “patient,” used interchangeably, refers to any animal, including mammals, preferably mice, rats, other rodents, rabbits, dogs, cats, swine, cattle, sheep, horses, or primates, and most preferably humans.
As used herein, the term “treating” or “treatment” refers to one or more of (1) preventing the disease; for example, preventing a disease, condition or disorder in an individual who may be predisposed to the disease, condition or disorder but does not yet experience or display the pathology or symptomatology of the disease; (2) inhibiting the disease; for example, inhibiting a disease, condition or disorder in an individual who is experiencing or displaying the pathology or symptomatology of the disease, condition or disorder; and (3) ameliorating the disease; for example, ameliorating a disease, condition or disorder in an individual who is experiencing or displaying the pathology or symptomatology of the disease, condition or disorder (i.e., reversing the pathology and/or symptomatology) such as decreasing the severity of disease.
When employed as pharmaceuticals, the compounds of the invention can be administered in the form of pharmaceutical compositions which is a combination of a compound of the invention and at least one pharmaceutically acceptable carrier. These compositions can be prepared in a manner well known in the pharmaceutical art, and can be administered by a variety of routes, depending upon whether local or systemic treatment is desired and upon the area to be treated. Administration may be topical (including ophthalmic and to mucous membranes including intranasal, vaginal and rectal delivery), pulmonary (e.g., by inhalation or insufflation of powders or aerosols, including by nebulizer; intratracheal, intranasal, epidermal and transdermal), ocular, oral or parenteral. Methods for ocular delivery can include topical administration (eye drops), subconjunctival, periocular or intravitreal injection or introduction by balloon catheter or ophthalmic inserts surgically placed in the conjunctival sac. Parenteral administration includes intravenous, intraarterial, subcutaneous, intraperitoneal or intramuscular injection or infusion; or intracranial, e.g., intrathecal or intraventricular, administration. Parenteral administration can be in the form of a single bolus dose, or may be, for example, by a continuous perfusion pump. Pharmaceutical compositions and formulations for topical administration may include transdermal patches, ointments, lotions, creams, gels, drops, suppositories, sprays, liquids and powders. Conventional pharmaceutical carriers, aqueous, powder or oily bases, thickeners and the like may be necessary or desirable.
This invention also includes pharmaceutical compositions which contain, as the active ingredient, one or more of the compounds of the invention above in combination with one or more pharmaceutically acceptable carriers. In making the compositions of the invention, the active ingredient is typically mixed with an excipient, diluted by an excipient or enclosed within such a carrier in the form of, for example, a capsule, sachet, paper, or other container. When the excipient serves as a diluent, it can be a solid, semi-solid, or liquid material, which acts as a vehicle, carrier or medium for the active ingredient. Thus, the compositions can be in the form of tablets, pills, powders, lozenges, sachets, cachets, elixirs, suspensions, emulsions, solutions, syrups, aerosols (as a solid or in a liquid medium), ointments containing, for example, up to 10% by weight of the active compound, soft and hard gelatin capsules, suppositories, sterile injectable solutions, and sterile packaged powders.
In preparing a formulation, the active compound can be milled to provide the appropriate particle size prior to combining with the other ingredients. If the active compound is substantially insoluble, it can be milled to a particle size of less than 200 mesh. If the active compound is substantially water soluble, the particle size can be adjusted by milling to provide a substantially uniform distribution in the formulation, e.g. about 40 mesh.
The compounds of the invention may be milled using known milling procedures such as wet milling to obtain a particle size appropriate for tablet formation and for other formulation types. Finely divided (nanoparticulate) preparations of the compounds of the invention can be prepared by processes known in the art, for example see International Patent Application No. WO 2002/000196.
Some examples of suitable excipients include lactose, dextrose, sucrose, sorbitol, mannitol, starches, gum acacia, calcium phosphate, alginates, tragacanth, gelatin, calcium silicate, microcrystalline cellulose, polyvinylpyrrolidone, cellulose, water, syrup, and methyl cellulose. The formulations can additionally include: lubricating agents such as talc, magnesium stearate, and mineral oil; wetting agents; emulsifying and suspending agents; preserving agents such as methyl- and propylhydroxy-benzoates; sweetening agents; and flavoring agents. The compositions of the invention can be formulated so as to provide quick, sustained or delayed release of the active ingredient after administration to the patient by employing procedures known in the art.
The compositions can be formulated in a unit dosage form, each dosage containing from about 5 to about 100 mg, more usually about 10 to about 30 mg, of the active ingredient. The term “unit dosage forms” refers to physically discrete units suitable as unitary dosages for human subjects and other mammals, each unit containing a predetermined quantity of active material calculated to produce the desired therapeutic effect, in association with a suitable pharmaceutical excipient.
The active compound can be effective over a wide dosage range and is generally administered in a pharmaceutically effective amount. It will be understood, however, that the amount of the compound actually administered will usually be determined by a physician, according to the relevant circumstances, including the condition to be treated, the chosen route of administration, the actual compound administered, the age, weight, and response of the individual patient, the severity of the patient's symptoms, and the like.
For preparing solid compositions such as tablets, the principal active ingredient is mixed with a pharmaceutical excipient to form a solid preformulation composition containing a homogeneous mixture of a compound of the present invention. When referring to these preformulation compositions as homogeneous, the active ingredient is typically dispersed evenly throughout the composition so that the composition can be readily subdivided into equally effective unit dosage forms such as tablets, pills and capsules. This solid preformulation is then subdivided into unit dosage forms of the type described above containing from, for example, 0.1 to about 500 mg of the active ingredient of the present invention.
The tablets or pills of the present invention can be coated or otherwise compounded to provide a dosage form affording the advantage of prolonged action. For example, the tablet or pill can comprise an inner dosage and an outer dosage component, the latter being in the form of an envelope over the former. The two components can be separated by an enteric layer which serves to resist disintegration in the stomach and permit the inner component to pass intact into the duodenum or to be delayed in release. A variety of materials can be used for such enteric layers or coatings, such materials including a number of polymeric acids and mixtures of polymeric acids with such materials as shellac, cetyl alcohol, and cellulose acetate.
The liquid forms in which the compounds and compositions of the present invention can be incorporated for administration orally or by injection include aqueous solutions, suitably flavored syrups, aqueous or oil suspensions, and flavored emulsions with edible oils such as cottonseed oil, sesame oil, coconut oil, or peanut oil, as well as elixirs and similar pharmaceutical vehicles.
Compositions for inhalation or insufflation include solutions and suspensions in pharmaceutically acceptable, aqueous or organic solvents, or mixtures thereof, and powders. The liquid or solid compositions may contain suitable pharmaceutically acceptable excipients as described supra. In some embodiments, the compositions are administered by the oral or nasal respiratory route for local or systemic effect. Compositions in can be nebulized by use of inert gases. Nebulized solutions may be breathed directly from the nebulizing device or the nebulizing device can be attached to a face masks tent, or intermittent positive pressure breathing machine. Solution, suspension, or powder compositions can be administered orally or nasally from devices which deliver the formulation in an appropriate manner.
The amount of compound or composition administered to a patient will vary depending upon what is being administered, the purpose of the administration, such as prophylaxis or therapy, the state of the patient, the manner of administration, and the like. In therapeutic applications, compositions can be administered to a patient already suffering from a disease in an amount sufficient to cure or at least partially arrest the symptoms of the disease and its complications. Effective doses will depend on the disease condition being treated as well as by the judgment of the attending clinician depending upon factors such as the severity of the disease, the age, weight and general condition of the patient, and the like.
The compositions administered to a patient can be in the form of pharmaceutical compositions described above. These compositions can be sterilized by conventional sterilization techniques, or may be sterile filtered. Aqueous solutions can be packaged for use as is, or lyophilized, the lyophilized preparation being combined with a sterile aqueous carrier prior to administration. The pH of the compound preparations typically will be between 3 and 11, more preferably from 5 to 9 and most preferably from 7 to 8. It will be understood that use of certain of the foregoing excipients, carriers, or stabilizers will result in the formation of pharmaceutical salts.
The therapeutic dosage of the compounds of the present invention can vary according to, for example, the particular use for which the treatment is made, the manner of administration of the compound, the health and condition of the patient, and the judgment of the prescribing physician. The proportion or concentration of a compound of the invention in a pharmaceutical composition can vary depending upon a number of factors including dosage, chemical characteristics (e.g., hydrophobicity), and the route of administration. For example, the compounds of the invention can be provided in an aqueous physiological buffer solution containing about 0.1 to about 10% w/v of the compound for parenteral administration. Some typical dose ranges are from about 1 μg/kg to about 1 g/kg of body weight per day. In some embodiments, the dose range is from about 0.01 mg/kg to about 100 mg/kg of body weight per day. The dosage is likely to depend on such variables as the type and extent of progression of the disease or disorder, the overall health status of the particular patient, the relative biological efficacy of the compound selected, formulation of the excipient, and its route of administration. Effective doses can be extrapolated from dose-response curves derived from in vitro or animal model test systems.
The compounds of the invention can also be formulated in combination with one or more additional active ingredients which can include any pharmaceutical agent such as anti-viral agents, vaccines, antibodies, immune enhancers, immune suppressants, anti-inflammatory agents, analgesics, and drugs for the treatment of diabetes or obesity, hyperglycemia, hypertension, hyperlipidemia, and the like. Agents for treatment of metabolic disorders with which a compound of the invention could be combined include, but are not limited to, amylin analogues, incretin mimetics, inhibitors of the incretin-degrading enzyme dipeptidyl peptidase-IV, agonists of peroxisome proliferator-activated receptor (PPAR)-a and PPAR-g, and CB1 cannabinoid receptor inhibitors.
The invention will be described in greater detail by way of specific examples. The following examples are offered for illustrative purposes, and are not intended to limit the invention in any manner. Those of skill in the art will readily recognize a variety of noncritical parameters which can be changed or modified to yield essentially the same results.
EXAMPLES
All compounds were purified by either flash column chromatography or reversed-phase liquid chromatography using a Waters FractionLynx LC-MS system with mass directed fractionation. Column: Waters XBridge C 18 5 μm, 19×100 mm; mobile phase A: 0.15% NH 4 OH in water and mobile phase B: 0.15% NH 4 OH in acetonitrile; the flow rate was 30 ml/m, the separating gradient was optimized for each compound using the Compound Specific Method Optimization protocol as described in literature [“Preparative LC-MS Purification: Improved Compound Specific Method Optimization”, K Blom, B. Glass, R. Sparks, A. Combs, J. Combi. Chem., 2004, 6, 874-883].
The separated product was then typically subjected to analytical LC/MS for purity check under the following conditions: Instrument; Agilent 1100 series, LC/MSD, Column: Waters Sunfire™ C 18 5 μm, 2.1×5.0 mm, Buffers: mobile phase A: 0.025% TFA in water and mobile phase B: 0.025% TFA in acetonitrile; gradient 2% to 80% of buffer B in 3 min with flow rate 1.5 mL/min.
Example 1
5-{3-Fluoro-4-[(5S)-2-(cis-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]dec-7-yl]phenyl}-N-methylpyridine-2-carboxamide
Step 1: 1-benzyl 3-ethyl piperidine-1,3-dicarboxylate
Benzyl chloroformate (Aldrich, cat #:119938) (191 mL, 1.34 mol) was slowly added to a cooled (at 0° C.) mixture of ethyl piperidine-3-carboxylate (Aldrich, cat #:194360) (200 g, 1.27 mol) and triethylamine (266 mL, 1.91 mol) in methylene chloride (1000 mL). The reaction mixture was allowed to gradually warm to ambient temperature and stirred for 3 h. The reaction was quenched by the addition of 1N HCl aq. solution and the product was extracted several times with methylene chloride. The combined extracts were washed with water, saturated aq. NaHCO 3 , water, brine, dried over MgSO 4 , filtered and concentrated under reduced pressure to afford the desired product as oil (359.8 g, 97%). LC/MS 292.2 (M+H) + .
Step 2: 1-benzyl 3-ethyl 3-(3-methylbut-2-en-1-yl)piperidine-1,3-dicarboxylate
To a solution of 1-benzyl 3-ethyl piperidine-1,3-dicarboxylate (120.0 g, 0.412 mol) in THF (400 ml) cooled at −78° C. was added dropwise 270 mL of sodium bis(trimethylsilyl)amide solution (1M solution in THF from Aldrich, cat#:245585) over 2 h. The mixture was stirred at −78° C. for additional 1 h. Then 1-bromo-3-methylbut-2-ene (Aldrich cat #: 249904) (71 mL, 0.62 mol) was added slowly over 1 h. The mixture was stirred at −78° C. for 30 min, and allowed to warm to r.t. and stirred for an additional 3 h. The reaction mixture was quenched with 1N HCl aq. solution. Most of THF was removed under reduced pressure. The residue was extracted with ethyl acetate. The combined extracts were washed with sat. aq. NaHCO 3 and brine, then dried over MgSO 4 , filtered and concentrated under reduced pressure. The crude residue was purified by flash column chromatography on a silica gel column with 10˜20% ethyl acetate in hexane to yield the desired product (140 g, 94%). LC/MS: m/e=332.2 (M+H) + .
Step 3: 1-benzyl 3-ethyl 3-(2-oxoethyl)piperidine-1,3-dicarboxylate
Ozone was passed through a solution of 1-benzyl 3-ethyl 3-(3-methylbut-2-en-1-yl)piperidine-1,3-dicarboxylate (35.2 g, 0.0979 mol) in methylene chloride (800 mL) at −78° C. until the color of the solution turned blue. The reaction mixture was then flushed with nitrogen until the blue color dissipated. Dimethylsulfide (Aldrich, cat #: 274380) (14 mL, 0.19 mol) and triethylamine (26.5 mL, 0.19 mol) were added and the mixture was stirred at ambient temperature overnight. The volatile solvent were removed under reduced pressure and purified directly by flash chromatography on a silica gel column with 20% ethyl acetate in hexanes to afford the desired product in quantitative yield. LC/MS 334.2 (M+H) + .
Step 4: Benzyl 2-(cis-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]decane-7-carboxylate
To a suspension of cis-4-aminocyclohexanol hydrochloride (Available from Sijia Medchem Lab, China) (13.8 g, 0.0910 mol) and 1-benzyl 3-ethyl 3-(2-oxoethyl)piperidine-1,3-dicarboxylate (31.0 g, 0.0930 mol) in 1,2-dichloroethane (250 mL) was added triethylamine (23.3 mL, 0.167 mol) at room temperature. The mixture was stirred at 40° C. overnight. Sodium triacetoxyborohydride (Aldrich, cat #: 316393) (49.3 g, 0.232 mol) was added to the above mixture and stirred at r.t. for 1 h. LC/MS data indicated that the starting material was consumed, and an intermediate product with m/e: 433.2 (M+H) + was observed.
The mixture was then heated at 80° C. for 4 h or until LC/MS showed the intermediate amine (m/e: 433.2) was consumed. The reaction mixture was quenched with aq. NaHCO 3 . The organic layer was washed with brine, dried over MgSO 4 , filtered and concentrated under reduced pressure. The crude material was dried under reduced pressure overnight to give colorless viscous oil (26.9 g, 66.8%). LC/MS m/e 387.2 (M+H) + .
Step 5: Benzyl (5S)-2-(cis-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]decane-7-carboxylate
The racemic mixture obtained from above step (26.9 g) was purified on an Agilent 1100 series preparatory system using a Chiralcel OD-H column (3.0×25 cm, 5 micron particle size, Chiral Technologies) eluting with 30% ethanol/hexanes (isocratic, 22 mL/min.). The column loading was approximately 150 mg/injection and peak collection was triggered by UV absorbance at 220 nM. Peak 1 eluted at approximately at 8.5 min. and Peak 2 eluted at approximately 9.8 min. The fractions of Peak 2 were combined and concentrated to provide the desired product (11.9 g) as a white foamy solid. The optical purity of the pooled material from peak 2 was determined by using an Agilent 1100 series analytical system equipped with a Chiralcel OD-H column (4.6×250 mm, 5 micron particle size, Chiral Technologies) and eluting with 30% ethanol/hexanes (isocratic, 0.8 mL/min.). LC/MS m/e 387.2 (M+H) + . The absolute stereochemistry of the peak 2 was established based on X-ray single crystal structure determination of close analogs: Benzyl (5S)-2-(trans-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]decane-7-carboxylate and (5S)-2-(cis-4-{[tert-butyl(dimethyl) silyl]oxy}cyclohexyl)-2,7-diazaspiro[4.5]decan-1-one prepared as described in Steps 5a-c.
Step 5a: Benzyl 2-(cis-4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-1-oxo-2,7-diazaspiro[4.5]decane-7-carboxylate
To a stirred solution of benzyl 2-(cis-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]decane-7-carboxylate (60.00 g, 155.2 mmol) in anhydrous N,N-dimethylformamide (160 mL) at r.t. was added 1H-imidazole (32.0 g, 466 mmol) and tert-butyldimethylsilyl chloride (36.2 g, 233 mmol). The reaction mixture was stirred at r.t. for 4 h, quenched with water (150 mL), and extracted with EtOAc (3×150 mL). The combined organic layers were washed with brine, dried over sodium sulfate, filtered and concentrated under reduced pressure to afford the crude product (84 g). The pure product (55.4 g) was obtained by re-crystallization of the crude product from heptane. The mother liquor was concentrated and subjected to purification by flash chromatography on a silical gel column eluting with AcOEt/Haxane to give additional 14.4 g of the product with a total 89.7% yield.
Step 5b: 2-(cis-4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-2,7-diazaspiro[4.5]decan-1-one
To a solution of benzyl 2-(cis-4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-1-oxo-2,7-diazaspiro[4.5]decane-7-carboxylate (18.0 g, 35.9 mmol) in methanol (150 mL) was added 10% palladium on carbon (Aldrich, cat #: 520888) (1.8 g, 1.5 mmol) under the atmosphere of nitrogen. The reaction mixture was hydrogenated and shaken at 50 psi for 20 h. The reaction mixture was filtered through a pad of Celite and then washed with methanol (300 mL). The filtrate was concentrated under reduced pressure to give the desired product as a white solid in quantitative yield.
Step 5c: (5S)-2-(cis-4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-2,7-diazaspiro[4.5]decan-1-one
2-(cis-4-{[tert-Butyl(dimethyl)silyl]oxy}cyclohexyl)-2,7-diazaspiro[4.5]decan-1-one (7.00 g, 19.1 mmol) was dissolved in acetonitrile (50 mL) and methanol (7 mL) at r.t. After the starting material was completely dissolved, the solution was heated up to 70° C. To the above solution was slowly added a solution of (2R)-hydroxy(phenyl)acetic acid (1.45 g, 9.55 mmol) in acetonitrile (20 mL) at 65-70° C. After addition, the solution was heated at 74° C. for 10 min, and allowed to cool slowly to room temperature overnight. The crystalline formed was collected by filtration to afford 3.38 g of the desired product as (2R)-hydroxy(phenyl)acetic acid salt. The resulting salt (3.38 g) was dissolved in water (50 mL), and adjusted to pH-12 with 40 mL aq K 2 CO 3 solution (2.0 M). The mixture was extracted with dichloromethane (3 times). The combined organic layers were dried with magnesium sulfate, filtered, and concentrated under reduced pressure to afford the desired product as a free base (colorless crystalline solid) (2.37 g). The absolute stereochemistry of this compound was established by X-ray single crystal structure determination of (2R)-hydroxy(phenyl)acetic acid salt of (5S)-2-(cis-4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-2,7-diazaspiro[4.5]decan-1-one.
Step 6: (5S)-2-(cis-4-hydroxycyclohexyl)-2,7-diazaspiro[4.5]decan-1-one
Benzyl (5S)-2-(cis-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]decane-7-carboxylate prepared in Step 5 (0.266 g, 0.000688 mol) was dissolved in methanol (5.0 mL) and stirred under an atmosphere of hydrogen in the presence of 10% palladium on carbon (Aldrich, cat #: 520888) (20.0 mg) at r.t. for 2 h. The reaction mixture was filtered and the volatile solvents were removed under reduced pressure to afford the desired product in quantitative yield. LC/MS m/e 253.2 (M+H) + .
Step 7: (5S)-7-(4-bromo-2-fluorophenyl)-2-(cis-4-hydroxycyclohexyl)-2,7-diazaspiro[4.5]decan-1-one
A mixture of (5S)-2-(cis-4-hydroxycyclohexyl)-2,7-diazaspiro[4.5]decan-1-one (1.04 g, 0.00412 mol), 4-bromo-2-fluoro-1-iodobenzene (Aldrich, cat #: 283304) (1.85 g, 0.00615 mol), copper(I) iodide (Aldrich, cat #: 215554) (0.122 g, 0.000640 mol), potassium phosphate (2.63 g, 0.0124 mol) and 1,2-ethanediol (0.48 mL, 0.0086 mol) in 1-butanol (3.90 mL) was heated at 100° C. under nitrogen for 2 d. The reaction was quenched with water, and extracted with ether. The organic layers were combined, washed with water, brine, dried over Na 2 SO 4 , and filtered. The filtrate was evaporated under reduced pressure. The residue was purified by flash column chromatography on a silica gel column eluting with 0 to 5% methanol in DCM to yield the desired product (950 mg, 54.2%). LC/MS m/e 425.1/427.0 (M+H) + .
Step 8: 5-3-fluoro-4-[(5S)-2-(cis-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]dec-7-yl]phenyl-N-methylpyridine-2-carboxamide
Potassium phosphate (637 mg, 0.00300 mol) in water (3.00 mL) was added to a mixture of (5S)-7-(4-bromo-2-fluorophenyl)-2-(cis-4-hydroxycyclohexyl)-2,7-diazaspiro[4.5]decan-1-one (425 mg, 0.00100 mol), N-methyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine-2-carboxamide (Frontier Inc., cat #: M10074) (393 mg, 0.00150 mol) and tetrakis(triphenylphosphine)palladium (Aldrich, cat #: 216666) (35 mg, 0.000030 mol) in 1,4-dioxane (3.00 mL). The resulting mixture was heated at 120° C. for 24 h. The mixture was diluted with ethyl acetate and washed with water and brine. The organic layer was dried over Na 2 SO 4 , filtered, concentrated under reduced pressure. The residue was purified by flash column chromatography on a silica gel column eluting with 5% methanol in DCM to yield the desired product (285 mg, 59.3%). LC/MS m/e 481.2 (M+H) + . 1 H-NMR (400 MHz, DMSO-d 6 ): 8.89 (1H, dd, J=2.5, 0.6 Hz), 8.76 (1H, q, J=4.7 Hz), 8.22 (1H, dd, J=8.4, 2.5 Hz), 8.03 (1H, dd, J=8.4, 0.6 Hz), 7.65 (1H, dd, J=14.2, 2.1 Hz), 7.56 (1H, dd, J=8.5, 2.1 Hz), 7.13 (1H, t, J=8.5 Hz), 4.37 (1H, d, J=3.1 Hz), 3.78 (1H, m), 3.71 (1H, m), 3.21-3.38 (3H, m), 3.07 (1H, d, J=11.4 Hz), 2.81 (3H, d, J=4.7 Hz), 2.64-2.74 (2H, m), 2.18-2.26 (1H, m), 1.60-1.91 (8H, m), 1.39-1.51 (3H, m), 1.21-1.30 (2H, m).
Example 2
5-{3-Fluoro-4-[(5S)-2-(cis-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]dec-7-yl]phenyl}-N,N-dimethylpyridine-2-carboxamide
Step 1: 5-bromo-N,N-dimethylpyridine-2-carboxamide
Oxalyl chloride (20.0 mL, 0.236 mol) was added to a solution of 5-bromopyridine-2-carboxylic acid (Alfa Aesar, cat #: B25675) (10.1 g, 0.0500 mol) in methylene chloride (60 mL) at r.t. followed by 5 drops of DMF. The mixture was stirred at r.t. for 2 h. The volatiles were evaporated under reduced pressure. The residue was azotropically evaporated with toluene twice. The residue was then dissolved in DCM (30 mL) followed by the addition of 30 mL of dimethylamine in THF solution (2.0 M) (Aldrich, cat #: 391956) and Hunig's base (20.0 mL) (Aldrich, cat #: 496219). The mixture was stirred at r.t. for 3 h. The reaction mixture was diluted with DCM (100 mL) and washed with water, 1N HCl and brine. The organic phase was dried over Na 2 SO 4 , filtered and concentrated to give the desired product (10.5 g, 91.7%).
Step 2: N,N-dimethyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine-2-carboxamide
A mixture of 5-bromo-N,N-dimethylpyridine-2-carboxamide (5.73 g, 0.0250 mol), 4,4,5,5,4′,4′,5′,5′-octamethyl-[2,2′]bi[[1,3,2]dioxaborolanyl] (6.98 g, 0.0275 mol) (Aldrich, cat #: 473294), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) complexed with dichloromethane (1:1) (0.6 g, 0.0007 mol) (Aldrich, cat #: 379670), 1,1′-bis(diphenylphosphino)ferrocene (0.4 g, 0.8 mmol) (Aldrich, cat #: 177261), and potassium acetate (7.36 g, 0.0750 mol) in 1,4-dioxane (100 mL) was heated at 120° C. for 20 h. After cooling, the mixture was concentrated, diluted with ethyl acetate and washed with sat′d NH 4 Cl solution, water, brine; dried over Na 2 SO 4 . After filtration, the filtrate was concentrated and the crude material was further purified on a silica gel column eluting with ethyl acetate/hexane to give the desired product (4.7 g, 68%).
Step 3: 5-{3-Fluoro-4-[(5S)-2-(cis-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]dec-7-yl]phenyl}-N,N-dimethylpyridine-2-carboxamide
This compound was prepared by using procedures that were analogous to those described for the synthesis of Example 1, Step 8 starting from N,N-dimethyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine-2-carboxamide and (5S)-7-(4-bromo-2-fluorophenyl)-2-(cis-4-hydroxycyclohexyl)-2,7-diazaspiro[4.5]decan-1-one. LC/MS m/e 495.3 (M+H) + . 1 H-NMR (400 MHz, DMSO-d 6 ): 8.86 (1H, d, J=1.7 Hz), 8.15 (1H, dd, J=8.1, 2.3 Hz), 7.51-7.65 (3H, m), 7.12 (1H, t, J=8.9 Hz), 4.37 (1H, d, J=3.1 Hz), 3.78 (1H, m), 3.71 (1H, m), 3.22-3.38 (3H, m), 3.06 (1H, d, J=11.7 Hz), 3.00 (3H, s), 2.97 (3H, s), 2.64-2.74 (2H, m), 2.18-2.27 (1H, m), 1.60-1.91 (8H, m), 1.39-1.51 (3H, m), 1.22-1.30 (2H, m).
Example 3
N-Ethyl-5-{3-fluoro-4-[(5S)-2-(cis-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]dec-7-yl]phenyl}pyridine-2-carboxamide
Step 1: N-ethyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine-2-carboxamide
This compound was prepared by using procedures that were analogous to those described for the synthesis of Example 2, Steps 1 & 2 starting from 5-bromopyridine-2-carboxylic acid.
Step 2: N-Ethyl-5-{3-fluoro-4-[(5S)-2-(cis-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]dec-7-yl]phenyl}pyridine-2-carboxamide
This compound was prepared by using procedures that were analogous to those described for the synthesis of Example 1, Step 8 starting from N-ethyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine-2-carboxamide and (5S)-7-(4-bromo-2-fluorophenyl)-2-(cis-4-hydroxycyclohexyl)-2,7-diazaspiro[4.5]decan-1-on. LC/MS m/e 495.3 (M+H) + .
Example 4
5-{3-Chloro-4-[(5S)-2-(cis-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]dec-7-yl]phenyl}-N-ethylpyridine-2-carboxamide
Step 1: (5S)-7-(4-bromo-2-chlorophenyl)-2-(cis-4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-2,7-diazaspiro[4.5]decan-1-one
A mixture of (5S)-2-(cis-4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-2,7-diazaspiro[4.5]decan-1-one (0.282 g, 0.000769 mol), 4-bromo-2-chloro-1-iodobenzene (0.293 g, 0.000922 mol) (Lancaster, cat #: 19245), copper(I) iodide (0.015 g, 0.000077 mol), potassium phosphate (0.490 g, 0.00231 mol) and 1,2-ethanediol (0.0857 mL, 0.00154 mol) in 1-butanol (0.75 mL) was heated at 100° C. under nitrogen for 2 d. The reaction mixture was filtered, concentrated under reduced pressure, and the residue was purified by flash chromatography on a silica gel column (eluting with 0 to 50% ethyl acetate in hexanes) to afford the desired product.
Step 2: 5-{3-chloro-4-[(5S)-2-(cis-4-hydroxycyclohexyl)-1-oxo-2,7-diazaspiro[4.5]dec-7-yl]phenyl}-N-ethylpyridine-2-carboxamide
To a stirred mixture of (5S)-7-(4-bromo-2-chlorophenyl)-2-(cis-4-{[tert-butyl(dimethyl)silyl]oxy}cyclohexyl)-2,7-diazaspiro[4.5]decan-1-one (20 mg, 0.00004 mol), [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) complex with dichloromethane (1:1) (2.0 mg), tetrakis(triphenylphosphine)palladium (1.0 mg) and potassium carbonate (14.9 mg, 0.000108 mol) in anhydrous N,N-dimethylformamide (1 mL) was added N-ethyl-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine-2-carboxamide (14.5 mg, 0.054 mmol). The resulting reaction mixture was heated at 150° C. and stirred overnight, followed by the removal of TBS protecting group by the addition of 1.7 M of fluorosilicic acid in water (0.10 mL) and the mixture was stirred at r.t. overnight. The reaction mixture was then directly purified by RP-HPLC to afford the desired product. LC/MS m/e 511.2 (M+H) + . 1 H-NMR (400 MHz, DMSO-d 6 ): 8.92 (1H, d, J=2.3 Hz), 8.84 (1H, t, J=5.9 Hz), 8.26 (1H, dd, J=8.2, 2.3 Hz), 8.06 (1H, d, J=8.2 Hz), 7.89 (1H, d, J=2.2 Hz), 7.74 (1H, dd, J=8.5, 2.2 Hz), 7.30 (1H, t, J=8.5 Hz), 4.39 (1H, d, J=3.1 Hz), 3.80 (1H, m), 3.72 (1H, m), 3.24-3.44 (5H, m), 3.01 (1H, d, J=11.4 Hz), 2.63-2.74 (2H, m), 2.40-2.53 (1H, m), 1.64-1.91 (8H, m), 1.41-1.53 (3H, m), 1.20-1.32 (2H, m), 1.13 (3H, t, J=7.2 Hz).
Example 5
Enzymatic Assay of 11βHSD1
All in vitro assays were performed with clarified lysates as the source of 11βHSD1 activity. HEK-293 transient transfectants expressing an epitope-tagged version of full-length human 11βHSD1 were harvested by centrifugation. Roughly 2×10 7 cells were resuspended in 40 mL of lysis buffer (25 mM Tris-HCl, pH 7.5, 0.1 M NaCl, 1 mM MgCl 2 and 250 mM sucrose) and lysed in a microfluidizer. Lysates were clarified by centrifugation and the supernatants were aliquoted and frozen.
Inhibition of 11βHSD1 by test compounds was assessed in vitro by a Scintillation Proximity Assay (SPA). Dry test compounds were dissolved at 5 mM in DMSO. These were diluted in DMSO to suitable concentrations for the SPA assay. 0.8 μL of 2-fold serial dilutions of compounds were dotted on 384 well plates in DMSO such that 3 logs of compound concentration were covered. 20 μL of clarified lysate was added to each well. Reactions were initiated by addition of 20 μL of substrate-cofactor mix in assay buffer (25 mM Tris-HCl, pH 7.5, 0.1 M NaCl, 1 mM MgCl 2 ) to final concentrations of 400 μM NADPH, 25 nM 3 H-cortisone and 0.007% Triton X-100. Plates were incubated at 37° C. for one hour. Reactions were quenched by addition of 40 μL of anti-mouse coated SPA beads that had been pre-incubated with 10 μM carbenoxolone and a cortisol-specific monoclonal antibody. Quenched plates were incubated for a minimum of 30 minutes at RT prior to reading on a Topcount scintillation counter. Controls with no lysate, inhibited lysate, and with no mAb were run routinely. Roughly 30% of input cortisone is reduced by 11βHSD1 in the uninhibited reaction under these conditions.
Example 6
Cell-Based Assay for 11βHSD1 Activity
Peripheral blood mononuclear cells (PBMCs) were isolated from normal human volunteers by Ficoll density centrifugation. Cells were plated at 4×10 5 cells/well in 200 μL of AIM V (Gibco-BRL) media in 96 well plates. The cells were stimulated overnight with 50 ng/ml recombinant human IL-4 (R&D Systems). The following morning, 200 nM cortisone (Sigma) was added in the presence or absence of various concentrations of compound. The cells were incubated for 48 hours and then supernatants were harvested. Conversion of cortisone to cortisol was determined by a commercially available ELISA (Assay Design).
Various modifications of the invention, in addition to those described herein, will be apparent to those skilled in the art from the foregoing description. Such modifications are also intended to fall within the scope of the appended claims. Each reference, including all patent, patent applications, and publications, cited in the present application is incorporated herein by reference in its entirety.
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The present invention relates to certain spirocyclic compounds that are inhibitors of 11-β hydroxyl steroid dehydrogenase type 1 (11βHSD1), compositions containing the same, and methods of using the same for the treatment of diabetes, obesity and other diseases.
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RIGHTS OF THE GOVERNMENT
The invention described herein may be manufactured and used by or for the Government of the United States for all governmental purposes without the payment of any royalty.
BACKGROUND OF THE INVENTION
This invention relates to the processing of titanium alloy articles fabricated by powder metallurgy to improve the microstructure of such articles.
Titanium alloy parts are ideally suited for advanced aerospace systems because of their excellent general corrosion resistance and their unique high specific strength (strength-to-density ratio) at room temperature and at moderately elevated temperatures. Despite these attractive features, the use of titanium alloys in engines and airframes is often limited by cost due, at least in part, to the difficulty associated with forging and machining titanium.
To circumvent the high cost of titanium alloy parts, several methods of making parts to near-net shape have been developed to eliminate or minimize forging and/or machining. These methods include superplastic forming, isothermal forging, diffusion bonding, investment casting and powder metallurgy, each having advantages and disadvantages.
Until relatively recently, the primary motivation for using the powder metallurgy approach for titanium was to reduce cost. In general terms, powder metallurgy involves powder production followed by compaction of the powder to produce a solid article. The small, homogeneous powder particles provide a uniformly fine microstructure in the final product. If the final article is made net-shape by the application of Hot Isostatic Pressing (HIP), a lack of texture can result, thus giving equal properties in all directions. The HIP process has been practiced within a relatively broad temperature range, for example, about 700° to 1200° C. (1300°-2200° F.), depending upon the alloy being treated, and within a relatively broad pressure range, for example, 1 to 30 ksi, generally about 15 ksi.
In U.S. Pat. Nos. 4,534,808 and 4,536,234 we disclose methods for refining the microstructures of as-produced net-shape titanium articles made by powder metallurgy for the purpose of improving mechanical properties, such as tensile and fatigue strengths. Briefly, these methods comprise beta-solution heat treating the article, rapidly cooling the article, and annealing the article at a temperature below the beta-transus temperature. We have now discovered a method for producing articles by powder metallurgy which affords closer control of the microstructure of the final article.
Accordingly, it is an object of the present invention to provide a process for producing articles having a desired microstructure by powder metallurgy of titanium alloys.
Other objects, aspects and advantages of the present invention will be apparent to those skilled in the art after reading the detailed description of the invention as well as the appended claims.
SUMMARY OF THE INVENTION
In accordance with the present invention there is provided a process for producing titanium alloy articles having a desired microstructure which comprises the steps of:
(a) providing prealloyed titanium alloy powder;
(b) filling a suitable die or mold with the powder;
(c) hot isostatic press (HIP) consolidating the powder in the filled mold at a pressure of 30 Ksi or greater and at a temperature of about 60 to 80 percent of the beta transus temperature of the alloy, in degrees C.
Optionally, following the hot isostatic pressing step, the article may be heat treated to alter its microstructure.
BRIEF DESCRIPTION OF THE DRAWING
In the drawing,
FIGS. 1-4 are 600× photomicrographs illustrating the fine microstructures of Ti-6Al-4V and Ti-10V-2Fe-3Al alloys compacted according to the invention;
FIGS. 5-10 are 600× photomicrographs of Ti-6Al-4V powder compacts prepared according to the invention, then heat treated according to the invention, then heat treated under various conditions; and
FIGS. 11-14 are 600× photomicrographs of Ti-10V-2Fe-3Al powder compacts prepared according to the invention, then heat treated under various conditions.
DETAILED DESCRIPTION OF THE INVENTION
The alloy to be used in this invention can be any titanium alloy. Typical alloys include the following:
Alpha and Near-Alpha Alloys:
Ti-0.8Ni-0.8Mo
Ti-5Al-2.5Sn
Ti-8Al-1Mo-1V
Ti-6Al-2Sn-4Zr-2Mo-0.1Si
Ti-6Al-2Nb-1Ta-0.8Mo
Ti-2.25Al-11Sn-5Zr-1Mo
Alpha-Beta Alloys:
Ti-6Al-4b
Ti-6Al-6V-2Sn
Ti-8Mn
Ti-7Al-4Mo
Ti-4.5Al-5Mo-1.5Cr
Ti-6Al-2Sn-4Zr-6Mo
Ti-5Al-2Sn-2Zr-4Mo-4Cr
Ti-6Al-2Sn-2Zr-2Mo-2Cr
Ti-3Al-2.5V
Beta Alloys:
Ti-13V-11Cr-3Al
Ti-8Mo-8V-2Fe-3Al
Ti-3Al-8V-6Cr-4Mo-4Zr
Ti-10V-2Fe-3Al
Ti-11.5Mo-6Zr-4.5Sn
Ti-15V-3Cr-3Al-3Sn
The alloy may further contain up to about 6 w/percent of a dispersoid such as boron, thorium or a rare earth element.
For production of high quality, near-net titanium shapes according to the invention, spherical powder free of detrimental foreign particles is desired. In contrast to flake or angular particles, spherical powder flows readily, with minimal bridging tendency, and packs to a consistent density (about 65%).
A variety of techniques may be employed to make the titanium alloy powder, including the rotating electrode process (REP) and variants thereof such as melting by plasma arc (PREP) or laser (LREP) or electron beam, electron beam rotating disc (EBID), powder under vacuum (PSV), and the like. These techniques typically exhibit cooling rates of about 100° to 100,000° C./sec. The powder typically has a diameter of about 25 to 600 microns. Optionally, prior to use in the present invention, the titanium alloy powder can be worked to promote better metallurgical bonding. The strain energizing process (SEP), which involves working the powder particles by deforming them in a rolling mill, increases the aspect ratio of the powder. Additionally, this process permits the alpha morphology of the powder to be modified for fatigue strength enhancement.
Production of shapes may be accomplished using a metal can, ceramic mold or fluid die technique. In the metal can technique, a metal can is shaped to the desired configuration by state-of-the-art sheet-metal methods, e.g. brake bending, press forming, spinning, superplastic forming, etc. The most satisfactory container appears to be carbon steel, which reacts minimally with the titanium, forming titanium carbide which then inhibits further reactions. Fairly complex shapes have been produced by this technique.
The ceramic mold process relies basically on the technology developed by the investment casting industry, in that molds are prepared by the lost-wax process. In this process, wax patterns are prepared as shapes intentionally larger than the final configuration. This is necessary since in powder metallurgy a large volume difference occurs in going from the wax pattern (which subsequently becomes the mold) and the consolidated compact. Knowing the configuration aimed for in the compacted shape, allowances can be made using the packing density of the powder to define the required wax-pattern shape.
The fluid die or rapid omnidirectional consolidation (ROC) process is an outgrowth of work on glass containers. In the current process, dies are machined or cast from a range of carbon steels or made from ceramic materials. The dies are of sufficient mass and dimensions to behave as a viscous liquid under pressure at temperature when contained in an outer, more rigid pot die, if necessary. The fluid dies are typically made in two halves, with inserts where necessary to simplify manufacture. The two halves are then joined together to form a hermetic seal. Powder loading, evacuation and consolidation then follow. The fluid die process is claimed to combine the ruggedness and fabricability of metal with the flow characteristics of glass to generate a replicating container capable of producing extremely complex shapes.
In the metal can and ceramic mold processes, the powder-filled mold is supported in a secondary pressing medium contained in a collapsible vessel, e.g., a welded metal can. Following evacuation and elevated-temperature outgassing, the vessel is sealed, then placed in an autoclave or other apparatus capable of isostatically compressing the vessel.
Consolidation of the titanium alloy powder is accomplished by applying a pressure of at least 30 ksi, preferably at least about 35 ksi, at a temperature of about 60 to 80 percent of the beta transus temperature of the alloy (in degrees C.) for about 4 to 48 hours. It will be recognized by those skilled in the art that the practical maximum applied pressure is limited by the apparatus employed.
Following consolidation, the compacted article is recovered, using techniques known in the art. The resulting article is fully dense and has a very fine microstructure. The microstructure of the compacted article can be subsequently altered by annealing, beta-solution heat treatment or a combination thereof.
Annealing is typically carried out at a temperature about 15 to 30% below the beta-transus temperature (in °C.) of the alloy for about 2 to 36 hours in a vacuum or inert atmosphere to protect the surface of the article from oxidation, followed by air or furnace cooling to room temperature. For example, annealing of Ti-6Al-4V alloy, which has a beta-transus of about 1000° C., is typically carried out between 700° and 850° C.
Beta-solution heat treatment may be carried out by heating the article to approximately the beta-transus temperature of the alloy, i.e., about 5% below to about 10% above the beta-transus temperature (in °C., for about 10 to 240 minutes, followed by rapid cooling. Cooling may be accomplished by quenching the article in a suitable liquid quenching medium, such as water or oil.
The following example illustrates the invention.
EXAMPLE
-35 mesh Ti-6Al-4V (Ti-6-4) and Ti-10V-2Fe-3Al (Ti-10-2-3) powders prepared by the rotating electrode process (REP) and the plasma rotating electrode process (PREP), respectively, were employed. One-half of each batch of powder was used in the as-produced condition and one-half was subjected to the strain energing process (SEP), using a double pass reduction (60%).
Compaction of the above powders was performed in a 45 ksi (315 MPa) autoclave with a workspace of 140 mm (5.6 inch) diameter×280 mm (11.2 inch) length. The powders were filled into welded mold steel cans. The final compact dimension after removal of the can was 50 mm (2.0 inch) diameter×180 mm (3.2 inch) long. The consolidation conditions are given in Table I, following.
TABLE I______________________________________Compaction Conditions Consolidation Powder Temp Press.Desig. Alloy Treat. °C. ksi Time, hr.______________________________________HPLT1 Ti-6-4 -- 650 45 24HPLT2 Ti-6-4 SEP 595 45 24HPLT3 Ti-10-2-3 -- 595 45 24HPLT4 Ti-10-2-3 SEP 540 45 24______________________________________
Specimens of each of the compacts were heat treated in accordance with the schedule shown in Table II. Room temperature tensile tests were performed on the as-compacted specimens and the heat-treated specimens. Due to the small dimensions of the material available, tensile tests were conducted on subsize smooth bar specimens 2.5 mm (0.1 inch) gage diameter×17.5 mm (0.7 inch) gage length. Tensile test strain rate was maintained at 0.005 mm/mm/min through the 0.2% yield point followed by 1.25 mm/min cross head speed to failure.
TABLE II______________________________________Tensile Results Heat Treatment, % YS ELDesig. °C./hr/m* (ksi) UTS (ksi) (%) RA (%)______________________________________HPLT1 None 157 164 8 19 815/24/AC 136 147 22 38HPLT2 None -- 149 0.2 0 705/2/FC -- 150 0 1 705/24/FC 153 155 1 5 815/2/FC 160 163 1 4 815/24/FC 144 160 7 17 955/2/FC 140 149 8 26HPLT3 None 138 144 14 49 760/1/WQ + 178 188 3 6 510/8/AC 760/3/AC + -- 210 1 4 370/4/AC 790/3/AC + 212 227 1 1 370/4/ACHPLT4 None 145 146 1 3 750/1/WQ + 166 169 1 2 550/8/AC 760/1/WQ + -- 159 0 0 510/8/AC______________________________________ *m = cooling technique: AC = air cool FC = furnace cool WQ = water quench
Examination of the above data indicates that the Ti-6-4 compacted at 595° C. (HPLT2) and the Ti-10-2-3 compacted at 540° C. (HPLT4) displayed almost no elongation in the as-compacted/non-heat-treated condition. Microscopic examination of these specimens revealed particle debonding, including flat debonded particle boundaries, believed to result from SEP'ing the powders. In contrast, the specimens compacted at higher temperatures (Ti-6-4 at 650° C. (HPLT1) and Ti-10-2-3 at 595° C. (HPLT3)) displayed adequate elongation.
The as-compacted microstructure of HPLT1 through HPLT4 are shown in FIGS. 1-4, respectively. The microstructures of all four compacts are very fine due to the low compaction temperatures which did not allow much coarsening of the fine powder particle microstructure. The microstructure of HPLT1 and HPLT2 (FIGS. 1 and 2) consist of a very fine alpha phase. Part of the fine alpha phase has a lenticular morphology, similar to the microstructure of the as-produced powder particles, and part is equiaxed (1-2 microns) in a matrix of beta.
The as-produced Ti-10-2-3 powder particles have a columnar beta structure at the particle surface, the result of a high cooling rate. This microstructure degenerates into a beta dendritic structure, the result of slower cooling rates inside the particle. Referring to FIGS. 3 and 4, in the as-compacted Ti-10-2-3 (HPLT3 and HPLT4, respectively), micron size alpha precipitation is visible. In some regions, such as in the upper part of FIG. 3, traces of the columnar structure are still visible.
The results of recrystallization of the HPLT2 and HPLT4 compacts are shown in FIGS. 5-10 and FIGS. 11-14, respectively. The recrystallization conditions are given in Table III.
TABLE III______________________________________RecrystallizationFIGS. Desig Condition °C./hr/cooling method______________________________________ 5 HPLT2 705/2/FC 6 HPLT2 705/24/FC 7 HPLT2 815/2/FC 8 HPLT2 760/24/FC 9 HPLT2 815/24/FC10 HPLT2 955/2/FC11 HPLT4 750/1/WQ + 550/8/AC12 HPLT4 760/1/WQ + 510/8/AC13 HPLT4 760/3/AC + 370/4/AC14 HPLT4 790/3/AC + 370/4/AC______________________________________
The amount of recrystallization is shown in FIGS. 5-10 in increasing order. Full recrystallization is achieved both at 955/2 and 815/24. Examination of Table II reveals that only under these two conditions was tensile elongation of the compact restored.
With reference to FIGS. 11-14, the beta solution heat treatments followed by 370° C. aging generally resulted in microstructures with almost no alpha precipitates, or with precipitates too small to be resolved at an optical level (FIGS. 13, 14). However, solution treatment followed by 550° C. and 510° C. again (FIGS. 11 and 12) resulted in microstructures with micron size globular and elongated alpha precipitates. Examination of Table II reveals that these heat treatments resulted in a substantial increase in strength (From 144 to 227 ksi) with a loss of tensile elongation (from 14% to 1%).
Various modifications may be made in the present invention without departing from the spirit of the invention or the scope of the appended claims.
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A process for producing titanium alloy articles by Hot Isostatic Pressing of a rapidly-solidified titanium alloy powder is provided wherein such pressing is carried out at a pressure greater than 30 ksi, and a temperature of about 60 to 80 percent of the beta-transus temperature of the alloy, in degrees C. Hot Isostatic Pressing under these conditions allows retention of the fine microstructure of the rapidly-solidified powder. The compacted article may be subjected to heat treatment to alter its microstructure.
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TECHNICAL FIELD
[0001] The present invention relates to the field of thermal machines. It relates in particular to a cooled flow deflection apparatus for a fluid-flow machine which operates at high temperatures, as claimed in the precharacterizing clause of claim 1 .
[0002] Such a flow deflection apparatus is generally known from the prior art, for example in the form of a cooled stator blade or rotor blade for a gas turbine.
PRIOR ART
[0003] Present-day flow deflection apparatuses, especially stator blades or rotor blades in a gas turbine, are subjected to ambient temperatures which are above the maximum permissible material temperature. The use of special internal cooling channels allows the metal temperature to be reduced to a level which is required on the basis of the life of the apparatus.
[0004] [0004]FIGS. 1 and 2 respectively show a cross section and longitudinal section of an example of a rotor blade of a gas turbine, as is currently used. The blade 10 essentially comprises a blade airfoil section 11 and a blade root 12 , by means of which it is attached to the rotor of the gas turbine. A number of cooling channels 17 run in the longitudinal direction of the blade 10 in the interior of the (hollow) blade airfoil section 11 , through which cooling channels 17 a cooling fluid, generally cooling air which enters through the blade root 12 , flows. The cooling fluid runs, with a cooling effect, in the cooling channels 17 along the insides of the hot-gas walls 14 and then (for film cooling) emerges to the outside through appropriate film-cooling openings which are arranged on the leading edge 18 , on the trailing edge 19 and at the blade tip (the emerging cooling fluid is indicated by the arrows in FIG. 2). The individual cooling channels 17 are separated from one another by separating walls 13 which at the same time have deflection devices 16 to ensure that the cooling fluid flows successively through adjacent cooling channels in alternately opposite directions.
[0005] Until now, and in this case specifically in the case of rotating guide apparatuses such as rotor blades, the cooling channels 17 and their separating walls 13 have been cast.
[0006] The known, cast separating walls 13 and deflection devices 16 , which are also referred to as ribs, have a number of disadvantages, however:
[0007] The transitional region ( 15 in FIG. 1) from the hot-gas wall 14 to the separating wall (rib) 13 is an area which is difficult to cool owing to the large amount of material in that area. Increased heat transfer together with increased cooling-air consumption is required in order to ensure adequate strength there.
[0008] The cold separating walls (ribs) 13 , around which the cooling air flows, lead to thermal stresses with the hot-gas wall 14 .
[0009] Casting of the internal channels leads to a high blade weight, which can lead to high centrifugal-force stresses both for the blade root 12 and for the blade airfoil section 11 .
[0010] The complex casting lengthens casting development and increases the amount of scrap.
DESCRIPTION OF THE INVENTION
[0011] The object of the invention is thus to provide a cooled flow deflection apparatus which avoids the described disadvantages of the known apparatus and in particular is simple to produce, can be flexibly matched to the respective application, and is efficiently cooled.
[0012] The object is achieved by the totality of features of claim 1 . The essence of the invention is no longer to produce, in particular to cast, the separating walls, which are used to bound the cooling channels, jointly with the apparatus, but to construct them as separate inserts which are subsequently inserted into the apparatus, and are secured there. The invention is thus considerably different to solutions such as those described in U.S. Pat. No. 5,145,315 or U.S. Pat. No. 5,516,260, in which specific inserts in cast cooling channels are used for specific guidance of the cooling fluid.
[0013] The use of inserts (for example, in the case of blades, inserted through the blade root or through the blade tip) composed of metal or non-metal materials as a substitute for cast separating walls and, possibly, deflection devices, has a number of advantages:
[0014] There is no large amount of material in the transitional region from the hot-gas wall to the insert (to the separating wall).
[0015] There are no thermal stresses between the insert (separating wall) and the hot-gas wall.
[0016] In the case of rotating blades, the blade weight and thus the centrifugal-force stresses are reduced both in the blade root and in the blade airfoil section.
[0017] In the case of cast blades, the cast core is simpler, as a result of which both its capability to be produced and that of the blade are simpler.
[0018] The cooling system can easily be adjusted by replacing the inserts, for example by varying the deflection radius of deflection devices or by introducing connecting cross sections between two cooling channels.
[0019] A first preferred embodiment of the flow deflection apparatus according to the invention is characterized in that the flow deflection apparatus is in the form of a hollow casting, and in that holders, which are in the form of rails and into which the separating walls are inserted, are integrally formed in the interior of the flow deflection apparatus. This considerably simplifies assembly and attachment of the inserts, and ensures that the separating walls or inserts are sealed well at the edges. The separating walls are in this case preferably flat strips composed of a metallic or heat-resistant non-metallic (ceramic or composite) material.
[0020] A secure seating for the inserts is achieved if, according to a second preferred embodiment of the invention, the inserted separating walls are, for security, connected by an integral material joint, preferably by soldering or welding, to the flow deflection apparatus.
[0021] In the simplest form, the separating walls may be straight.
[0022] It is particularly simple and advantageous if, according to another embodiment, the cooling fluid flows in mutually opposite directions in two adjacent cooling channels, if the cooling fluid is deflected from the outlet of the one cooling channel into the inlet of the other cooling channel by means of a deflection device, and if the deflection is produced by a separating wall which is bent into a U-shape.
[0023] One particularly preferred embodiment of the flow deflection apparatus according to the invention is characterized in that the flow deflection apparatus is a blade in a gas turbine. Owing to the comparatively complex geometry of the blade, the invention in this case results in considerable simplifications.
[0024] Another embodiment, which is particularly advantageous for rotor blades which rotate at high speed, is characterized in that the cooling channels and separating walls extend essentially in the radial direction with respect to the rotation axis of the gas turbine, in that the inserted separating walls are, for security, connected by an integral material joint, preferably by soldering or welding, to the blade, and in that the integral material joint is arranged at the end of the separating walls close to the axis.
BRIEF DESCRIPTION OF THE FIGURES
[0025] The invention will be explained in more detail in the following text with reference to exemplary embodiments and in conjunction with the drawing, in which:
[0026] [0026]FIG. 1 shows the cross section through a turbine blade having cast cooling channels according to the prior art;
[0027] [0027]FIG. 2 shows a longitudinal section through the blade shown in FIG. 1;
[0028] [0028]FIG. 3 shows a cross section, comparable to that in FIG. 1, through a blade according to one exemplary embodiment of the invention; and
[0029] [0029]FIG. 4 shows a longitudinal section, comparable to that in FIG. 2, through the blade shown in FIG. 3.
APPROACHES TO IMPLEMENTATION OF THE INVENTION
[0030] [0030]FIGS. 3 and 4 respectively show a cross section and longitudinal section of an exemplary embodiment of a cooled flow deflection apparatus according to the invention in the form of a rotor blade for a gas turbine. The geometry of the blade 20 is similar to that of the known blade 10 shown in FIGS. 1 and 2.
[0031] Once again, the blade 20 essentially comprises a blade airfoil section 21 and a blade root 22 , by means of which it is attached to the rotor of the gas turbine. A number of cooling channels 27 , through which a cooling fluid which enters through the blade root 22 flows, run in the longitudinal direction of the blade 20 , in the interior of the (hollow) blade airfoil section 21 . The cooling fluid runs in cooling channels 27 along the insides of the hot-gas walls 24 , with a cooling effect, and in this case as well emerges to the outside through appropriate film cooling openings which are arranged on the leading edge 28 , on the trailing edge 29 , and at the blade tip. The individual cooling channels 27 are separated from one another by separating walls 23 which at the same time have deflection devices 26 to ensure that the cooling fluid flows successively through adjacent cooling channels in alternately opposite directions.
[0032] In contrast to FIGS. 1 and 2, the separating walls 23 are in this case not cast, however, that is to say produced together with the blade 20 in one casting process, but are separate inserts, in the form of strips, which, once the blade 20 has been cast, are introduced through the blade root 22 or through the opposite blade tip. In order to allow the separating walls 23 to be inserted as required and to be secured after insertion, holders 30 which are in the form of rails and in which the longitudinal edges of the separating walls 23 are guided during insertion are integrally formed on the insides of the hot-gas walls.
[0033] The separating walls (inserts) 23 may have any desired shape. For example, they may be straight. If a number of cooling channels are intended to be connected to one another by means of deflection devices 26 , it is advantageous for the separating walls 23 to be bent into a U-shape. The separating walls 23 can be secured on one or more sides, for example by soldering or welding. They may be fixed in the blade tip region or in the blade root region. The latter has the advantage that the centrifugal forces which occur load the insert or the separating wall in tension, thus preventing them from bulging out.
[0034] In principle, the separating walls which can be inserted are provided at the same time that the blades are produced. However, it is also feasible within the scope of the invention for the cast separating walls subsequently to be removed from completely cast blades as shown in FIGS. 1 and 2 and for separate separating walls to be inserted and to be secured as a substitute for them.
LIST OF REFERENCE SYMBOLS
[0035] [0035] 10 , 20 Blade
[0036] [0036] 11 , 21 Blade airfoil section
[0037] [0037] 12 , 22 Blade root
[0038] [0038] 13 Separating wall (rib)
[0039] [0039] 14 , 24 Hot-gas wall
[0040] [0040] 15 , 25 Transitional region
[0041] [0041] 16 , 26 Deflection device
[0042] [0042] 17 , 27 Cooling channel
[0043] [0043] 18 , 28 Leading edge
[0044] [0044] 19 , 29 Trailing edge
[0045] [0045] 23 Insert
[0046] [0046] 30 Holder (in the form of a rail)
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Apparatus is disclosed for providing cooling channels in the interior of a gas turbine rotor blade. The cooling channels are formed by metallic inserts which extend from adjacent the root of the blade toward the tip. The inserts are substantially flat and are secured in the interior of the airfoil section by means of rails which engage the longitudinal edges of the inserts and serve as a guide during insertion. The rails are preferable formed integrally with the blade casting.
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RELATED APPLICATIONS
[0001] This application claims the benefit of European Application No. 08150005.0, filed Jan. 2, 2008, the entire disclosure of which is herein incorporated by reference.
TECHNICAL FIELD
[0002] The present invention is directed to a polymer blend formulation and to heat shrinkable film, bags, pouches and the like made therefrom. The invention is further directed to a method of producing a heat shrinkable film with the proper gas permeability properties so that it is ideal for packaging and preservation of gassing cheese.
BACKGROUND
[0003] Gassing cheese products are generally characterized by the emission of carbon dioxide during their curing process. Packaging films used for packaging of such cheese must be able to allow carbon dioxide escape, so that a possible “ballooning” effect is avoided. At the same time, oxygen permeability should be as low as possible, so that the oxidation-deterioration of the cheese is minimized.
[0004] Heat shrinkable films are often used for gassing cheese packaging due to the good aesthetic appearance that heat shrinkability induces. High transparency of the pack is also important, so that possible consumers are attracted by the pack. The majority of heat shrinkable films used in this area comprise PVDC as barrier layer. PVDC is difficult to extrude and quite easy to burn and deteriorate during the extrusion process.
[0005] PVDC formulations like for example described in prior art patents are commonly used.
[0006] Generally these PVDC formulations incorporate high percentage of plasticizers or stabilizers in order to increase the permeability to CO2. Common plasticizers/stabilizers are epoxidized compounds like epoxidized soybean oil, epoxidized linseed oil, etc. One negative effect is that these compounds tend to migrate from the PVDC layer to other layers, thus creating delaminations and, most dangerously, change of barrier properties as time passes. This is an undesirable phenomenon.
[0007] So, several features that should characterize a heat shrinkable film intended for use in packaging of gassing cheese are
[0000] 1. High shrinkage
2. Excellent optics
3. Efficient heat sealability so that bags can be made
4. Avoidance of plasticizer use
5. Good processability of PVDC, no oxidation during extrusion
6. High CO2 permeability, not changing over time
7. High O2 barrier, not changing over time.
[0008] These features are matched with the PVDC combination of the present invention and with the heat shrinkable films we further advice.
SUMMARY OF THE INVENTION
[0009] It is therefore the object of this invention to make a polymer blend providing the above characteristics.
[0010] This is solved by a polymer blend comprising
A. PVDC polymer B. Ethylene vinyl acetate with more than 40% vinyl acetate (per weight) C. PVC D. Epoxidized oil compound and optionally other additives.
[0015] For example, the invention comprises a PVDC combination with the following recipe:
Blend of
[0000]
a copolymer PVDC as base resin
epoxidized materials less than 2% per weight
ethylene vinyl acetate copolymer with percentage of 40 to 50% vinyl acetate per weight
PVC content more than 0% and less than 2%
silica and talc
possibly other materials like silicon polymers, high density polyethylene, tetrasodium pyrophospthate
[0022] It is further the object of this invention to extrude the above described PVDC formulation without deterioration even in high shear rates.
[0023] It is further the object of this invention to produce a multilayer film incorporating a PVDC layer comprising the above described recipe. The other layers may preferably comprise ethylene alpha olefin copolymers, propylene alpha olefin copolymers, propylene ethylene copolymers, styrene polymers or ionomers.
THE DEFINITIONS USED IN THE FOLLOWING ARE AS FOLLOWS
[0024] The term “film” refers to a flat or tubular flexible structure of thermoplastic material.
[0025] The term “heat shrinkable” refers to a film that shrinks at least 10% in at least one of the longitudinal and transverse directions when heated at 90° C. for 4 seconds. The shrinkability is measured according to ASTM 2732 with water as a heating medium. This test method covers the determination of the degree of unrestrained linear thermal shrinkage at given specimen temperatures of a plastic film and sheeting of 0.76 mm thickness or less.
[0026] All measurement methods mentioned herein are readily available for the skilled person. For example, they can be obtained from the American National Standards Institute at: www.webstore.ansi.org
[0027] The phrase “longitudinal direction” or “machine direction” herein abbreviated “MD” refers to a direction along the length of the film.
[0028] The phrase “outside layer” refers to the film layer which comes in immediate contact with the outside environment (atmosphere).
[0029] The phrase “middle layer” refers to the layer which is exactly in the middle between outer and sealing layer, such as outer layer/next layer/middle layer/next layer/sealing layer.
[0030] The phrase “inner layer” refers to the film layer that comes in direct contact with the product packed. This is also called “sealing layer” as this layer must be hermetically sealed in order to protect the product from ingress of air.
[0031] As used herein, the term “homopolymer” refers to a polymer resulting from polymerization of a single monomer.
[0032] As used herein, the term “copolymer” refers to a polymer resulting from polymerization of at least two different polymers.
[0033] As used herein, the term “polymer” includes both above types.
[0034] As used herein the term “polyethylene” identifies polymers consisting essentially of the ethylene repeating unit. The ones that have a density more than 0.940 are called high density polyethylene (HDPE), the ones that are have less than 0.940 are low density polyethylene (LDPE).
[0035] As used herein the phrase “ethylene alpha olefin copolymer” refers to polymers like linear low density polyethylene (LLDPE), medium density polyethylene (MDPE), very low density polyethylene (VLDPE), ultra low density polyethylene (ULDPE), metallocene catalysed polymers and polyethylene plastomers and elastomers.
[0036] As used herein the phrase “styrene polymers” refers to styrene homopolymer such as polystyrene and to styrene copolymers such as styrene-butadiene copolymers, styrene-butadiene-styrene copolymers, styrene-isoprene-styrene copolymers, styrene-ethylene-butadiene-styrene copolymers, ethylene-styrene copolymers and the like.
[0037] As used herein the phrase “ethylene methacrylate copolymers” refers to copolymers of ethylene and methacrylate monomer. The monomer content is preferably less than 40%.
[0038] As used herein the phrase “ethylene vinyl acetate copolymer” refer to copolymers of ethylene and vinyl acetate.
[0039] As used herein, the term EVOH refers to saponified products of ethylene vinyl ester copolymers. The ethylene content is typically in the range of 25 to 50%.
[0040] As used herein the term PVDC refers to a vinylidene chloride copolymer wherein a major amount of the copolymer comprises vinylidene chloride and a minor amount of the copolymer comprises one or more monomers such as vinyl chloride and/or alkyl acrylates and methacrylates.
[0041] As used herein the term polyamide refers to homopolymers and copolymers. Typical examples are polyamide 6, polyamide 66, polyamide 6/66, polyamide 6/12 and MXD nylon.
[0042] As used herein the term “polypropylene” refers to any homopolymer, copolymer, terpolymer, tetrapolymer etc. that includes mer units of propylene. The term as used in the present application includes homopolymers, random copolymers, propylene alpha olefin copolymers, propylene ethylene copolymers propylene-ethylene-alpha olefin copolymers and other propylene polymers.
[0043] As used herein, the term “polybutylene” refers to homopolymer of butene-1 or to copolymers with ethylene or propylene.
DETAILED DESCRIPTION
[0044] The PVDC used in this invention is preferably a copolymer of vinylidene chloride and vinyl chloride or a copolymer of vinylide chloride and methyl acrylate or a blend of both.
[0045] The percentage of EVA used preferably is less than 20% per weight of the total blend.
[0046] The percentage of PVC used preferably is less than 2% per weight of the total polymer blend.
[0047] The percentage of the epoxidized oil compound preferably is less than 5% per weight of the total polymer blend.
[0048] The plasticizer-stabilizer used is preferably one of epoxidized soybean oil, epoxidized linseed oil.
[0049] The blend of EVA copolymer, PVC and additives can be a ready made compound in pallet or powder form. A preferred compound is BAYMOD L2450 purchased by the company Lanxess.
[0050] The epoxidized soybean oil or epoxidized linseed oil may be preblended to the PVDC copolymer or blended at the same time with the rest of components. Well known mixing techniques may be used to secure that the final blend is homogeneous.
[0051] Powder is preferable when the PVDC used is also powder.
[0052] In a second aspect, a plastic film is disclosed comprising a layer comprising the composition as mentioned above.
[0053] Preferably, the film is comprising five layers, where the middle layer comprises the composition as defined above and the film is heat shrinkable.
[0054] In the outside layer the following materials may be used:
1. A polypropylene homopolymer or copolymer having a vicat softening point of less than 105° C. measured under ASTM D 1525. Preferably the polymer is homogeneous, having low molecular weight distribution and comonomer distribution. 2. PP polymer such as random copolymer or homopolymer (among others) 3. Polyethylene polymer such as an alpha olefin copolymer with density 0.860 to about 0.960 or such as an ethylene ester copolymer 4. a cyclic olefin copolymer 5. a styrene polymer 6. an ionomer or a methacrylic acid copolymer 7. a polyamide (care is needed in the barrier property evaluation).
[0062] A preferred version comprises a:
1. styrene butadiene copolymer 2. a blend of styrene butadiene copolymer and an ethylene alpha olefin copolymer
[0065] Between the inner heat sealing layer and the oxygen barrier layer may exist further layers that could comprise any of the polymers mentioned in the possibilities for inner heat sealing layer. Preferred materials are ethylene vinyl acetate, ethylene alpha olefin copolymers, EMA polymers, polypropylene copolymers, polybutylene, styrene homopolymers or copolymers.
[0066] Between the outer layer and the PVDC layer, one or more layers may be present.
[0067] Preferred materials are ethylene vinyl acetate, ethylene alpha olefin copolymers, EMA polymers, polypropylene copolymers, polybutylene, styrene homopolymers or copolymers.
[0068] Typical materials used in the sealing layer are ethylene alpha olefin copolymers and polypropylene copolymers.
[0069] Any of the layers described above may also include additives well known in the art such as slip agents, antiblock, polymer processing aids, antistatic, antifog, acid scavengers, odor scavengers and the like. A person skilled in the art may select the right additives according to any particular needs.
[0070] In a preferred version of the application, the film is irradiated with e beam radiation of levels from 1 to 10 MRAD.
[0071] The material of this invention is preferably biaxially oriented and heat shrinkable.
[0072] In a further aspect, the invention comprises a bag or pouch made by the film of the invention and a cheese packed in such a film.
EXAMPLES
Example 1
[0073] A 5 layer film is produced in a double bubble commercial line with the following structure:
[0000] Inner (sealing) layer, 100% PL1, thickness 25 microns
Adjacent layer 93% E1+7% ADDITIVES, thickness 5 microns
Barrier layer PVDC 1, thickness 4.5 microns
Adjacent layer 30% M1+65% E3+5% ADDITIVES, thickness 11 microns
Outer layer 100% SB1, thickness 7.5 microns
See table 1, 2
Example 2
[0074] Inner (sealing) layer, 100% PL1
Adjacent layer 93% E1+7% ADDITIVES
Barrier layer PVDC 2
Adjacent layer 30% M1+65% E2+5% ADDITIVES
Outer layer 100% SB1
Thicknesses the same as example 1.
Comparative Example 3
[0075] A 5 layer film is produced in a double bubble (the double bubble method is described in U.S. Pat. No. 3,456,044) commercial line with the following recipe
[0000] Inner (sealing layer), 100% PL1
Adjacent layer 93% E1+7% ADDITIVES
Barrier layer PVDC commercial grade
Adjacent layer 30% M1+65% E2+5% ADDITIVES
Outer layer 95% S1+5% ADDITIVES
[0076] The difference between the examples 1 and 2 which represent the invention and ex. 3 is that the PVDC formulation used in ex. 3 is believed to have a much bigger percentage of migratory materials like epoxidized oils (more than 5% in the blend). These materials are used in order to adjust the permeability to CO 2 and O 2 .
[0077] The present invention proposes another way to adjust the permeability, without sacrificing the processability of the blend. As seen in table 3, the formulations of the invention are much more stable even after 3 months.
[0078] With the inventive formulations, problems like delaminations of PVDC are also much improved.
[0079] All the samples were e-beam radiated with a dose of 4 MRAD prior to bag making.
[0000]
TABLE 1
Melt
Index
Density
Melting point
Type
Description
Manufacturer
g/10 min
g/cm 3
° C.
E1
EVA
Dupont 3135 X
0.35
0.93
95
E2
EVA
Dupont 3165
0.7
0.94
89
S1
SB
DK13
10
1.01
COPOLYMER
M1
EMA copolymer
ARKEMA LOTRYL
2-3.5
0.95
61
29MAO3
P1
Ethylene
DOW AFFINITY PL
1
0.902
100
octene
1880
copolymer
Manufacture of the Three PVDC
[0080] PVDC 1. Blend of PVDC copolymer (which already incorporates about 2% per weight epoxidized soybean oil) with 11% BAYMOD L2450.
[0081] PVDC 2. Blend of PVDC copolymer (which already incorporates about 2% per weight epoxidized soybean oil) with 16% BAYMOD L2450. This blend is used for packaging of special “high gassing” types of cheeses.
[0082] PVDC 3. Commercial PVDC with more than 5% epoxidized soybean oil.
[0083] Measurements were done three days after the irradiation step.
[0000]
TABLE 3
O 2
CO 2
CO 2 transmission
transmission
transmission
After 3 months
Example 1
155
810
750
Example 2
410
2100
1950
Example 3
140
780
450
[0084] O 2 transmission is measured in 23 C, 75% RH according to ASTM D3985. Units are CC/M 2 *atm*day.
[0085] CO 2 transmission is measured according to internal method using a MOCON type instrument. Units are CC/M 2 *atm*day. Conditions 23° C. at 0% RH.
[0086] We see that the combinations 1 and 2 are much more stable overtime. This is beneficial as it reduces the risks of pack “ballooning” after a certain period of time.
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The present invention is directed to a polymer blend formulation and to heat shrinkable film, bags, pouches and the like made therefrom. The invention is further directed to a method of producing a heat shrinkable film with the proper gas permeability properties so that it is ideal for packaging and preservation of gassing cheese.
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This is a divisional of application Ser. No. 08/266,178, filed Jun. 27, 1994, which is a file wrapper continuation of Ser. No. 07/851,074, filed Mar. 13, 1992, now abandoned.
BACKGROUND OF THE INVENTION
1. Field of the Invention
This invention relates to radiodiagnostic reagents and peptides, and methods for producing labeled radiodiagnostic agents. Specifically, the invention relates to technetium-99m (Tc-99m) labeled reagents, methods and kits for making such reagents, and methods for using such reagents to image sites of infection and inflammation in a mammalian body.
2. Description of the Prior Art
A variety of radionuclides are known to be useful for radioimaging, including 67 Ga, 99m Tc (Tc-99m), 111 In, 123 I, 125 I, 169 Yb or 186 Re. The sensitivity of imaging methods using radioactively-labeled peptides is much higher than other techniques known in the art, since the specific binding of the radioactive peptide concentrates the radioactive signal over the area of interest, for example, an inflammatory site.
There is a clinical need to be able to determine the location and/or extent of sites of focal or localized infection. In a substantial number of cases conventional methods of diagnosis (such as physical examination, x-ray, CT and ultrasonography) fail to identify such sites (e.g., an abscess). In some cases, biopsy may be resorted to, but is preferably avoided at least until it is necessary in order to identify the pathogen responsible for an abscess at a known location. Identifying the site of such "occult"' infection is important because rapid localization of the problem is critical to effective therapeutic intervention.
In the field of nuclear medicine, certain pathological conditions can be localized or the extent of such conditions determined by imaging the internal distribution of administered radioactively-labeled tracer compounds (i.e. radiotracers or radiopharmaceuticals) that accumulate specifically at the pathological site. However, an abscess may be caused by any one of many possible pathogens, so that a radiotracer specific for a particular pathogen would have limited scope. On the other hand, infection is almost invariably accompanied by inflammation, which is a general response of the body to tissue injury. Therefore, a radiotracer specific for sites of inflammation would be expected to be useful in localizing sites of infection caused by any pathogen.
One of the main phenomena associated with inflammation is the localization of leukocytes (white blood cells), usually monocytes and neutrophils, at the site of inflammation. A radiotracer specific for leukocytes would be useful in detecting leukocytes at the site of a localized infection. Currently approved nuclear medicine procedures for imaging sites of infection use either indium-111 labeled leukocytes ( 111 In-WBC) (see, e.g. Peters, 1992, J. Nucl. Med. 33: 65-67) or gallium-67 ( 67 Ga) citrate (see, e.g. Ebright et al., 1982, Arch. Int. Med. 142: 246-254). A major disadvantage of using 111 In-labeled WBCs is that the preparation of the radiotracer requires sterile removal of autologous blood, sterile isolation of the leukocytes from the blood, sterile labeling of the leukocytes using conditions that do not damage the cells (since damaged WBC are taken up by the reticuloendothelial system when re-injected) and return (re-injection) of the (now labeled) leukocytes to the patient. Furthermore, a delay of 12 to 48 hours between injection and imaging may be required for optimal images. While Tc-99m labeled leukocytes have been used to shorten this delay period (see, e.g. Vorne et al., 1989, J. Nucl. Med. 30: 1332-1336), ex-corporeal labeling is still required. A preferred radiotracer would be one that does not require removal and manipulation of autologous blood components.
67 Ga-citrate can be administered by intravenous injection. However, this compound is not specific for sites of infection or inflammation. Moreover, a delay of up to 72 hours is often required between injection of the radiotracer and imaging. In addition, the γ-(gamma) emissions energies of 67 Ga are not well suited to conventional gamma cameras.
Radiolabeled monoclonal and polyclonal antibodies raised against human leukocytes (including monocytes, neutrophils, granulocytes and other) have been developed. Tc-99m labeled antigranulocyte monoclonal antibodies (see, e.g. Lind et al., 1990, J. Nucl. Med. 31: 417-473) and 111 In-labeled non-specific human immunoglobulin (see, e.g. LaMuraglia et al., 1989, J. Vasc. Surg. 10: 20-28) have been tested for the detection of inflammation secondary to infection. 111 In-labeled IgG shares the disadvantages of 111 In-labeled WBC, in that 24-48 hours are required between injection and optimal imaging. In addition, all radiolabeled antibodies are difficult to produce and face protracted regulatory agency approval procedures as biologics.
Small readily synthesized molecules are preferred for routinely used radiopharmaceuticals. There is clearly a need for small synthetic molecules that can be directly injected into a patient and will image sites of infection and inflammation by localizing at sites where leukocytes have accumulated.
One class of compounds known to bind to leukocytes are chemotactic peptides that cause leukocytes to move up a peptide concentration gradient (see Wilkinson, 1988, Meth. Enzymol. 162: 127-132). These compounds bind to receptors on the surface of leukocytes with very high affinity. These peptides are derived from a number of sources, including complement factors, bacteria, tuftsin, elastin, fibrinopeptide B, fibrinogen Bβ, platelet factor 4 and others. Small synthetic peptides derived from these chemotactic compounds and radiolabeled would be very useful as radiotracers for imaging sites of inflammation in vivo.
Radiolabeled peptides have been reported in the prior art.
Zoghbi et al., 1981, J. Nucl. Med. 22: 32 (Abst) disclose formyl peptide chemotactic factors derived from bacteria coupled to 111 In-labeled transferrin.
Jiang et al., 1982, Nuklearmedizin 21: 110-113 disclose a chemotactic formylated peptide radiolabeled with 125 I.
Fischman et al., 1991, J. Nucl. Med. 32: 482-491 relates to chemotactic formyl peptide-- 111 In-labeled DTPA conjugates.
EPC 90108734.6 relates to chemotactic formyl peptide-- 111 In-labeled DTPA conjugates.
U.S. Pat. No. 4,986,979 relates to the use of radiolabeled chemotactic formyl peptides to radiolabel leukocytes ex-corporeally via a photoaffinity label.
PCT W090/10463 relates to the use of radiolabeled chemotactic formyl peptides to radiolabel leukocytes ex-corporeally via a photoaffinity label.
The use of chelating agents for radiolabeling polypeptides, methods for labeling peptides and polypeptides with Tc-99m are known in the prior art and are disclosed in copending U.S. patent applications Ser. Nos. 07/653,012 now abandoned, which issued on Aug. 5, 1997 as U.S. Pat. No. 5,654,272 from continuation application Ser. No. 08/263,758, filed Jun. 22, 1994 and 07/807,062 which issued on Aug. 22, 1995 as U.S. Pat. No. 5,443,815, which are hereby incorporated by reference.
SUMMARY OF THE INVENTION
The present invention provides scintigraphic imaging agents that are radioactively-labeled peptides. The peptides of the invention are comprised of peptides that bind leukocytes and are covalently linked to a radioisotope complexing group wherein the complexing group binds a radioisotope.
In a first aspect of the present invention, radiolabeled peptides are provided capable of imaging site of inflammation in a mammalian body, such peptides comprising a specific binding peptide that binds to leukocytes, and a radiolabel-binding moiety of formula
Cp(aa)Cp
wherein Cp is a protected cysteine residue and (aa) stands for an amino acid, and wherein the radiolabel-binding moiety is covalently linked to the specific binding peptides. In a preferred embodiment, the amino acid is glycine. In another preferred embodiment, the radiolabel-binding moiety is linked to the specific peptide via one or more amino acids.
In a second aspect, the present invention provides leukocyte-binding peptides that are covalently linked to a radiolabel-binding moiety having the following structure:
A--CH(B)-- C(RR')!.sub.n --X
wherein A is H, HOOC, H 2 NOC, or --NHOC; B is H, SH or NHR", where R" is H, lower alkyl or --C═O; X is SH or NHR", where R" is H, lower alkyl or --C═O; R and R' are independently H or lower alkyl; n is 0, 1 or 2; and: 1. where B is NHR", where R" is H, lower alkyl or --C═O, X is SH and n is 1 or 2; and 2. where X is NHR", where R" is H, lower alkyl or --C═O, B is SH and n is 1 or 2; 4. where B is H, A is HOOC, H 2 NOC, or --NHOC, X is SH and n is 0 or 1; and wherein the thiol moiety is in the reduced form.
A peptide for imaging sites of inflammation within a mammalian body, comprising a specific binding peptide having an amino acid sequence comprising between 4 and 100 amino acids and wherein the peptide binds to leukocytes, and a radiolabel-binding moiety that forms a neutral complex with technetium-99m.
In yet another aspect, the present invention provides leukocyte-binding peptides that are covalently linked to a radiolabel-binding moiety having the following structure: ##STR1## wherein each R is independently H, lower alkyl having 1 to 6 carbon atoms, phenyl, or phenyl substituted with lower alkyl or lower alkoxy, and wherein each n is independently 1 or 2. In a preferred embodiment, the radiolabel-binding moiety has the structure ##STR2##
In an additional aspect of the invention, technetium-99m complexed peptides are provided, for imaging sites of inflammation within a mammalian body, comprising a leukocyte binding peptide having an amino acid sequence comprising between 4 and 100 amino acids and a radiolabel-binding moiety that forms a complex with technetium-99m, wherein the technetium-99m complexed peptide has a net charge of -1.
The invention also comprises complexes of the peptides of the invention with Tc-99m, kits for preparing the peptides of the invention radiolabeled with Tc-99m, methods for radiolabeling the peptides of the invention with Tc-99m and methods for using the radiolabeled peptides of the invention for imaging sites of infection or inflammation in mammalian body by gamma scintigraphy.
DETAILED DESCRIPTION OF THE INVENTION
The present invention provides Tc-99m labeled peptides for imaging target sites within a mammalian body that bind to leukocytes and are covalently linked to a radiolabel complexing group wherein the complexing group binds a radioisotope.
The peptides of this invention bind to leukocytes, preferably monocytes and neutrophils and most preferably to neutrophils. For purposes of this invention, the term "bind to leukocytes" is intended to mean that the peptides of the present invention are capable of accumulating at sites of infection or inflammation in mammalian body sufficient to allow detection of such sites by gamma scintigraphy.
In Cp(aa)Cp-containing peptides, the Cp is a protected cysteine where the S-protecting groups are the same or different and may be but not limited to:
--CH 2 --aryl (aryl is phenyl or alkyl or alkyloxy substituted phenyl);
--CH--(aryl) 2 , (aryl is phenyl or alkyl or alkyloxy substituted phenyl);
--C--(aryl) 3 , (aryl is phenyl or alkyl or alkyloxy substituted phenyl);
--CH 2 --(4-methoxyphenyl);
--CH--(4-pyridyl)(phenyl) 2 ;
--C(CH 3 ) 3
-9-phenylfluorenyl;
--CH 2 NHCOR (R is unsubstituted or substituted alkyl or aryl);
--CH 2 --NHCOOR (R is unsubstituted or substituted alkyl or aryl);
--CONHR (R is unsubstituted or substituted alkyl or aryl);
--CH 2 --S--CH 2 --phenyl
The preferred protecting group has the formula --CH 2 --NHCOR wherein R is a lower alkyl having 1 and 8 carbon atoms, phenyl or phenyl-substituted with lower alkyl, hydroxyl, lower alkoxy, carboxy, or lower alkoxycarbonyl.
Labeling with Tc-99m is an advantage of the present invention because the nuclear and radioactive properties of this isotope make it an ideal scintigraphic imaging agent. This isotope has a single photon energy of 140 keV and a radioactive half-life of about 6 hours, and is readily available from a 99 Mo- 99m Tc generator. Other radionuclides known in the prior art have effective half-lives which are much longer (for example, 111 In, which has a half-life of 67.4 h) or are toxic (for example, 125 I).
Peptides of the present invention can be chemically synthesized in vitro. Peptides of the present invention can generally advantageously be prepared on an amino acid synthesizer. The peptides of this invention can be synthesized wherein the complexing group is covalently linked to the peptide during chemical in vitro synthesis, using techniques well known to those with skill in the art. Such peptides covalently-linked to the complexing group upon synthesis are advantageous because specific sites of covalent linkage can be determined therein.
In forming a complex of radioactive technetium with the peptides of this invention, the technetium complex, preferably a salt of Tc-99m pertechnetate, is reacted with the peptides of this invention in the presence of a reducing agent; in a preferred embodiment, the reducing agent is stannous chloride. In an additional preferred embodiment, the reducing agent is a solid-phase reducing agent. Complexes and means for preparing such complexes are conveniently provided in a kit form comprising a sealed vial containing a predetermined quantity of the peptides of the invention that are to be labeled and a sufficient amount of reducing agent to label the peptide with Tc-99m. Alternatively, the complex may be formed by reacting the peptides of this invention with a pre-formed labile complex of technetium and another compound known as a transfer ligand. This process is known as ligand exchange and is well known to those skilled in the art. The labile complex may be formed using such transfer ligands as tartrate, citrate, gluconate or mannitol, for example. Among the Tc-99m pertechnetate salts useful with the present invention are included the alkali metal salts such as the sodium salt, or ammonium salts or lower alkyl ammonium salts. The reaction of the peptides of this invention with Tc-pertechnetate or preformed Tc-99m labile complex can be carried out in an aqueous medium at room temperature. The anionic complex which has a charge of -1! is formed in the aqueous medium in the form of a salt with a suitable cation such as sodium cation, ammonium cation, mono, di- or tri-lower alkyl amine cation, etc. Any conventional salt of the anionic complex with a pharmaceutically acceptable cation can be used in accordance with this invention.
In another embodiment of the present invention, the peptides of the invention that are to be labeled are reduced prior to labeling by incubating the peptides with a reducing agent. In a preferred embodiment, the reducing agent is stannous chloride. In an additional preferred embodiment, the reducing agent is a solid-phase reducing agent. The pre-reduced peptide is then labeled by reaction with a Tc-99m under reducing conditions or with pre-reduced Tc-99m or Tc-99m complex.
In a preferred embodiment of the invention, a kit for preparing technetium-labeled peptides is provided. The peptides of the invention can be chemically synthesized using methods and means well-known to those with skill in the art and described hereinbelow. Peptides thus prepared are comprised of between 3 and 100 amino acid residues, and are covalently linked to a radioisotope complexing group wherein the complexing group binds a radioisotope. An appropriate amount of the peptide is introduced into a vial containing a reducing agent, such as stannous chloride or a solid-phase reducing agent, in an amount sufficient to label the peptide with Tc-99m. An appropriate amount of a transfer ligand as described (such as tartrate, citrate, gluconate or mannitol, for example) can also be included. Technetium-labeled peptides according to the present invention can be prepared by the addition of an appropriate amount of Tc-99m or Tc-99m complex into the vials and reaction under conditions described in Example 2 hereinbelow.
Radioactively labeled peptides provided by the present invention are provided having a suitable amount of radioactivity. In forming the Tc-99m radioactive anionic complexes, it is generally preferred to form radioactive complexes in solutions containing radioactivity at concentrations of from about 0.01 millicurie (mCi) to 100 mCi per ml.
Technetium-labeled peptides provided by the present invention can be used for visualizing sites of inflammation, including abscesses and sites of "occult" infection. The Tc-99m labeled peptides provided by the present invention can also be used for visualizing sites of inflammation caused by tissue ischemia, including such disorders as inflammatory bowel disease and arthritis. In accordance with this invention, the technetium-labeled peptides or anionic complexes either as a complex or as a salt with a pharmaceutically acceptable cation are administered in a single unit injectable dose. Any of the common carriers known to those with skill in the art, such as sterile saline solution or plasma, can be utilized after radiolabeling for preparing the injectable solution to diagnostically image various organs, tumors and the like in accordance with this invention. Generally, the unit dose to be administered has a radioactivity of about 0.01 mCi to about 100 mCi, preferably 1 mCi to 20 mCi. The solution to be injected at unit dosage is from about 0.01 ml to about 10 ml. After intravenous administration, imaging of the organ or tumor in vivo can take place in a matter of a few minutes. However, imaging can take place, if desired, in hours or even longer, after injecting into patients. In most instances, a sufficient amount of the administered dose will accumulate in the area to be imaged within about 0.1 of an hour to permit the taking of scintiphotos. Any conventional method of scintigraphic imaging for diagnostic purposes can be utilized in accordance with this invention.
The technetium-labeled peptides and complexes provided by the invention may be administered intravenously in any conventional medium for intravenous injection such as an aqueous saline medium, or in blood plasma medium. Such medium may also contain conventional pharmaceutical adjunct materials such as, for example, pharmaceutically acceptable salts to adjust the osmotic pressure, buffers, preservatives and the like. Among the preferred media are normal saline and plasma.
The methods for making and labeling these compounds are more fully illustrated in the following Examples. These Examples illustrate certain aspects of the above-described method and advantageous results. These Examples are shown by way of illustration and not by way of limitation.
EXAMPLE 1
Solid Phase Petide Synthesis
Solid phase peptide synthesis (SPPS) was carried out on a 0.25 millimole (mmole) scale using an Applied Biosystems Model 431A Peptide Synthesizer and using 9-fluorenylmethyloxycarbonyl (Fmoc) amino-terminus protection, coupling with dicyclohexylcarbodiimide/hydroxybenzotriazole or 2-(1H-benzo-triazol-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate/hydroxybenzotriazole (HBTU/HOBT), and using p-hydroxymethylphenoxymethyl-polystyrene (HMP) resin for carboxyl-terminus acids or Rink amide resin for carboxyl-terminus amides. Resin-bound products were routinely cleaved using a solution comprised of trifluoroacetic acid, water, thioanisole, ethanedithiol, and triethylsilane, prepared in ratios of 100:5:5:2.5:2 for 1.5-3 h at room temperature. Where appropriate N-α-formyl groups were introduced by treating the cleaved, deprotected peptide with acetic anhydride in 98% formic acid. Where appropriate the "pica"' group was introduced by conjugating picolylamine to a precursor peptide using diisopropylcarbodiimide and N-hydroxysuccinimide. Crude peptides were purified by preparative high pressure liquid chromatography (HPLC) using a Waters Delta Pak C18 column and gradient elution using 0.1% trifluoroacetic acid (TFA) in water modified with acetonitrile. Acetonitrile was evaporated from the eluted fractions which were then lyophilized. The identity of each product was confirmed by fast atom bombardment mass spectroscopy (FABMS).
EXAMPLE 2
A General Method for Radiolabeling with Tc-99m
0.1 mg of a peptide prepared as in Example 1 was dissolved in 0.1 ml of 0.05M potassium phosphate buffer (pH 7.4). Tc-99m gluceptate was prepared by reconstituting a Glucoscan vial (E.I. DuPont de Nemours, Inc.) with 1.0 ml of Tc-99m sodium pertechnetate containing up to 200 mCi and allowed to stand for 15 minutes at room temperature. 25 μl of Tc-99m gluceptate was then added to the peptide and the reaction allowed to proceed at room temperature for 30 min and then filtered through a 0.2 μm filter.
The Tc-99m labeled peptide purity was determined by HPLC using a Vydak 218TP54 analytical column (RP-18, 5 micron, 220×4.6 mm) and eluted as described in the Footnotes in Table I. Radioactive components were detected by an in-line radiometric detector linked to an integrating recorder. Tc-99m gluceptate and Tc-99m sodium pertechnetate elute between 1 and 4 minutes under these conditions, whereas the Tc-99m labeled peptide eluted after a much greater amount of time.
The following Table illustrates successful Tc-99m labeling of peptides prepared according to Example 1 using the method described herein.
__________________________________________________________________________ FABMS Radiochemical HPLCPeptides MH.sup.+ Yield R.sub.1 (min)__________________________________________________________________________C.sub.Mob GC.sub.Acm PLYKKIIKKLLES (SEQ. ID NO.: 1) 2028 97% Boundformyl-MLFC.sub.Acm GC.sub.Acm (SEQ. ID NO.: 2) 843 100% 11.1,11.9.sup.1C.sub.Acm GC.sub.Acm (VGVAPG).sub.3 amide (SEQ. ID. NO.: 1865 100% 17.7.sup.1formyl-MIFLC.sub.Acm GC.sub.Acm (SEQ. ID NO.: 3) 957 100% 11.4.sup.1C.sub.Acm GC.sub.Acm TKPR (SEQ. ID NO.: 4) 906.5 100% 16.1.sup.1formyl-MLFC.sub.Acm GPica (SEQ. ID NO.: 5) 760 100% 10.9,12.2.sup.1formyl-Nle-LF-Nle-YKC.sub.Acm GC.sub.Acm (SEQ. ID NO.: 6) 1230 97% 15.6-16.8.sup.2PicGC.sub.Acm (VGVAPG).sub.3 amide (SEQ. ID NO.: 12) 1795 92% 12.4.sup.2PicGC.sub.Acm (VPGVG).sub.4 amide (SEQ. ID NO.: 13) 1992 100% 12.0.sup.1PicGC.sub.Acm PLYKKIIKKLLES (SEQ. ID NO.: 7) 1910 81% 12.9,13.3.sup.3C.sub.Acm GC.sub.Acm PLYKKIIKKLLES (SEQ. ID NO.: 8) 2093 96% 12.6.sup.3pGluGVNDNEEGFFSARC.sub.Acm GC.sub.Acm amide (SEQ. ID NO.: 1957 95% 16.3,16.7.sup.3PicGC.sub.Acm GHRPLDKKREEAPSLRPAPPPISGGGYR (SEQ. ID NO.: 3377 94% 11.3.sup.3(VPGVG).sub.4 GGGC.sub.Acm GC.sub.Acm amide (SEQ. ID NO.: 2231 67% 11.2,11.5.sup.3(VGVAPG).sub.3 GGGC.sub.Acm GC.sub.Acm amide (SEQ. ID NO.: 2035 33% 10.6.sup.3AcC.sub.Acm GC.sub.Acm GGG(VPGVG).sub.4 amide (SEQ. ID NO.: 2275 97% 9.6,9.9.sup.3AcC.sub.Acm GC.sub.Acm Aca(VPGVG).sub.4 amide (SEQ. ID NO.: 2216 76% 11.6,12.6.sup.3__________________________________________________________________________Ac = acetyl; Pic = picolinoyl (pyridine-2-carbonyl); Acm= acetamidomethyl; Mob = 4-Methoxybenzylaminocaproic acidne (2-(aminomethyl)pyridine); Aca = εHPLC methods (indicated by superscript after R.sub.1):general: solvent A = 0.1% CF3COOH/H2O solvent B.sub.70 = 0.1% CF.sub.3 COOH/70% CH.sub.3 CN/H.sub.2 O solvent B.sub.90 = 0.1% CF.sub.3 COOH/90% CH.sub.3 CN/H.sub.2 O solvent flow rate = 1 ml/min
Vydak column=Vydak 218TP54 RP-18, 5μ×220 mm×4.6 mm analytical column with guard column
Brownlee column=Brownlee Spheri-5, RP-18 5μ×220×4.6 mm column
______________________________________Method 1: Brownlee column 100% A to 100% B.sub.70 in 10 minMethod 2: Vydak column 100% A to 100% B.sub.90 in 10 minMethod 3: Vydak column 100% A to 100% B.sub.70 in 10 min______________________________________
It should be understood that the foregoing disclosure emphasizes certain specific embodiments of the invention and that all modifications or alternatives equivalent thereto are within the spirit and scope of the invention as set forth in the appended claims.
__________________________________________________________________________SEQUENCE LISTING(1) GENERAL INFORMATION:(iii) NUMBER OF SEQUENCES: 17(2) INFORMATION FOR SEQ ID NO:1:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 16 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 1..3(D) OTHER INFORMATION: /label=Protected-Cys/note= "The thiol of the amino terminal cysteineis protected by a 4-methoxybebzyl group; the thiolof the cysteine at position 3 is protected by an(xi) SEQUENCE DESCRIPTION: SEQ ID NO:1:CysGlyCysProLeuTyrLysLysIleIleLysLysLeuLeuGluSer151015(2) INFORMATION FOR SEQ ID NO:2:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 6 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 4..6(D) OTHER INFORMATION: /label=MODIFIED-CYS/note= "The thiol group of each cysteine isprotected by an acetamidomethyl group; the aminoterminal amine is formylated."(xi) SEQUENCE DESCRIPTION: SEQ ID NO:2:MetLeuPheCysGlyCys15(2) INFORMATION FOR SEQ ID NO:3:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 7 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 5..7(D) OTHER INFORMATION: /label=Modified-Cys/note= "The thiol group of each cysteine isprotected by an acetamidomethyl group; the aminoterminal amine is formylated."(xi) SEQUENCE DESCRIPTION: SEQ ID NO:3:MetIlePheLeuCysGlyCys15(2) INFORMATION FOR SEQ ID NO:4:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 7 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 1..3(D) OTHER INFORMATION: /label=Modified-Cys/note= "The thiol group of each cysteine isprotected with an acetamidomethyl group."(xi) SEQUENCE DESCRIPTION: SEQ ID NO:4:CysGlyCysThrLysProArg15(2) INFORMATION FOR SEQ ID NO:5:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 6 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Peptide(B) LOCATION: 4..6(D) OTHER INFORMATION: /label=Modified-Cys/note= "The thiol of the cysteine is protected byan acetamidomethyl group; residue X =2- aminomethylpyridine"(xi) SEQUENCE DESCRIPTION: SEQ ID NO:5:MetLeuPheCysGlyXaa15(2) INFORMATION FOR SEQ ID NO:6:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 9 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 1..4(D) OTHER INFORMATION: /label=Norleucine/note= "Each X residue = norleucine; the aminoterminal amine of the amino terminal norleucine isformylated."(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 7..9(D) OTHER INFORMATION: /label=Modified-Cys/note= "The thiol of each cysteine residue isprotected by an acetamidomethyl group."(xi) SEQUENCE DESCRIPTION: SEQ ID NO:6:XaaLeuPheXaaTyrLysCysGlyCys15(2) INFORMATION FOR SEQ ID NO:7:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 16 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 1..3(D) OTHER INFORMATION: /label=Picolinoyl/note= "The amino terminal residue ispyridine-2- carbonyl; the thiol of the cysteine isprotected by an acetamidomethyl group."(xi) SEQUENCE DESCRIPTION: SEQ ID NO:7:XaaGlyCysProLeuTyrLysLysIleIleLysLysLeuLeuGluSer151015(2) INFORMATION FOR SEQ ID NO:8:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 16 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 1..3(D) OTHER INFORMATION: /label=Modified-Cys/note= "The thiol group of each cyteine isprotected by an acetamidomethyl group."(xi) SEQUENCE DESCRIPTION: SEQ ID NO:8:CysGlyCysProLeuThrLysLysIleIleLysLysLeuLeuGluSer151015(2) INFORMATION FOR SEQ ID NO:9:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 31 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 1..3(D) OTHER INFORMATION: /label=Picolinoyl/note= "The amino terminal residue ispyridine-2- carbonyl; the thiol of the cysteineresidue is protected by an acetoamidomethyl(xi) SEQUENCE DESCRIPTION: SEQ ID NO:9:XaaGlyCysGlyHisArgProLeuAspLysLysArgGluGluAlaPro151015SerLeuArgProAlaProProProIleSerGlyGlyGlyTyrArg202530(2) INFORMATION FOR SEQ ID NO:10:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 17 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 15..17(D) OTHER INFORMATION: /label=Modified-Cys/note= "The thiol of each cysteine is protected byan acetamidomethyl group; the carboxyl terminus isamidated; the amino terminal glutamic acid is(xi) SEQUENCE DESCRIPTION: SEQ ID NO:10:GluGlyValAsnAspAsnGluGluGlyPhePheSerAlaArgCysGly151015Cys(2) INFORMATION FOR SEQ ID NO:11:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 21 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 4..6(D) OTHER INFORMATION: /label=MODIFIED-CYS/note= "The thiol group of each cysteine isprotected by an acetamidomethyl group; the aminoterminal amine is formylated."(xi) SEQUENCE DESCRIPTION: SEQ ID NO:11:CysGlyCysValGlyValAlaProGlyValGlyValAlaProGlyVal151015GlyValAlaProGly20(2) INFORMATION FOR SEQ ID NO:12:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 21 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 1..3(D) OTHER INFORMATION: /label=Picolinoyl/note= "The amino terminal residue ispyridine-2- carbonyl; the thiol of the cysteineresidue is protected by an acetoamidomethyl(xi) SEQUENCE DESCRIPTION: SEQ ID NO:12:XaaGlyCysValGlyValAlaProGlyValGlyValAlaProGlyVal151015GlyValAlaProGly20(2) INFORMATION FOR SEQ ID NO:13:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 23 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 1..3(D) OTHER INFORMATION: /label=Picolinoyl/note= "The amino terminal residue ispyridine-2- carbonyl; the thiol of the cysteineresidue is protected by an acetoamidomethyl(xi) SEQUENCE DESCRIPTION: SEQ ID NO:13:XaaGlyCysValProGlyValGlyValProGlyValGlyValProGly151015ValGlyValProGlyValGly20(2) INFORMATION FOR SEQ ID NO:14:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 26 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 24..26(D) OTHER INFORMATION: /label=MODIFIED-CYS/note= "The thiol group of each cysteine isprotected by an acetamidomethyl group; the carboxylterminus is an amide."(xi) SEQUENCE DESCRIPTION: SEQ ID NO:14:ValProGlyValGlyValProGlyValGlyValProGlyValGlyVal151015ProGlyValGlyGlyGlyGlyCysGlyCys2025(2) INFORMATION FOR SEQ ID NO:15:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 24 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 22..24(D) OTHER INFORMATION: /label=MODIFIED-CYS/note= "The thiol group of each cysteine isprotected by an acetamidomethyl group; the carboxylterminus is an amide."(xi) SEQUENCE DESCRIPTION: SEQ ID NO:15:ValGlyValAlaProGlyValGlyValAlaProGlyValGlyValAla151015ProGlyGlyGlyGlyCysGlyCys20(2) INFORMATION FOR SEQ ID NO:16:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 26 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 1..3(D) OTHER INFORMATION: /label=MODIFIED-CYS/note= "The thiol group of each cysteine isprotected by an acetamidomethyl group; the aminoterminal amine is acetylated."(xi) SEQUENCE DESCRIPTION: SEQ ID NO:16:CysGlyCysGlyGlyGlyValProGlyValGlyValProGlyValGly151015ValProGlyValGlyValProGlyValGly2025(2) INFORMATION FOR SEQ ID NO:17:(i) SEQUENCE CHARACTERISTICS:(A) LENGTH: 24 amino acids(B) TYPE: amino acid(D) TOPOLOGY: linear(ii) MOLECULE TYPE: peptide(ix) FEATURE:(A) NAME/KEY: Peptide(B) LOCATION: 4..5(D) OTHER INFORMATION: /label=Modified-Cys/note= "The thiol of the cysteine is protected byan acetamidomethyl group; residue X =2- aminomethylpyridine"(ix) FEATURE:(A) NAME/KEY: Modified-site(B) LOCATION: 1..3(D) OTHER INFORMATION: /label=aminocaproate/note= "Residue Xaa = epsilon amino caproicacid."(xi) SEQUENCE DESCRIPTION: SEQ ID NO:17:CysGlyCysXaaValProGlyValGlyValProGlyValGlyValPro151015GlyValGlyValProGlyValGly20__________________________________________________________________________
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This invention relates to radiolabeled peptides and methods for producing such peptides. Specifically, the invention relates to technetium-99m (Tc-99m) labeled leukocyte-binding peptides, methods and kits for making such peptides, and methods for using such peptides to image sites of infection and inflammation in a mammalian body.
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CROSS-REFERENCE TO RELATED APPLICATIONS
Commonly-assigned U.S. patent applications Ser. No. 08/561,337, filed Nov. 21, 1995 entitled "Improved Fault Tolerant Controller System and Method" by W. A. Brant, M. E. Nielson an G. Howard; Ser. No. 08/363,132 entitled "A Fault Tolerant Memory System" by G. Neben, W. A. Brant and M. E. Nielson; and Ser. No. 08/363,655 entitled "Method and Apparatus for Fault Tolerant Fast Writes Through Buffer Dumping" by W. A. Brant, G. Neben, M. E. Nielson and D. C. Stallmo (a continuation-in-part application of U.S. Ser. No. 08/112,791 by Brant and Stallmo which is itself a continuation-in-part of application Ser. No. 638,167 filed Jan. 6, 1991 by Brant, Stallmo, Walker and Lui the latter of which is now U.S. Pat. No. 5,274,799) describe fault tolerant data processing apparatus and processes which interface between hosts and data storing subsystems.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to data processing structures and procedures which provide interfacing between computer type systems and low cost but slow performing mass data storage devices or subsystems. More particularly, the present invention relates to digital data handling structures and methods which optimize cost/performance interfacing between host systems which exchange data with relatively inexpensive high capacity data storage devices. While not necessarily so limited, the present invention is especially useful in systems having a dynamic ability to overcome errors resulting from various sources during transmission of digital data between computer oriented complexes.
2. Description of the Related Art
The costs of manufacturing disk drives as a media for storing digital data has reduced dramatically in recent years. It has far outpaced the cost reductions associated with solid state and other data storage devices. Smaller form factor disk drives permit disk subsystems to exploit the performance advantages of having more disk drives to service requests in parallel.
The components of disk subsystems have also become significantly more reliable in recent years. Mean Time Between Failure (MTBF) ratings have progressed from 15,000 hours in 1988 to 500,000-800,000 hours for both disk drives and power supplies. The MTBF for controller electronics continues to improve with integration and lower power requirements.
The personal computer (PC) technology has become ever more popular for use as major elements in data processing and handling systems and subsystems. System configurations known as RAID (Redundant Array of Inexpensive Disks) computers have likewise evolved.
Caching controllers that interface with host computers or the like for directing data exchanges with large arrays of magnetic data storing disks, or other storage media, have developed for providing a storage medium for large quantities of digital information. These controllers respond to read and write commands from a remote computer system to receive, and/or deliver data over interconnecting busses. They often employ expensive solid state storage, such as RAM, to cache host data to minimize the relatively long latency of the disk subsystem.
Preferably, the caching controller should function so that it minimizes delays and demands on the host system, while including the ability to recover wherever possible from errors from single points of failure. System configurations and operations capable of dynamically overcoming single points of failure are sometimes referred to as fault tolerant systems. The aforementioned related patent applications describe such redundant fault tolerant systems and operations in a disk array controller environment.
It is known to improve storage system reliability by redundant recordings of the same data on duplicate tape or disk drive systems. This allows improved reliability in that the data is still available from the back-up recording in the event of failure of the primary drive. Furthermore, the redundancy helps to somewhat reduce the amount of time required to read that data in that the controller can issue concurrent read commands to both of the redundant storage devices. The data is selected from the drive which first produces it.
The cache controller avoids wait time by the host computer, or central processor, in reading or writing relative to a disk by buffering write data into a protected fast memory, and servicing most read data from fast memory. A system, as described in the cross-referenced copending patent application, can include redundant storage media array controllers for responding to host computer requests for transferring data between that host computer and an arrangement for low cost but large quantity data storage.
In "Computer Architecture, A Quantitative Approach" by D. A. Patterson and J. L. Hennessey (Morgan Kaufmann Publishers, Inc., Second Edition, 1990, 1996), discusses processor memory, or RAM, and how it is cached. It describes the disciplines, such as direct map, set associative, and the like.
SUMMARY OF THE INVENTION
The present invention advantageously utilizes an array of relatively slow devices, such as low cost disk drives, with the data replicated across those devices so as to enhance the probability that one of the read/write heads is relatively close to the desired data upon the occurrence of a read command. The controller renders a logical decision as to which drive can produce the desired data with the least delay.
The present invention deliberately uses mapping and caching techniques to replicate data across a multiplicity of disk drives to substantially enhance the ability to quickly recover the data. The data is replicated across the drives, and replications of the data on the same drive is likewise possible, thereby minimizing the time for a read/write head to encounter the desired data. Thus, inexpensive storage improves the speed of data recovery.
The controller optimizes the seek and rotational latency times. A given controller can concurrently service a plurality of data recovery operations. The mere presence of a particular data exchange request as from the host is not necessarily the next item that will receive execution. The controller determines which service requests are queued ahead of a given request, and further projects where each of the read/write heads of the disk drives will reside at that time. Thus, the controller can determine which disk drive head will actually recover the requested data well in advance of its actually producing that result.
A series of products based on a single hardware package further leverages the value of using contemporary, off-the-shelf components. A disk based disk cache, a high performance simplex and/or duplex mirrored disk subsystem, and a low maintenance mass storage unit using RAID5 are possible. RAID3 configurations can be configured with hardware accelerators.
The most economical disk drives have found continuing favor in high volume applications, such as PCs and workstations. Leveraging the cost performance of these disk drives into high read/write performance applications requires packaging large numbers of disks coupled with a controller to manage the complexity of distributing data among all the drives, and the use of data parity codes and data striping to mitigate the decreased MTBF.
As disk drives become smaller, the performance advantages of using very large numbers of disks becomes feasible since space requirements are small, and power and control distribution is over small distances. As the cost per megabyte (MB) falls, it becomes less expensive to increase disk subsystem performance by storing the data on multiple drives instead of using expensive controllers that distribute and reconstruct data with parity, such as in RAIDS systems.
With regard to disk based disk cache management strategies, the mechanical characteristics and the size of the disk based disk cache suggest special constraints for managing the disk based disk cache that would not apply to conventional caching mechanisms. Different management strategies will have varying impact on complexity/performance measures.
The core technologies of fault tolerant subsystem design and high transaction processing capabilities support new architectures and platforms to create product differentiation through performance. High performance subsystems have commanded, and will continue to command, higher margins than those based on contemporary features and capacity. Like other performance driven manufacturers of all products, low end commodity machines follow the high performance flagship product.
The subsystem in accordance with this invention exploits the cost and high reliability characteristics of high volume, widely available small form factor disks drives and standard processor platforms. The system incorporates components of such high reliability or sufficient spares such that hot pluggable Customer Replaceable Units (CRU's) are not necessary to ensure adequate service life. The present invention is well suited to advantageously utilize the 1.8" (or smaller) disk drives, as well as IBM PC, Mips PC, or Dec Alpha PC compatible motherboards. It can employ purchased multitasking operating systems and standard power supplies.
The advantages of this approach are manifold. These include exploitation of contemporary core technologies (not mere implementations), dual controller/fault tolerant storage subsystems, environmental/configuration sense and control, controllers based on PC technology, development tools that are numerous, cheap, and sophisticated, volumes and competition which jointly keep the cost per MIP very low, third party development of faster controllers, third party interface hardware and driver software availability, and third party operating systems.
The present invention is concerned with controllers that execute data exchanges between requesting host computers, and one or more satellite data storage units associated with that controller. The present invention can accommodate implementation in conjunction with a caching disk array controller in a fault tolerant disk array subsystem.
A controller in which one feature of the present invention is useful has a plurality of elements arranged to receive data exchange controlling commands from a remote computer. These commands are utilized in conjunction with a fast memory to buffer data accompanying such commands between the computer and at least one satellite data storage unit, such as an array of disk drives. The memory controller includes a subset of elements whose primary purpose is for retrieving data from the fast memory for transfer to an output terminal.
Apparatus in accordance with this invention provides interfacing between a host data processing device and a subsystem for storing large quantities of data. A controller is coupled for exchanging data and commands with the host, and with the subsystem. A plurality of low cost disks are coupled to this controller. The controller responds to commands from the host to read data from an address in the subsystem by inspecting the contents of the array of low cost disks to identify the presence of data corresponding to the address from the host. The controller transfers the data from the host specified data address from the disk to the host if the data is found to reside there.
This controller can also function upon a failure to find data in the disk array corresponding to the host specified address by recovering the data from the subsystem for both transfer to the host and storage in a plurality of disks in the array. The controller can also sense the disk having its read/write head closest to the requested data by the host for producing that data from the sensed disk.
The controller can further determine the time required for accommodating any previously occurring operations with the disk array before determining which disk has its said head closest to the data associated with a given read request from the host.
The method of this invention utilizes a plurality of low cost disks for interfacing between a host data processing device and a subsystem capable of storing large quantities of data. This method includes the step of receiving data exchanging commands from the host, and responding to commands from the host to read data from an address in the subsystem by inspecting the contents of the disks in the array. This inspection is to determine whether the data corresponding to the address is present in at least one of the disks.
Data from the specified address is transferred from one of the disks to the host in response to a favorable result from the inspecting step. Conversely, a failure to produce a positive result from the inspecting step results in the steps of recovering the data from the subsystem, transferring that recovered data to the requesting host, and storing that recovered data in a plurality of disks in the array.
Once presence of the specified data on the disks of the array is determined, the disk having its read/write head closest to that data requested by the host is selected, and the data is produced to the host from the selected disk. If necessary, the method of this invention includes the step of determining the time required for accommodating any previously occurring operations with the disks prior to performing the disk selecting step.
Those having normal skill in the art will recognize the foregoing and other objects, features, advantages and applications of the present invention from the following more detailed description of the preferred embodiments as illustrated in the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a system block diagram of a disk based disk array coupled to perform interfacing between a host and a mass data storage subsystem in accordance with the present invention.
FIG. 2 shows a typical circuit board module configuration implementing the present invention.
FIG. 3 is a physical depiction of a typical disk mounting board suitable for attachment to a motherboard shown in FIG. 2.
FIG. 4 is block diagram of a logical depiction of the disk subsystem in accordance with the present invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
The storage hierarchy associated with the various contemporary storage configurations appears as follows in order of highest cost but fastest performance first and lowest cost but slowest performance last:
1. The registers of a Microprocessor;
2. An on-chip cache;
3. An off-chip cache;
4. Main memory;
5. I/O buffers;
6. A solid state disk cache;
7. A disk based disk cache;
8. A high performance disk;
9. A high capacity disk;
10. Slower high capacity disks; and
11. Optical, tape and/or library.
A storage subsystem that has the MB cost of disk coupled with the performance of many disks operated in parallel can fill several intermediate slots in this hierarchy. Spin synchronizing of the disks can help keep disk access times relatively low. Further down the hierarchy, inexpensive controllers coupled to an array in RAID1 configurations can yield high I/O rates.
Still further down the hierarchy, RAID5 configurations reduce the cost of protected storage with small redundancy groups and higher capacity disk (more data under each disk head). Even higher capacity, but slower, configurations of protected data can be built with high capacity drives and large redundancy groups; i.e., 35+1. All these products can be based on a common purchased hardware platform and contemporary developed ASIC based daughter cards. RAID3 is supported with daughter cards with flow through parity generators.
The preferred embodiments of the present invention are herein described in the environment of a data processing system, including at least one remote host computer, such as host 10 in FIG. 1. Host 10 is in a relatively remote location with regard to disk subsystems responsive to interface exchanging local controller 20. Host 10 is in bidirectional communication with controller 20 of a disk based disk cache subsystem 16 via link 11.
Controller 20 employs its own buffer to interface with a separate disk based disk cache array 22 via bidirectional connections, such as connector 15. Fully redundant data paths interconnect the host with the controllers, as well as between the controllers. Controller 20 can include independent paths to write data to its memory in a mirrored fashion so that data is protected against loss.
FIGS. 1 and 2 illustrate the use of a plurality of disk drives 22 with FIG. 2 presenting the physical top view of a board implemented in accordance with the present invention. Floppy disk drive 45 is included for introducing programs into the controllers and storage units of board 40. Power supply 46 renders board 40 self-contained, while battery 48 provides temporary back-up power for board 40. The controller 20 module includes a processor chip with its associated high speed registers and buffer memory.
The system shown in FIG. 1 is an improvement over either directly coupling host 10 to the high volume data storage subsystem 25, or using a solid state type device, such as caching through use of a RAM for such interfacing. As to the former situation, the improvement is in that it significantly offloads the host computer from dedicated disk management tasks. With regard to the latter, the high cost of solid state interfacing devices is significantly avoided by a large margin, while providing an acceptable compromise in approximating the operating speed thereof.
Array 22 as shown in FIG. 2 includes a printed circuit (PC) board 50. The base 51 of board 50 is attached to motherboard 40 via connector 52 shown in FIG. 3. Six small disk drives 53-58 (1.8-inch disk drives, for example) are attached to base 51 of PC board 50. The host interface 11 and the interface 24 to the mass data storage subsystem are likewise connected as boards to motherboard 50.
FIG. 4 presents the logical diagram of the disc drives 53-58 which communicate in pairs through standard disk drive interfaces 61, 62 and 63. The IDE standard for a PC-style disk drive interface handles pairs of drives, and could suffice for interfaces 61-63. Thus, disks 53-58 are the disks of the disk based disc cache interfacing system, while the other disks shown in array 22 might actually provide the disk storage devices for disk subsystem 25 possibly under the supervision of another controller (not shown). Conversely, an entirely separate high capacity data storage device can independently provide the subsystem 25 functions.
Internal data bus 59 can take the form of EISA, VESA or PCI types of standard disk drive interfaces. Application Specific Integrated Circuit (ASIC) 60 functions in response to commanding signals from the controller 20 to accomplish actual data exchanges with disks 53-58. ASIC 60 is substantially subservient to controller 20 to address the disk drives for storing or retrieving data.
Accordingly, host 10 interfaces with the disk based disk cache on board 40. Small Computer System Interface (SCSI) type connections are well suited for host interface 11, as well as interface 24. Both commands and data to and from the host computers 10 are handled via connections 11, all of which can occur concurrently. Through local busses, local processor 20 strips host 10 originated command signals from the interfaces to direct the operation of its fast memory elements and disk array 22 in handling the data associated with those commands.
Controller 20 determines the allocation of low cost disk array 22 in transferring data across interface 24 for storage in low cost (but low speed) disk subsystem 25. Typically, subsystem 25 includes its own controller to handle data exchanges coordinated with controller 20. A typical board is shown in FIG. 2 wherein interfacing modules 11 and 24 are coupled to cooperate with controller 20. Array 22 is made of a multiplicity of small disk drives which can encompass both the disk cache array 50 and, if desired, the disks of mass storage system 25 in FIG. 1.
A variety of possible disk based disk cache management strategies are possible. The mechanical characteristics and the size of the disk based disk cache suggest special constraints for managing the disk based disk cache that would not apply to conventional caching mechanisms. Different management strategies will have varying impact on complexity/performance measures. The following outlines several strategies potentially available for application in managing disk based cache systems.
A direct mapped strategy uses a simple function, such as a modulo operation, to map logical blocks to a physical location. A direct mapped strategy always writes a specific logical block to the same physical location. Therefore, the search entails a constant time segment.
A typical direct mapped write operation writes N copies of the data to the disk based disk cache comprised of N disks with one copy to each disk. In fault tolerant systems, the host may be signalled that the write operation is complete as soon as two of the N writes are completed. The logical write operation need not wait for the completion of all physical operations.
Unlike write operations, direct mapped read operations only need to access one device within the disk based disk cache. Therefore, the cache management strategy should select the device which can most quickly access the data. The factors that affect device access time are seek and rotational latency of each candidate drive, and the time necessary to complete previously queued operations for that drive. The cache management strategy minimizes device queuing by selecting the device which can most quickly access the data. Device rotational synchronization can minimize device latency. Devices are preferably synchronized so that the rotation of each device is offset by 1/N (where N is the number of devices in the system).
In direct mapping, the drives of array 22 can be considered to represent a linear set of logical data storage addresses with each sector stacked on top of the other. If, for example, there are twenty drives, each with twenty addressable sectors, there are four-hundred addressable sectors. The access time for all those sectors is not the same. It depends upon the rotational latency and the seek latency of each individual drive with regard to the actual location of the read/write head.
The number of bytes of data retainable by array 22 is markedly smaller than subsystem 25 can store. Direct map is a relatively simple algorithm. A certain number of bits describe the address of data in store 25, but it is possible to ignore the top of the address as this identifies the location of that byte in storage array 22. For instance, if store 22 has 65,000 locations with sixteen bits of address while store 25 has 4 gigabytes located in thirty-two address bits, a byte in store 22 shares addresses with 65K locations of store 25. Store 22 is selected to have enough capacity to hold the most important data that is used frequently by host 10. Data which becomes unimportant is replaced by some other data that has acquired importance in the system operation.
Host 10 specifies a particular address associated with the subsystem 25 storage. The lower segment of the address is used by a straightforward algorithm that allows the controller 20 to map into the disk cache. When host 10 requests a read operation from a thirty-two bit address, the disk cache controller 20 looks at the lower sixteen bits. Controller 20 retrieves the byte in conjunction with a tag or page frame number which completes identification of the location address with respect to the storage in subsystem 25.
Controller 20 recognizes that a match of the upper sixteen address bits represents data contained at the address specified by the lower sixteen bits. Controller 20 thus recognizes that the data is in the cache memory 50, and therefore can produce that data to host 10 with minimum delay. A failure to match means that access to storage subsystem 25 is needed. However, the retrieved data is stored in cache 50, and also transferred to host 10.
In the exemplary embodiment herein described, the disk 53-58 array on board 50 is designated as the disk based disk cache. On a write operation specified by host 10, the data is passed through to subsystem 25 for storage. The data is likewise placed in a cache 50 location at the location specified by the lower sixteen-bits of the address from host 10. The controller 20 might place the data on all of the drives associated with cache 50. A subsequent request for a read of that same data by host 10 results in controller 20 determining where the request resides in the queue of operations, and which read/write head of one of the drives on board 50 is closest to that data. Controller 20 knows where each disk of the cache is in its rotation.
Three operations involve time in association with an I/O function. The first relates to the wait in a queue of other I/O operation requests ahead of the request under consideration. The next time increment is the latency time which stems from the time it takes a read/write head to acquire an appropriate position over the data. The final time increment is the transfer time associated with acquisition of the data from the disk, and actual transfer to the requesting host or other device. The queuing and latency times are minimized by the processor of controller 20.
In operation, the processor of controller 20 in accordance with the present invention responds to a read request from host 10 by inspecting the contents of its associated disk cache. If the address of the requested data fails to match the disk cache stored data, a decision is made to pass the data read request directly through to the mass data storage device 25. The data acquisition is accomplished with substantially the same time increment as would occur if host 10 were directly coupled to storage subsystem 25.
However, when a match does occur, controller 20 recognizes that it is possible to retrieve that data from the cache storage, and return it to host 10 at a considerably faster rate than if the request were directly transferred to subsystem 25. The use of a plurality of low cost disk drives for the cache with common data stored thereon and the recognition of which disk has its read/write head closest to that data renders it possible to rapidly acquire and transfer the data to the requesting host 10.
Write commands from the host 10 are immediately recognized, and promptly passed to storage subsystem 25 without delay.
Another disk based disk cache management strategy is a set associative strategy. Set association uses a simple function (like a modulo operation) to map a logical block address to a table entry. Each table entry contains a fixed number of physical locations in which the logical block might be located. This approach helps alleviate thrashing that sometimes occurs for some workloads with a direct mapped strategy.
Multiple variations of set association are possible depending upon the eviction algorithm used to manage the table entries. For example, the logical data within the table entry can be evicted in a random, revolving, least recently used (LRU) or fastest fit algorithm. The optimum table entry management approach depends upon the cache workload.
A fully associative LRU cache management strategy allows any logical data block to be mapped to any physical location. With a true LRU, logical write operations evict the least recently used logical data block. Logical read operations use an index mechanism, such as a hash table, to find the physical location of the logical data. This approach favors cache workloads with a high locality of reference.
The fully associative, fastest fit cache management strategy evicts the closest possible physical location in order to optimize the write operation. Due to read operation interspersed between the write operations, logical write operations will cause each physical disk to evict different data. Therefore, the fastest fit strategy is not a mirroring approach. Writes may be optimized at the expense of slower reads or even cache misses. Reads require an index mechanism, such as a hash table, to find the physical location of the logical data.
Another disk based disk cache management strategy is the fully associative, hybrid LRU/fastest fit strategy. Instead of evicting the least recently used data item, a hybrid system searches the N least recently used entries to find the fastest fit. The strategy offers some write performance without sacrificing cache effectiveness. The meta data required by this strategy is the same as the LRU strategy.
While the exemplary preferred embodiments of the present invention are described herein with particularity, those having normal skill in the art will recognize various changes, modifications, additions and applications other than those specifically mentioned herein without departing from the spirit of this invention.
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Large numbers of relatively small (e.g., 1.8" or smaller) off-the-shelf disk drives are controlled to maximize the highest throughput performance at the least cost between a host computer and a mass storage subsystem. Host data is stored redundantly so as to form a cache. The controller recognizes data contained in its associated disk cache so as to produce that data to a requesting host with minimum delay. Data not in the disk cache as well as write commands are transferred to the controller of a mass storage subsystem with no substantial delay.
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RELATED APPLICATIONS
[0001] This application is a divisional of application Ser. No. 14/814,013, filed Jul. 30, 2015, which is a divisional of application Ser. No. 14/388,012, filed Sep. 25, 2014, now abandoned, which was the National Stage filing of International PCT/JP2013/058104, filed Mar. 21, 2013, the entirety of which is herein incorporated by reference.
TECHNICAL FIELD
[0002] The present invention relates to drugs capable of contributing to enhancement of agonist activity for PPARs, by which improvement of lifestyle diseases, particularly metabolic syndromes can be enhanced.
BACKGROUND ART
[0003] As PPARs (peroxisome proliferator-activated receptor) in bodies of vertebrates like humans, PPARα and PPARγ are currently known, and PPARδ (β) has been recently found. In the present Specification, these are collectively called PPARs.
[0004] Among them, it is known that PPARα corresponds to hypertension and arteriosclerosis resulting from adhesion of neutral fat to a vessel wall and has a function to activate lipase, which is an enzyme for decomposing neutral fat. Some medicines for the above-mentioned function have been already developed.
[0005] In addition, PPARγ draws attention as a receptor which can enhance insulin sensitivities of tissues, and it is known that diabetes or the like can be prevented by appropriately activating PPARγ to improve insulin resistance. Some medicines for this purpose have been developed.
LIST OF CITATION
Patent Document
[0006] Patent Document 1: JP 2007-112720 A1
[0007] Patent Document 2: WO 2007/007757
SUMMARY OF INVENTION
Technical Problem to be Solved
[0008] Patent Document 1 is an invention related to a medicine primarily for enhancing the agonist activity for PPARα, which includes a fibrate-based drug as an active ingredient in order to contribute to prevention or treatment of metabolic syndromes. Patent Document 2 is an invention related to a medicine primarily for enhancing the sensitivity of PPARγ.
[0009] As mentioned above, the known PPARs have a plurality of above-mentioned subclasses of α, γ and δ, each of which is supposed to have a specific active function. However, in pathological view, there are more complex chained mechanisms. Specifically, hyperlipidemia results from neutral fat adhering to a vessel wall, and this fat is also related to blood glucose. That is, if the blood glucose cannot be appropriately controlled, intracellular fat is accumulated and causes obesity, which is one of the recently controversial characteristics of metabolic syndrome. Thus, symptoms of hyperlipidemia, diabetes and metabolic syndrome are connected with each other, and even if only one symptom of them is targeted, they are not radically treated. That is a problem. In particular, although metabolic syndrome shows a phenomenon that a symptom of obesity is exhibited by fat excessively accumulated in fat cells universally existing everywhere in a body, it has been elucidated that PPARδ is promising as a substance showing effective agonist activity on the fat cells universally existing in such a manner. However, in fact, innovative chemical structures, compounds or extracts as medicines for effectively activating PPARδ have not been proposed yet.
[0010] An object of the present invention is to disclose a medicine which can activate PPARδ which is supposed to be effective in metabolic syndrome treatment conventionally considered to be difficult, to disclose a medicine which can concurrently enhance both PPARα and PPARγ agonist activities and also be effective in treatments of hyperlipidemia and diabetes, and to disclose a medicine which can be utilized in total improvement and treatment for improving lifestyle diseases.
Solution to Problem
[0011] In the present invention, the composition enhancing the agonist activity for PPARs was sought in naturally-derived medium chain fatty acids and their derivatives. The medium chain fatty acids and their derivatives were focused for the following inference. That is, higher animals like humans take, as foods, higher fatty acids (long chain fatty acids) such as palmitic acid, stearic acid, linoleic acid, linolenic acid, arachidonic acid, eicosapentaenoic acid or docosahexaenoic acid contained in plants and animals, metabolize them with β-oxidation in the body, and consume them as energy sources. In addition to the application as the energy sources, some fatty acids such as arachidonic acid are once taken into the body as starting materials for important biological activity and used for maintaining vital phenomenon phenomena while being free as required. In addition, eicosapentaenoic acid, docosahexaenoic acid and the like are also supposed to be associated with prevention of lifestyle diseases such as hypertension. These higher fatty acids are decomposed, through medium chain fatty acids such as octanoic acid, decanoic acid and dodecanoic acid as intermediates by β-oxidation, into short chain fatty acids such as acetic acid, propionic acid and butanoic acid by further β-oxidation, but conventionally humans have not been supposed to utilize medium chain fatty acids. Accordingly, while higher fatty acids are directly associated with vital phenomenon phenomena as nutrients and physiologically active substances so that they have been studied well, the importance of medium chain fatty acids has not been enough discussed enough. However, each of some animals, like insects, and plants successfully utilize the medium chain fatty acids so as to maintain its their species as members in the ecosystem. In particular, pheromones of insects contain a large amount of medium chain fatty acids and their derivatives, and royal jelly of bees and constituents of a queen bee substance also contain the medium chain fatty acid derivatives. In addition, humans take bee products as foods, and have been utilized humans utilize not only honey but also propolis, pollen dumpling, royal jelly and bees wax as foods. Thus, the inventors focused on medium chain fatty acids such as decanoic acid and decenoic acid contained in royal jelly, and expected that these derivatives had some positive impacts on the physiological activity of humans. As a further basis, human must have utilized a medium chain fatty acid at least once in the course of evolution, and it was also focused that a receptor of medium chain fatty acid remained as a trace even now, through evolution.
[0012] In addition, as components which exhibit nuclear receptors PPARα agonist activity, PPARγ agonist activity and PPARδ agonist activity, the research was advanced on medium chain fatty acid ester bodies among the medium chain fatty acids. As a result, it was found that a medium chain fatty acid with a lactone structure (γ, δ, ε ) had the activity.
[0000]
[0013] When activities of the above-described three lactone structures, γ-decanolactone (Chemical formula 1), δ-decanolactone (Chemical formula 2) and ε-decanolactone (Chemical formula 3) were verified, the δ-decanolactone (Chemical formula 2) showed a relatively strong activity, and as a size of the lactone ring, six-membered ring was suitable.
[0014] Subsequently, compositions having the following structures were prepared and the activity of them was studied in order to verify the influences of the aliphatic chain lengths.
[0015] δ-hexanolactone (6-methyltetrahydro-2H-pyran-2-one),
[0016] δ-octanolactone (6-propyltetrahydro-2H-pyran-2-one),
[0017] δ-nonanolactone (6-butyltetrahydro-2H-pyran-2-one),
[0018] δ-decanolactone (6-pentyltetrahydro-2H-pyran-2-one),
[0019] δ-undecanolactone (6-hexyltetrahydro-2H-pyran-2-one),
[0020] δ-docecanolactone (6-heptyltetrahydro-2H-pyran-2-one),
[0021] δ-tridecanolactone (6-octyltetrahydro-2H-pyran-2-one), and
[0022] δ-tetradecanolactone (6-nonyltetrahydro-2H-pyran-2-one).
[0000] As a result, the δ-nonanolactone (carbon number in the side chain: C4, Chemical formula 4), δ-decanolactone (carbon number in the side chain: C5, Chemical formula 5) and δ-undecanolactone (carbon number in the side chain: C6, Chemical formula 6) respectively showed the strong agonist activity. The agonist activity was observed not only in PPARδas originally expected, but also in PPARα and PPARγ.
[0000]
[0023] Subsequently, in order to enhance the activity intensity, α and β positions of each δ lactone ring were substituted for double bonds to obtain 6-butyl-5,6-dihydro-2H-pyran-2-one (Chemical formula 7), 6-pentyl-5,6-dihydro-2H-pyran-2-one (Chemical formula 8) and 6-hexyl-5,6-dihydro-2H-pyran-2-one (Chemical formula 9).
[0000]
[0024] The present invention is directed to an application for enhancing the PPARs agonist activity of the known compounds comprising Chemical formulae 7 and 8 (carbon number C9, C10), and a structure and an application of novel compounds having a lactone structure comprising Chemical formula 9 (C11). That is, these compounds have efficacies to enhance the PPARα, δ and γ agonist activities and are utilized as an improving drug for lifestyle diseases.
[0025] A synthetic method for each compound is as below.
(Chemical Formula 7)
[0026] A solution of diisopropylamine (1.21 ml, 8.63 mmol) in THF (tetrahydrofuran) (33 ml) was cooled to −78° C. under a nitrogen atmosphere, to which a butyllithium-hexane solution (1.1 M, 7.27 ml, 8.00 mmol) was added, and 10 minutes later, a solution of 6-butyltetrahydro-2H-pyran-2-one (1.00 g, 6.40 mmol) in THF (2 ml) was dropped, and stirred for 10 minutes. Subsequently, a solution of phenylselenyl chloride (1.19 g, 6.21 mmol) in THF (5 ml) was slowly dropped, and stirred at −78° C. for another 30 minutes, to which a saturated ammonium chloride solution was dropped to terminate the reaction. The reaction mixture was extracted with hexane, and its organic layer was dried with anhydrous sodium sulfate and distilled off under reduced pressure. The residue was purified by a silica gel column chromatography (hexane-ethyl acetate 10:1-8:1-6:1) so as to obtain a pure phenylselenide (842 mg, 42%) as a diastereomer mixture.
[0027] A solution of phenylselenide (842 mg, 2.70 mmol) in THF (14 ml) was cooled to 0° C., to which sodium bicarbonate (454 mg, 5.40 mmol) was added, and 30% hydrogen peroxide water (1.53 g, 45.0 mmol) was slowly dropped while stirring. This was stirred at 0° C. for another one hour, to which a sodium thiosulfate aqueous solution was added to terminate the reaction. The reaction mixture was extracted with chloroform, and its organic layer was dried with anhydrous sodium sulfate and distilled off under reduced pressure. The residue was purified by a silica gel column chromatography (hexane-ethyl acetate 5:1-4:1) so as to obtain a pure desired substance (257 mg, 62%).
[0028] A pale yellow oily substance; NMR δ H (CDCl 3 ): 6.89 (1H, ddd, J=10.2, 5.6, 3.6 Hz), 6.03 (1H, dt, J=10.2, 2.0 Hz), 4.43 (1H, m), 2.34 (2H, m), 1.80 (1H, m), 1.65 (1H, m), 1.50 (1H, m), 1.37 (3H, m), 0.92 (3H, t, J=7.0 Hz).
(Chemical Formula 8)
[0029] 6-Pentyltetrahydro-2H-pyran-2-one (1.00 g, 5.87 mmol), diisopropylamine (1.08 ml, 7.71 mmol), a butyllithium-hexane solution (1.0 M, 6.48 ml, 6.48 mmol), phenylselenyl chloride (1.71 g, 8.93 mmol) were reacted, post-treated and purified under the same conditions to obtain a pure phenylselenide (1.39 g, 73%).
[0030] Phenylselenide (1.39 g, 4.27 mmol), sodium bicarbonate (719 mg, 8.56 mmol) and 30% hydrogen peroxide water (2.43 g, 71.4 mmol) were reacted, post-treated and purified in the same manner to obtain a pure desired substance (342 mg, 47%).
[0031] A pale yellow oily substance; NMR δ H (CDCl 3 ): 6.89 (1H, ddd, J=9.6, 5.6, 3.4 Hz), 6.02 (1H, dt, J=9.6, 1.2 Hz), 4.43 (1H, m), 2.34 (2H, m), 1.79 (1H, m), 1.65 (1H, m), 1.52 (1H, m), 1.41 (1H, m), 1.32 (4H, m), 0.90 (3H, t, J=6.6 Hz).
(Chemical Formula 9)
[0032] 6-Hexyltetrahydro-2H-pyran-2-one (1.00 g, 5.43 mmol), diisopropylamine (0.99 ml, 7.06 mmol), a butyllithium-hexane solution (1.1 M, 5.92 ml, 6.51 mmol), phenylselenyl chloride (1.56 g, 8.15 mmol) were reacted, post-treated and purified under the same conditions to obtain a pure phenylselenide (1.04 g, 56%).
[0033] Phenylselenide (1.04 g, 3.06 mmol), sodium bicarbonate (512 mg, 6.09 mmol) and 30% hydrogen peroxide water (1.73 g, 50.9 mmol) were reacted, post-treated and purified in the same manner to obtain a pure desired substance (521 mg, 94%).
[0034] A pale yellow oily substance; NMR δ H (CDCl 3 ): 6.89 (1H, ddd, J=9.4, 4.8, 3.2 Hz), 6.03 (1H, dt, J=9.4, 2.0 Hz), 4.42 (1H, m), 2.34 (2H, m), 1.80 (1H, m), 1.65 (1H, m), 1.50 (1H, m), 1.30 (7H, m), 0.89 (3H, t, J=6.8 Hz).
[0035] [Among the above-mentioned three compounds, the compound shown in Chemical formula 7 has a composition known as an essential oil of lauraceous plants such as Cryptocarya massoy . In addition, the compound shown in Chemical formula 8 is also a known compound known as massoialactone contained in an unprocessed cane sugar. The compound shown in Chemical compound 9 is a novel compound.
Advantageous Effects of Invention
[0036] Lifestyle diseases such as hyperlipidemia, diabetes and metabolic syndrome can be comprehensively improved by appropriately administering the drug of the present invention.
BRIEF DESCRIPTION OF DRAWINGS
[0037] FIG. 1 is a graph evaluating the PPARα agonist activity of the compounds of the present invention with Comparative Examples.
[0038] FIG. 2 is a graph evaluating the PPARδ agonist activity of the compounds of the present invention with Comparative Examples.
[0039] FIG. 3 is a graph evaluating the PPARγ agonist activity of the compounds of the present invention with Comparative Examples.
[0040] FIG. 4 is a photograph showing the agonist activity test of the compound of Chemical formula 9 for PPARα.
[0041] FIG. 5 is a photograph showing the agonist activity test of the compound of Chemical formula 9 for PPARδ.
[0042] FIG. 6 is a graph comparing activities by the difference in the stereo-structure of the compound of Chemical formula 9
DESCRIPTION OF EMBODIMENTS
[0043] The compounds having lactone structures shown in the present invention are suitable as preventive or ameliorating drugs for hyperlipidemia, ameliorating drugs for diabetes and preventive or ameliorating drugs for metabolic syndrome, and intended to be administered as oral agents. Embodiments of the oral agents may include a tablet, a granule, a powder, and a capsule in its original diluted oily state.
EXAMPLES
[0044] The agonist activities of PPARα, PPARδ and PPARγ, respectively, were visually verified by a reporter gene assaying method using COS-1 cells so as to evaluate them. The evaluation method is as below.
[0045] The COS-1 cells were collected by trypsinization, centrifuged (1000 rpm, 4° C., 3 min.), and then seeded on a 60 mm Petri dish for cultivation in a density of 6×10 5 cells/well. After cultivation at 37° C. under 5% CO 2 for 24 hours, cells were transformed using EFFECTENE® Transfection Reagent (QIAGEN®). EC buffer(150 ml), pPPARα-GAL4 (0.25 μg), pPPARδ-GAL4 (0.25 μg) or pPPARγ-GAL4 (0.25 μg), p17M2G (1 μg), pSEAP control vector (1 μg) were put into a 1.5 ml Eppendorf tube, to which 18 μl of Enhancer was added, and stirred by a vortex for 1 second. This was left to stand at room temperature for 3 minutes, to which 25 μl of Effectene was added, stirred by the voltex for 10 seconds, and left to stand at room temperature for 7 minutes. Simultaneously, the medium for transformation in the 60 mm Petri dish for cultivation was removed, to which 40 ml of medium was added to exchange the medium. Seven minutes later, 1 ml of medium was added to the Eppendorf tube, suspended twice, dropped to a 60 mm Petri dish for cultivation, and cultivated 37° C. under 5% CO 2 for 16 hours.
[0046] The cells were collected by trypsinization after 16 hours, centrifuged (1000 rpm, 4° C., 3 min.), and then suspended in 6 ml of medium, and seeded on a 96-well plate at 125 μl/well. The sample solution was added at 1.25 μl/well after 2-3 hours, and cultivated 37° C. under 5% CO 2 for 24 hours. Then the medium was collected at 25 μl/well, a secreted alkaline phosphatase (SEAP) activity was measured using GREAT ESCAPE™ SEAP (Clontech Laboratories, Inc.) kit. As the outline, 1× dilution buffer was added at 25 μl/well, mildly stirred, sealed with a scotch tape, and incubated at 65° C. for 30 minutes. Subsequently, it was cooled at 4° C., and returned to room temperature, then an assay buffer was added at 90 μl/well. It was left to stand at room temperature for 5 minutes, to which 10 μl of MUP solution was added at 10 μl/well. At room temperature, it was left to stand in a dark room for 1 hour, and then fluorescence intensity based on 4-methylumbelliferyl phosphate (Ex=360 nm, Em=460 nm) was measured.
[0047] In order to measure the activity for PPARα, luciferase activity measuring cocktail (Invitrogen) was added to other 96 well plate at 100 μl/well to measure the emission intensity. Compensation among each well was performed by dividing the measured value of the luciferase activity by the SEAP activity value.
[0048] FIG. 1 shows a graph evaluating the agonist activity for PPARα, the compounds shown as raw materials are the compounds represented by Chemical formulae 4 to 6 respectively before substitution for double bonds, and the compounds shown as oxidants are Chemical formulae. 7 to 9, i.e. C9 to C11 in which the α and β positions in the lactone ring of the raw material are substituted by double bonds, which are the compounds of the present invention. In addition, results of the compounds of the carbon numbers C8 and C12 were similarly shown as comparative examples. The structure of carbon number C8 lacks one side chain in the carbon number C9, and the structure of carbon number C12 adds one side chain to the carbon number C11, in which no double bond is provided. The carbon numbers C9 to C11 represents numbers of the carbon atoms in the compounds of Chemical formulae 4 to 6 and Chemical formulae 7 to 9. As shown in FIG. 1 , a fibrate-based control substance WY14643 was used for evaluating the PPARα agonist activity, and a case of the 50 μM concentration was designated as a ratio 1.00. As the results, a sample of the same concentration as of the control substance showed higher activity than that of an indicator. Also, a sample adjusted to the one-tenth concentration, i.e. the 5 μM concentration showed activity almost equal to that of the control substance. In addition, since each oxidant showed an activity superior to that of the raw material, it was found that the compound in which the α and β positions in the lactone ring were substituted by double bonds had more preferable activity. In conclusion, all substances of the present invention can be expected as agents for enhancing the agonist activity for PPARα. Whereas, C8 shown as a comparative example can hardly be expected for the activity in a case of 5 μM dilution, and C12 did not show strong activity expected by the inventor in both cases of 50 μM and 5 μM.
[0049] FIG. 2 shows a graph evaluating the PPARδ agonist activity, the same compounds as those shown in FIG. 1 are used, and 1 nM of GW0742 was used as the control substance. Concentrations of the samples to be evaluated are 50 μM and 5 μM. For this evaluation, although each oxidant had high concentration, it did not show higher activity than that of the control substance. However, the control substance has characteristics that when its concentration is lower than 1 nM, its activity is extremely lowered, meanwhile the activity is not improved even by heightening the concentration. In addition, these deserve enough evaluation as results of comparison between the control substance which shows remarkable characteristics among the known substances and the oxidants of the present invention. On the other hand, C8 and C12 shown as comparative examples showed little activity in the result at 5 μM rather than the value at the concentration of 50 μM.
[0050] FIG. 3 shows a graph evaluating the PPARγ agonist activity, and 10 μM of Trogliazone was used as the control substance. Concentrations of the samples to be evaluated are 50 μM and 5 μM. When the concentrations of the oxidant samples were set to 50 μM, all oxidants showed higher activities than that of the control substance. Meanwhile, C8 and C12 shown as comparative examples showed only considerably lower activities than the values of C9 to C11 in the case of 50 μM concentration, and showed little activities in the case of 5 μM.
[0051] Since the present invention is originally directed to compounds having agonist activities for PPARα, δ and γ, oxidants of C9 to C11 (Chemical formulae 7 to 9) were identified based on the comprehensive evaluations of the activities of PPARα, δ and γ shown in FIGS. 1 to 3 . That is, all of the compounds having the structures of C9 to C11 showed effective agonist activities for PPARs.
[0052] Next, a novel compound C11 was focused, and further activity tests using HepG2 cells were carried out. FIG. 4 shows a photograph verifying the agonist activity of C11 for PPARα and shows the influence on human liver cells. In the figure, GAPDH represents a housekeeping indicator, ACS represents expression of lipid metabolism gene, and CPT1A represents expression of lipolytic gene. As a drug for comparison, Bezafibrate known as PPARα agonist activity enhancer was used with 50 μM dilution, and the compound C11 of the present invention was used at concentrations of 50 μM and 25 μM. As a result, when the C11 compound was administered, a gene expression at least equal to or greater than that of Bezafibrate could be verified.
[0053] Subsequently, an agonist activity test on fat cell differentiation induction-associated genes was similarly carried out for C11, and the results are shown in FIG. 5 . In this test, the differentiation induction method using 3T3-L1 cells was conducted. For preparing samples, a plate having a total of 24 depressions of 6 lines×4 rows was used, and a known mouse fat cells was used to observe PPARγ agonist activities. In relation to 5 samples shown in the figure, in order from the right, a sample without insulin administration, a sample dosed with 1.7 μM of insulin, a sample dosed with 25 μM of C11 compound, a sample dosed with 12 μM of C11 compound and a sample dosed with 6 μM of C11 compound are shown. CAPDH is a housekeeping indicator, C/EBPα is a control, and Adiponectine is an expressed gene. As is obvious from the results, all samples dosed with C11 showed effective activities.
[0054] Furthermore, regarding C10, it was verified whether the difference of the spatial structure affected the activity. C10 has R body and S body like Chemical formulae 10 and 11, and in FIG. 6 , three PPARs were compared with each other about whether the activities are different depending on the difference of the bodies. The results of three tests were averaged. As a result, it could be verified that there was no significant difference between activities of the R body and the S body. Thus, C10 is useful for efficient manufacture, because the spatial structure need not be taken into consideration in the manufacture. In relation to PPARα, there is a significant difference between values of the R and S bodies in the case of 25 μM, and the reason may be that a difference in any toxicity affected the values. Also, since C9 and C11 respectively have a structure that the number of the side chains differs from that of C10 by only 1 chain, it is considered that the difference in the spatial structure does not affect the activity like C10.
[0000]
(R)-6-pentyl-5,6-dihydro-2H-pyran-2-one
[0055]
(S)-6-pentyl-5,6-dihydro-2H-pyran-2-one
[0056] A synthesis method of Chemical formula 11 is as below.
[0057] A solution of diisopropylamine (1.1 ml, 7.7 mmol) in THF (33 ml) was cooled to −78° C. under a nitrogen atmosphere, to which a butyllithium-hexane solution (1.0 M, 6.5 ml, 8.0 mmol) was added, and 10 minutes later, a solution of 6-pentyltetrahydro-2H-pyran-2-one (10S) (1.0 g, 5.9 mmol) in THF (2 ml) was dropped, and stirred for 10 minutes. Subsequently, a solution of phenylselenyl chloride (1.2 g, 6.2 mmol) in THF (5 ml) was slowly dropped, and stirred at −78° C. for another 30 minutes, to which a saturated ammonium chloride solution was slowly dropped to terminate the reaction. The reaction mixture was extracted with ether, and its organic layer was dried with anhydrous sodium sulfate and distilled off under reduced pressure. When the residue was purified by a silica gel column chromatography (hexane-ethyl acetate 10:1-8:1-6:1), a pure phenylselenide (10S-M) (1.4 g, 78%) was obtained. A solution of phenylselenide (1.4 g, 2.7 mmol) in THF (14 ml) was cooled to 0° C., to which sodium bicarbonate (720 mg, 8.6 mmol) was added, and 30% hydrogen peroxide water (2.4 g, 70.0 mmol) was slowly dropped while stirring. This was stirred at 0° C. for another one hour, to which a sodium thiosulfate aqueous solution was added to terminate the reaction. The reaction mixture was extracted with chloroform, then its organic layer was dried with anhydrous sodium sulfate and distilled off under reduced pressure. When the residue was purified by a silica gel column chromatography (hexane-ethyl acetate 5:1-4:1), a pure (S)-6-pentyl-5,6-dihydro-2H-pyran-2-one (10S-D) (342 mg, 47%) was obtained.
[0058] Note that the synthesis of (R)-6-pentyl-5,6-dihydro-2H-pyran-2-one (10R-D) of Chemical formula 10 conforms to the above method.
[0059] Data on apparatus for Chemical formula 10 and Chemical formula 11 is as below.
[0060] (Chemical Formula 10)
[0061] colorless oil; [α] 25 D : −76.0° (c=0.1, CHCl 3 ); 1 H-NMR (400 MHz, CDCl 3 )δ: 0.90 (3H, t, J=6.8 Hz), 1.32 (4H, m), 1.41 (1H, m), 1.52 (1H, m), 1.65 (1H, m), 1.80 (1H, m), 2.34 (2H, m), 4.43 (1H, m), 6.02 (1H, dt, J=9.6, 1.7 Hz), 6.89 (1H, m); ESIMS (positive ion mode): m/z 191.0972[M+Na] − .
[0062] (Chemical Formula 11)
[0063] colorless oil; [α] 25 D : +112.6° (c=0.1, CHCl 3 ); 1 H-NMR (400 MHz, CDCl 3 )δ: 0.90 (3H, t, J=7.0 Hz), 1.32 (4H, m), 1.41 (1H, m), 1.52 (1H, m), 1.65 (1H, m), 1.80 (1H, m), 2.34 (2H, m), 4.42 (1H, m), 6.02 (1H, dt, J=10.0, 1.5 Hz), 6.89 (1H, m); ESIMS (positive ion mode): m/z 191.0974[M+Na] − .
INDUSTRIAL APPLICABILITY
[0064] The drug of the present invention can be obtained by synthesis, while its molecular weight is relatively small, its synthesis method is not complex, and it can be stably provided as a medicine. Therefore, its industrial utility is high.
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A lifestyle disease improving drug is disclosed that enhances PPARα, δ and γ agonist activities that includes a compound having the lactone structure in accordance with the chemical formula 6-alkyl-5,6-dihydro-2H-pyran-2-one, the alkyl containing 4, 5, or 6 carbons. Methods for enhancing PPARα, γ and δ agonist activities in vertebrates or medically treating a vertebrate are disclosed. The methods include providing a composition of an active ingredient, the lifestyle disease improving drug, in a biologically acceptable medium and administering an effective amount of the composition to a vertebrate.
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RELATED APPLICATIONS
The present application is a division of U.S. application Ser. No. 09/264,801, filed Mar. 9, 1999, entitled “Methods of Tissue Heart Assembly,” now U.S. Pat. No. 6,102,944, which is a continuation of U.S. application Ser. No. 08/826,408, filed Mar. 27, 1997, entitled “Tissue Heart Valves with Subassemblies,” now issued as U.S. Pat. No. 5,928,281.
FIELD OF THE INVENTION
The present invention is directed to tissue-type prosthetic heart valves and in particular to stents used in the fabrication of such valves.
BACKGROUND OF THE INVENTION
Prosthetic heart valves are used to replace damaged or diseased heart valves. In vertebrate animals, the heart is a hollow muscular organ having four pumping chambers: the left and right atria and the left and right ventricles, each provided with its own one-way valve. The natural heart valves are identified as the aortic, mitral (or bicuspid), tricuspid and pulmonary valves. Prosthetic heart valves can be used to replace any of these naturally occurring valves. Two primary types of heart valve replacements or prostheses are known. One is a mechanical-type heart valve that uses a pivoting mechanical closure to provide unidirectional blood flow. The other is a tissue-type or “bioprosthetic” valve which is constructed with natural-tissue valve leaflets which function much like a natural human heart valve, imitating the natural action of the flexible heart valve leaflets which seal against each other or coapt between adjacent tissue junctions known as commissures. Each type of prosthetic valve has its own attendant advantages and drawbacks.
Operating much like a rigid mechanical check valve, mechanical heart valves are robust and long lived but require that valve implant patients utilize blood thinners for the rest of their lives to prevent clotting. They also generate a clicking noise when the mechanical closure seats against the associated valve structure at each beat of the heart. In contrast, tissue-type valve leaflets are flexible, silent, and do not require the use of blood thinners. However, naturally occurring processes within the human body may attack and stiffen or “calcify” the tissue leaflets of the valve over time, particularly at high-stress areas of the valve such as at the commissure junctions between the valve leaflets and at the peripheral leaflet attachment points or “cusps” at the outer edge of each leaflet. Further, the valves are subject to stresses from constant mechanical operation within the body. Accordingly, the valves wear out over time and need to be replaced. Tissue-type heart valves are also considerably more difficult and time consuming to manufacture.
Though both mechanical-type and tissue-type heart valves must be manufactured to exacting standards and tolerances in order to function for years within the dynamic environment of a living patient's heart, mechanical-type replacement valves can be mass produced by utilizing mechanized processes and standardized parts. In contrast, highly trained and skilled assembly workers make tissue-type prosthetic valves by hand. Typically, tissue-type prosthetic valves are constructed by sewing two or three flexible natural tissue-leaflets to a generally circular supporting wire frame or stent. The wire frame or stent is constructed to provide a dimensionally stable support structure for the valve leaflets which imparts a certain degree of controlled flexibility to reduce stress on the leaflet tissue during valve closure. A biocompatible cloth covering on the wire frame or stent provides sewing attachment points for the leaflet commissures and cusps. Similarly, a cloth covered suture ring can be attached to the wire frame or stent to provide an attachment site for sewing the valve structure in position within the patient's heart during a surgical valve replacement procedure.
With over fifteen years of clinical experience supporting their utilization, tissue-type prosthetic heart valves have proven to be an unqualified success. Recently their use has been proposed in conjunction with mechanical artificial hearts and mechanical left ventricular assist devices (LVADs) in order to reduce damage to blood cells and the associated risk of clotting without using blood thinners. Accordingly, a need is developing for a tissue-type prosthetic heart valve that can be adapted for use in conjunction with such mechanical pumping systems. This developing need for adaptability has highlighted one of the drawbacks associated with tissue-type valves—namely, the time consuming and laborious hand-made assembly process. In order to provide consistent, high-quality tissue-type heart valves having stable, functional valve leaflets, highly skilled and highly experienced assembly personnel must meticulously wrap and sew each leaflet, and valve component into an approved, dimensionally appropriate valve assembly. Because of variations in tissue thickness, compliance and stitching, each completed valve assembly must be fine tuned using additional hand-crafted techniques to ensure proper coaptation and functional longevity of the valve leaflets. As a result, new challenges are being placed upon the manufacturers of tissue-type prosthetic valves in order to meet the increasing demand and the increasing range of uses for these invaluable devices.
Accordingly, consistent with the developing practice of the medical profession, there is a continuing need for improved tissue-type prosthetic heart valves which incorporate the lessons learned in clinical experience, particularly the reduction of stress on the valve leaflets while maintaining desirable structural and functional features. Additionally, there is a growing need for improved tissue-type prosthetic heart valves which can be adapted for use in a variety of positions within the natural heart or in mechanical pumps, such as artificial hearts or ventricular assist devices, as well as alternative locations in the circulatory system. Further, in order to address growing demand for these devices, there is a need for tissue-type heart valves that are simpler and easier to manufacture in a more consistent manner than are existing valves.
SUMMARY OF THE INVENTION
Directed to achieving the foregoing objective and to remedying the problems in the prior art, disclosed herein are novel tissue heart valve constructions and components thereof, and simplified methods of fabricating the same. The improved tissue heart valves of the present invention are fabricated to include standardized leaflet structure subassemblies that can be modified readily to adapt to different intended applications. Of equal importance, the leaflet structure subassemblies uniformly distribute tensile loads along the entire peripheral leaflet cusp, reducing stress points and significantly improving the long-term functionality of the valve assembly. As an added benefit of the present invention, the stability and adaptability of the tissue valve subassembly is achieved through simplified manufacturing processes utilizing fewer steps and subassemblies. This manufacturing protocol can be incorporated into branched, adaptable manufacturing techniques for the production of tissue heart valves having a variety of end uses. Further, these improved construction techniques expedite the overall manufacturing process and improve the consistency of the tissue valves so produced while simultaneously reducing the need for post-assembly fine tuning and quality-control procedures.
According to one aspect of the present invention, a tissue-type heart valve includes a dimensionally stable, pre-aligned tissue leaflet subassembly, a generally circular wireform, and a generally circular support stent. The wireform has a bottom surface dimensioned to receive the pre-aligned tissue leaflet subassembly in fixed, mating engagement. The support stent has an upper surface dimensioned to seat and fix in meeting engagement with the pre-aligned tissue leaflet subassembly which is fixedly disposed in mating engagement with the bottom surface of the wireform.
Pursuant to this construction, an exemplary tissue valve includes a plurality of tissue leaflets that are templated and attached together at their tips to form a dimensionally stable and dimensionally consistent coapting leaflet subassembly. Then, in what is essentially a single process, each of the leaflets of the subassembly is aligned with and individually sewn to a cloth-covered wireform, from the tip of one wireform commissure uniformly, around the leaflet cusp perimeter, to the tip of an adjacent wireform commissure. As a result, the sewed sutures act like similarly aligned staples, all of which equally take the loading force acting along the entire cusp of each of the pre-aligned, coapting leaflets. The resulting tissue-wireform structural assembly thereby formed reduces stress and potential fatigue at the leaflet suture interface by distributing stress evenly over the entire leaflet cusp from commissure to commissure. This improved, dimensionally stable, reduced-stress assembly is operatively attached to the top of a previously prepared cloth-covered stent to clamp the tissue leaflet cusps on a load-distributing cloth seat formed by the top of the cloth-covered stent without distorting the leaflets or disturbing their relative alignment and the resultant coaptation of their mating edges.
The stent is secured to the assembly with the commissures of the stent extending up into the corresponding commissures of the leaflet, wireform assembly. The stent itself can be formed of an inner polyester film support secured to a surgically acceptable metal ring such as an Elgiloy™ metal stiffener having a cloth cover cut, folded and sewn around the support and stiffener combination. Alternatively, instead of having an Elgiloy outer band and a laminated polyester film support, the two stent layers can both be polyester layers or a single piece stent having appropriately flexible commissure posts. Either stent construction provides support and dimensional stability for the valve structure extending from commissure to commissure and being evenly distributed around each leaflet. This assembly methodology allows the evenly sutured tissue of the leaflet cusps to be sandwiched between the wireform and the stent and to thereby further distribute the loading forces more evenly around the attachment site. Because the tissue leaflets experience lower, more evenly distributed stresses during operation, they are less likely to experience distortion in use. Thus, a more stable, long lived, functional closure or coaptation of the leaflets is provided by this even distribution of attachment forces.
A number of additional advantages result from the present invention and the stent construction utilized therein. For example, for each key area of the stent, the flexibility can be optimized or customized. If desired, the coapting tissue leaflet commissures can be made more or less flexible to allow for more or less deflection to relieve stresses on the tissue at closing or to fine tune the operation of the valve. Similarly, the base radial stiffness of the overall valve structure can be increased or decreased to preserve the roundness and shape of the valve.
Unlike a rigid mechanical valve, the stent does not act as a rigid heart valve structure but as a radially stable, yet axially flexible support. A rigid structure is unnecessary by utilizing the teachings of the present invention because the valve leaflets are dimensionally pre-aligned along their mutually coapting mating or sealing edges prior to being directly attached to the base of the cloth-covered wireform. As a result, the entire sealing aspect of the valve can be aligned in three dimensions at once without the variability previously experienced in the construction of prior art tissue-type valves. In addition to eliminating the need for post-assembly adjustment, this pre-alignment provides for consistency and simplicity in the manufacture of the valve structure. Further, the wire form functions as a template for suturing the leaflet cusps to the valve subassembly with uniform stitching from commissure tip to commissure tip. This produces a dimensionally consistent structure that can interface with the stent in a previously unobtainable uniform manner. The consistent dimensional integrity of the leaflet wireform subassembly enables the stent to function as a stress relieving support clamp which further secures the leaflet cusps in the valve structure to provide an added degree of stability and stress distribution. If desired, providing the top of the stent with a single or double fold of covering cloth provides the stent lip with a deformable cloth seat that assists in the distribution of load around the leaflet cusps and simplifies sewing the stent to the tissue leaflet wireform subassembly. Those skilled in the art will appreciate that attaching the stent to the tissue leaflet wireform functions to stabilize the projecting commissure posts of the valve subassembly without stiffening their desirable axial flexibility. This novel construction technique eliminates the need for separate commissure posts at the tissue leaflet commissures and also eliminates multiple tissue and cloth layers at the wireform commissure posts which adds to uniformity and consistency in valve production and eliminates assembly steps. As a result, valve manufacture is not only improved, but also simplified and expedited as well.
The stent also functions as an adaptable structural interface, allowing the tissue-wireform-stent structural subassembly to be attached to a variety of additional structures dependent upon intended valve placement and operating environments. For example, with the supporting stent secured to the tissue-wireform structural assembly, the resulting valve assembly can be attached to, for example, a suture ring, a flange or a conduit depending on the desired valve application. To form a conduit valve, the suture ring can be attached directly to the inflow or base of the stent to enable the implanting surgeon to sew the valve in place within the heart. Alternatively, when the valve is to be used for artificial hearts or for left ventricular assist devices (LVADs), a more rigid flange can be attached to the stent inflow to function as a mechanical mount. In some circumstances it may be desirable to form a conduit valve wherein flexible or rigid conduits are required to replace a missing portion of a patient's aorta or to interface with an artificial blood pumping device. In such circumstances, an inlet conduit may be attached to the stent inflow and, if desired, a corresponding outflow conduit can be attached inside or outside of the valve wireform. Unlike prior art tissue heart valves, the present invention provides this flexibility and adaptability of use because key valve components can be standardized for different types of valves or valve applications. This manufacturing and structural consistency also improves quality control and provides repeatability and consistency in the formation of the valves. It also simplifies final assembly that in turn provides for increased production rates without sacrificing consistent product quality.
More specifically, as part of the flexibility of the present invention, the stent is designed to be adaptable so that different ways of attaching the valve to its various intended applications can be accommodated. The novel construction that allows for this universal application results from the stent providing a complete uniform support to the dimensionally stable, pre-aligned wireform/leaflet subassembly. Because of this adaptability, the valve of the present invention can function in a variety of applications, including that of a temporary heart valve prosthesis within a circulatory support system using a relatively rigid flange or a conduit assembly rather than a standard soft sewing ring. Alternatively, the present invention can function as a prosthetic valve having a soft, scallop-shaped sewing ring for aortic positioning or a soft flat sewing ring for mitral positioning, or as a conduit valve by incorporating proximal and distal conduits attached on both the inflow and outflow valve ends. The outflow conduit can have a sinus shape to improve blood flow if desired. Within an artificial heart system, the valve of the present invention mimics the hemodynamic pumping action of the heart while sustaining the patient until a donor heart is located and successfully transplanted. In this application, both blood inflow and outflow functions can be accommodated by the present invention.
Other objects and advantages of the present invention will become more apparent to those persons having ordinary skill in the art to which the present invention pertains from the following description taken in conjunction with the accompanying drawings.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is an exploded perspective view of an exemplary heart valve of the present invention illustrating the assembly relationship of the standardized components and alternative valve attachment application structures;
FIG. 2 is a perspective view illustrating the step of templating and trimming exemplary leaflets used in making a tissue heart valve of the present invention;
FIG. 3 illustrates the initial steps of templating and pre-aligning the leaflets of the valve subassembly;
FIG. 4 shows additional steps in the pre-alignment of the valve leaflet subassembly;
FIG. 5 is an enlarged view illustrating an exemplary attachment step of the pre-aligned leaflets to a wireform commissure tip;
FIG. 6 is a perspective view illustrating the subsequent preliminary attachment of the exemplary leaflet cusps to the wireform of FIG. 5;
FIG. 7 is a perspective view illustrating the. uniform attachment of the perimeter cusps of leaflets to the cloth covered wireform;
FIG. 8 is an enlarged view of one of the pairs of attached leaflet tabs of FIG. 7 illustrating the uniform attachment of the cusps to the wireform commissure tip;
FIG. 9 is a perspective view illustrating the attachment of the exemplary tissue leaflet-wireform structural subassembly to an exemplary stent of the present invention;
FIG. 10 is an enlarged view of one of the pairs of leaflet tabs of FIG. 9 illustrating a further attachment step of the stent to the wireform at the commissure tip, clamping the leaflet cusps therebetween;
FIG. 11 is an enlarged view of one of the commissure tips of the tissue-wireform structural assembly of FIG. 10 illustrating the clamping of the leaflets by the stent;
FIG. 12 is a perspective view illustrating a final attachment step of the exemplary tissue-wireform structural assembly to the stent;
FIG. 13 is an enlarged view taken on circle 13 of FIG. 12 illustrating additional exemplary attachment techniques;
FIG. 14 is an enlarged view taken on circle 14 of FIG. 12 illustrating additional exemplary attachment techniques;
FIG. 15 is a perspective view illustrating an exemplary attachment step of the tissue leaflet tabs at the commissure tip;
FIG. 16 is a view similar to FIG. 15 illustrating an alternative attachment step;
FIG. 17 is an exploded perspective view illustrating an exemplary multi-piece stent formed of a flexible support and an associated stiffener of the present invention;
FIG. 18 is a perspective view illustrating the attachment of the support to the stiffener of FIG. 17;
FIG. 19 is a perspective view illustrating an initial step in the covering of the stent components of FIG. 18 with cloth;
FIG. 20 is an enlarged view of the top of FIG. 19 illustrating additional steps in the attachment of the cloth to the stent components;
FIG. 21 is a perspective view illustrating additional steps of fabricating sewing tabs for attaching the cloth to the stent components;
FIG. 22 is an enlarged view of a portion of FIG. 20 illustrating subsequent fabrication steps;
FIG. 23 is an enlarged cross-sectional view taken on line 23 — 23 of FIG. 22;
FIG. 24 is a view similar to FIG. 22 illustrating additional fabrication steps;
FIG. 25 is a perspective view of the cloth-covered stent of FIG. 18 illustrating the cloth seating lip;
FIG. 26 is an enlarged cross-sectional view on line 26 — 26 of FIG. 25 illustrating additional aspects of the fabrication of the exemplary stent assembly;
FIG. 27 is a perspective view illustrating initial components of an exemplary suture ring of the present invention;
FIG. 28 is an enlarged cross-sectional view illustrating aspects of the fabrication of the exemplary suture ring;
FIG. 29 is a perspective view illustrating additional features of the exemplary suture ring assembly;
FIG. 30 is an enlarged sectional view of a portion of FIG. 29 illustrating additional aspects of the fabrication of the suture ring assembly;
FIG. 31 is an enlarged sectional view illustrating additional aspects of the finished exemplary suture ring assembly;
FIG. 32 is an exploded perspective view illustrating positioning and assembly of a suture ring and leaflet subassembly configuration;
FIG. 33 is a top perspective view illustrating additional suture ring leaflet subassembly attachment steps;
FIG. 34 is a bottom perspective view illustrating further exemplary suture ring attachment steps;
FIG. 35 is a cutaway perspective view illustrating an exemplary attachment of an outflow conduit to an exemplary valve of the present invention;
FIG. 36 is an enlarged cross-sectional view illustrating additional aspects of the conduit attachment;
FIG. 37 is a cross sectional view similar to FIG. 36 illustrating alternative conduit attachment features; and
FIG. 38 is an exploded perspective view illustrating additional valve attachment alternatives of the present invention.
DETAILED DESCRIPTION OF EXEMPLARY EMBODIMENTS
Referring more particularly to the drawings, FIG. 1 is an exploded assembly view, illustrating exemplary alternative embodiments of an improved, adaptable tissue valve 50 , its individual components and its alternative configurations produced in accordance with the teachings of the present invention. Valve 50 includes a pre-aligned, standardized leaflet subassembly 52 , a cloth-covered wireform 54 and a support stent 56 . As will be discussed in detail below, during assembly of valve 50 , the pre-aligned leaflet subassembly 52 and the cloth-covered wireform 54 are first assembled in accordance with the present invention to form a tissue-wireform structural assembly 58 (see FIGS. 2 to 9 ). Then, the structural assembly 58 is secured to stent 56 to form the assembled valve 50 .
As illustrated FIG. 1, valve 50 is uniquely configured to enable production of several useful alternative valves for a variety of end-use applications. For example, if the desired application is the replacement of a native heart valve, valve 50 can be attached to a relatively soft suture ring 60 for subsequent sewing into place within a heart (not shown). Alternatively, if it is desired to use valve 50 in a left ventricular assist device (LVAD) or in a mechanical heart pump, valve 50 can be mounted to an appropriately rigid mechanical flange 62 . Further, in both natural and mechanical applications where it is desirable to incorporate a conduit, valve 50 may be attached to either an inflow conduit 64 and/or an outflow conduit 66 .
Production of the Tissue-Wireform Structural Assembly
In the present disclosure, exemplary valve 50 is illustrated as a three-leaflet or tricuspid valve. However, it will be appreciated by those skilled in the art that valve 50 may be configured to have two leaflets or any other desired leaflet configuration depending on the intended application.
A first step in the assembly of tissue valve 50 is the attachment of tissue leaflets 68 to one another to form a consistently dimensioned, standardized leaflet subassembly. Tissue leaflets are typically formed from pericardial, porcine or similar tissue obtained from donor organs, which tissue is preserved or “fixed” prior to use in assembling a valve. Those skilled in the art will appreciate that the dimensions of leaflet subassembly 52 will vary depending upon the intended end use and associated positioning and dimensional requirements of the finished valve. However, pre-alignment and stitching in accordance with the teachings of the present invention not only simplifies the manufacture of valve 50 but also functions to align the entire valve mating or seating surfaces at once. This eliminates variations in leaflet alignment and dimensional relationships and significantly minimizes the need to adjust the tissue leaflets after final assembly of the valve in order to ensure proper coaptation at the mating edges of the leaflets.
Referring now to FIG. 2, the desired number of tissue leaflets 68 (in this example, three leaflets) are obtained from natural tissue as known in the art, and each leaflet 68 is trimmed to the appropriate desired shape and size for the intended valve use using template 69 , defining a generally straight or linear coapting mating edge 70 having opposing ends 71 , 72 and a generally arcuate peripheral cusp 73 extending therebetween. More particularly, each leaflet 68 is placed on a cutting board 74 and the selected template 69 is then placed over the leaflet 68 . Tissue 75 extending beyond the boundaries of template 69 is then cut away using a sharp razor blade 76 or similar cutting tool.
A characteristic of pericardial tissue is that one surface is smoother than the opposite surface. Accordingly, it is desirable that the less smooth surface be identified to serve as the mating surface at edge 70 with an adjacent leaflet edge 70 . After the leaflets 68 are trimmed and the mating surfaces identified, two of the leaflets 68 a , 68 b are pre-aligned or mated together along with template 69 as shown in FIG. 3 . The two leaflets 68 a , 68 b are then attached or stitched together at one end 71 to define the first in a plurality of pairs of aligned, mating leaflet ends. For example, a needle that has been “double-threaded,” that is, needle 78 that has been threaded with a looped (or “folded”) segment of thread 80 is inserted and pushed through the leaflets 68 a , 68 b at the location dictated by guide slot 82 at one end of template 69 . Template 69 may then be removed, with needle 78 being brought over the top of leaflets 68 a , 68 b and passed back through the loop and pulled tightly. Naturally, alternative attachment methods or stitches may be utilized within the scope and teaching of the present invention. The opposite ends 72 of the first two leaflets 68 a , 68 b of the exemplary three leaflet valve are not sewn together at this time.
Referring now to FIG. 4, a third leaflet 68 c is pre-aligned and attached to the other two leaflets 68 a , 68 b in a tricuspid format, again using template 69 . In particular, third leaflet 68 c is mated with template 69 , and the respective unsewn ends 72 of the first two leaflets 68 a , 68 b are spread out and then aligned with the respective opposite ends 71 , 72 of templated third leaflet 68 c . Again using guide slot 82 of the template 69 as a guide, a double-threaded needle with thread 80 is inserted through each of the unsewn pairs of the three leaflets 68 a , 68 b , 68 c to secure the leaflet ends together in pairs as shown. The template may then be removed, and, for each stitch, needle 78 may be brought over the top of leaflets 68 a , 68 b , 68 c and passed back through the loop and pulled tightly to produce leaflet subassembly 52 having three leaflet mating ends.
Referring now to FIGS. 5 and 6, it is preferred to attach leaflet subassembly 52 to the underside or bottom 83 of wireform 54 . Exemplary wireform 54 is a wire reinforced cloth having a cloth edge 84 and is shaped in a manner substantially conforming to the shape of the leaflet subassembly structure 52 . In the embodiment shown, wireform 54 is generally circular in shape and has a sinusoidal undulation defining a plurality of commissure tips 86 corresponding to the pairs of leaflet mating ends. The cloth of wireform 54 includes the circumferential cloth edge 84 that serves as a sewing or attachment surface for the leaflet subassembly 52 . Exemplary wireform 54 includes the three raised commissure tips 86 which receive the three respective pairs of attached mating ends of leaflets 68 a, b , and c of the pre-aligned leaflet subassembly 52 .
An exemplary technique for attaching the leaflet pairs at an end of the leaflet subassembly 52 to one of the commissure tips 86 of wireform 54 is shown in FIG. 5 . Needle 78 (not shown) with looped thread 80 , which was used to sew the leaflet ends together, is inserted up from leaflets 68 (as shown in dashed lines), through an inner edge of cloth edge 84 as indicated at 87 , so that the top surfaces of mating leaflets 68 are secured into contact with wireform 54 . The needle is then re-inserted through an outer edge of and from underneath cloth edge 84 as indicated at 88 ′, and a first lock 89 , preferably a single lock stitch, is made with thread 80 . The locking process can be repeated as indicated at 88 ″ with a second lock 90 , preferably a double lock stitch. Finally, the needle can be inserted into the middle of and from underneath cloth edge 84 as indicated at 91 and the thread pulled so that first and second locks 89 , 90 are pulled underneath cloth edge 84 and thereby hidden and protected during the remaining fabrication process. The excess thread is then trimmed and discarded. This method is repeated for securing each of the respective pairs of attached, aligned mating leaflet ends of mated leaflets 68 a , 68 b , 68 c of subassembly 52 to the respective commissure tips 86 of wireform 54 . Thus, wireform 54 functions as an additional, permanent template for positioning the leaflet commissures in their final position relative to one another. As an added benefit of the present invention, this manufacturing technique further stabilizes the position of the coapting valve leaflets relative to one another prior to attachment of the leaflet cusps to the wireform. Thus, it is possible to attach the entire peripheral leaflet cusp uniformly from the tip of one commissure to the next in order to produce consistent attachment stress along the leaflet edge.
Referring now to FIGS. 6 and 7, the next exemplary step for securing the exemplary leaflet subassembly 52 to wireform 54 is to attach peripheral cusps 92 of each of the leaflets 68 to cloth edge 84 . In that connection, slip knots 94 (i.e., knots that may be undone) are spaced periodically along wireform 54 to temporarily fit leaflet cusps 92 in position on wireform 54 . Three of the slip knots 94 may be made for each leaflet cusp 92 , with one at the center of the cusp and two at points of inflection with the commissures, as this helps to uniformly stabilize the cusp in position during attachment to wireform 54 .
As shown in FIGS. 7 and 8, temporarily secured leaflet cusps 92 then are attached to wireform cloth edge 84 , preferably using double-threaded “in-and-out” sutures 96 , starting from a center position 98 of each leaflet cusp 92 and running to the tips of each commissure 86 . At about one millimeter from the commissure tips 86 , the threads are locked, buried and trimmed, preferably as described previously. Thus, unlike prior art tissue valves wherein leaflets are attached individually and the peripheral stitching of the cusps terminates before the tips of the commissures, producing a potential stress point, the method of the present invention produces a novel tissue valve assembly having uniform stitching from commissure tip to commissure tip and consistently aligned coapting leaflet mating edges.
Attachment of the Tissue-Wireform Structural Assembly to a Support Stent
For purposes of further explanation, once the assembled tissue-wireform structural assembly, which is identified by reference numeral 58 , is produced as discussed above, the assembly 58 is then attached to a support or stent 56 . Referring to FIGS. 9, 10 , and 11 , the tissue-wireform structural assembly 58 is first fitted onto the correspondingly configured stent 56 in a manner that will uniformly clamp the peripheral cusp edges of the leaflets 68 between an upper surface 99 (see FIG. 1) of stent 56 and the lower surface of wireform 54 . This assembly technique further distributes stresses and loads of the leaflets 68 and contributes to their functional longevity. Moreover, pre-alignment of the leaflets 68 and attachment to the wireform 54 enables the dimensions of the entire valve 50 to be aligned at once and eliminates the dimensional variation that could occur in prior art valves due to the utilization of separate commissure posts. In particular, stent 56 is dimensioned to mate or seat with the configuration of assembly 58 , and assembly 58 is mated to stent 56 such that the lower surface of each commissure tip 86 of wireform 54 mates with the top surface of a corresponding and complementary stent commissure tip 100 . Care is taken to ensure that central opening 102 formed by coapting mating leaflets 68 is not distorted while mating tissue-wireform structural assembly 58 to stent 56 . Similarly, care is taken to ensure that leaflets 68 are uniformly clamped and remain evenly tensioned throughout this process.
Once wireform assembly 58 is mated to stent 56 , a temporary pin 104 can be inserted at the bottom curve of each leaflet cusp 92 to temporarily secure wireform assembly 58 to stent 56 . Stent 56 and assembly 58 then are sutured together as shown in FIGS. 10 and 11. Suturing of assembly 58 to stent 56 begins at the tops of the commissure tips 86 . In particular, a double-threaded needle (not shown) is inserted through stent commissure tip 100 as indicated at 105 ′, between free tab ends 106 , 108 of adjacent pairs of leaflets 68 , and through cloth edge 84 of wireform assembly 58 as indicated at 109 ″. The needle is then inserted through the looped thread to form a single lock 110 . A double lock 112 is then formed, with the needle being inserted through stent commissure tip at 105 ″ and through cloth edge 84 at 109 ″, substantially in the manner previously discussed so that double lock 112 is able to be pulled underneath cloth edge 84 . Excess thread exiting from cloth edge 84 as indicated at 113 may then be trimmed and discarded. The identical procedure may be performed for the remaining commissure tips 86 of the wireform assembly 58 . As a result, wireform commissure tips 86 evenly match with stent commissure tips 100 .
With reference to FIGS. 9 and 12 - 14 , the exemplary attachment procedure can be completed by inserting a double-threaded needle as previously described through stent 56 near the top of stent commissure tip 100 as indicated at 114 ′, through tissue leaflet 68 and through cloth edge 84 of wireform 54 as indicated at 115 ′. The needle is then re-inserted in a reverse manner through cloth edge at 115 ″, through stent commissure tip 100 at 114 ″ and passed through loop 115 of the double thread. With reference to FIG. 14, the suture is then tightened so that loop 115 is positioned securely and firmly against stent commissure tip 100 . In-and-out suturing 116 (see also FIGS. 15 and 16) is then performed along the mating edges of stent 56 and wireform assembly 58 up to the next wire form assembly and stent commissure tips 86 , 100 . With reference to FIG. 13, at a position near the top of the commissure tip 86 , a single lock 118 and a double lock 120 can be formed, and the thread can be buried beneath cloth edge 84 of wireform assembly 58 as described previously. It will be appreciated that the suturing just described may be initiated at any of the stent commissure tips 100 and that the in-and-out suturing 116 may be performed in either a clockwise or a counter-clockwise manner around the periphery of stent 56 .
Upon completion of the in-and-out suturing 116 around the periphery of stent 56 , the free tab ends 106 , 108 of each pair of tissue leaflets 68 need to be secured to the respective stent commissure tip 100 . Referring to FIGS. 15 and 16, two exemplary alternatives are provided to perform this task.
Referring to FIG. 15, a first exemplary alternative is to configure tab ends 106 , 108 to form a butt joint 122 . In particular, tab ends 106 , 108 are trimmed such that, when folded towards each other, the respective end edges of each tab end 106 , 108 mate evenly to form, preferably, a straight center line descending vertically from the top of commissure tip 100 . The two leaflet tab ends 106 , 108 are then stitched together with stitching 124 .
Referring to FIG. 16, a second exemplary alternative for securing leaflet tab ends 106 , 108 is to configure tab ends 106 , 108 to mate evenly to form a flush junction 126 with cloth edge 84 of wireform 54 on either side of commissure tip 100 . In particular, leaflet tab ends 106 , 108 can be trimmed so that the end edges of each tab 106 , 108 are sized to fit flush with cloth edge 84 of the wireform. Leaflet tab ends 106 , 108 are then stitched to cloth edge 84 of wireform 54 with stitching 128 as shown. The alternative flush junction 126 so formed provides a somewhat flatter commissure than butt junction 122 of the first alternative does, and, therefore, flush junction 126 may be more desirable when a more compact valve is needed. Both exemplary methods, however, allow even and reliable distribution of the load on the tissue leaflets at the commissures.
Assembly of an Exemplary Stent
From the foregoing description, it will be appreciated that stent 56 is configured to have a structure suitable for mating and supporting wireform assembly 58 . In that connection, an exemplary structure of stent 56 will now be described with reference to FIG. 17 . Those skilled in the art will appreciate that the exemplary stent described herein is a multi-piece construction. However, it is contemplated as being within the scope of the present invention to provide a single-piece stent. However, the multi-piece stent assembly illustrated may make it easier to engineer or fine tune the radial stability of the stent while maintaining desirable axial flexibility of the commissure posts. The first step in the assembly of exemplary stent 56 is to fabricate an inner support member 130 and an outer support member 132 , which, when mated together, generally form the shape of stent 56 which ultimately conforms to the configuration of wireform assembly 58 . In the exemplary embodiments inner support member 130 is configured with three upstanding posts 134 that serve as the support structures for the stent commissure tips 100 . Outer support member 132 also may include posts 136 that correspond to the posts 134 of the inner support member 130 . However, posts 136 are truncated and therefore do not match the height of posts 134 on inner member 130 . The inner and outer support members 130 , 132 may be fabricated from a metal or plastic material depending on the desired characteristics of valve 50 .
Disposed on inner support member 130 are a plurality of sewing holes 138 along the periphery of member 130 and on the posts 134 . The outer support member 132 includes at least one sewing hole 139 on each of its truncated posts 136 that correspond with respective ones of the sewing holes 138 on each post 134 of the inner member 130 . The inner diameter of outer support member 132 is sized to form a slip fit with the outer diameter of inner support member 130 .
Inner support member 130 is placed within outer support member 132 such that sewing holes 139 of outer support member 132 align with sewing holes 138 on the respective posts 134 of inner member 130 . The two members are then sewn together by inserting a double-threaded needle as described previously through the aligned holes 138 , 139 . As shown in FIG. 18, thread 140 inserted through each of the aligned holes 138 , 139 is then passed through end loop 142 and tightened. The thread may then be locked using, for example, a slip knot (not shown), which is a knot that may slide along the thread to abut the support members. Accordingly, posts 134 of inner support member 130 flex to a greater extent from base portions thereof to tops thereof, and outer support member 132 augments the radial stability of inner support member 130 , with the truncated posts 136 providing rigidity to base portions of posts 134 of inner support member 130 .
Referring now to FIG. 19, once the inner and outer support members 130 , 132 are sewn together, a covering cloth 144 , preferably made from woven polyester, is cut and formed into a cylindrical tube for covering the combined support members 130 , 132 . Those skilled in the art will appreciate that the covering cloth is equally applicable to single-piece stent assemblies. Covering cloth 144 includes two crease lines 146 , 148 , the first of which, 146 , is formed from folding an edge of cloth 144 to form a fold which receives posts 134 of inner support member 130 . There is approximately 1 mm to 1.5 mm between first crease line 146 and a top edge 149 (see FIGS. 17 and 18) of each post 134 in the exemplary embodiment. Second crease line 148 is located such that it corresponds to a lower edge 150 (see FIG. 18) of combined support members 130 , 132 .
Referring now to FIG. 20, to secure covering cloth 144 to support members 130 , 132 , a threaded needle may be inserted through cloth 144 , through a hole 151 of one of inner member posts 134 , through the second layer of cloth 144 and then back through cloth 144 through the same hole 151 and through cloth 144 . The needle then can be passed through a loop to form a first lock 152 . This threading step may be performed up to two more times. The excess thread is then trimmed and discarded. The same procedure can be followed for each of the three posts 134 on inner support member 130 .
Then, as shown in FIG. 21, the next exemplary step involves stitching covering cloth 144 to inner and outer support members 130 , 132 along an upper edge 137 of inner support member 130 . First, lower edge 154 of cloth 144 can be folded into the interior of support members 130 , 132 along crease line 148 such that second crease line 148 defines the lower end or bottom of the support member structure. This fold results in dual-layered cloth 144 (including outer and inner cloth layers 156 , 158 ) enveloping support members 130 , 132 . Then, using a single threaded needle, the layered cloth is stitched together at 155 along the curvature of the upper edge 153 of support members 130 , 132 . The stitching 155 is preferably backstitching, which is accomplished by inserting the needle a stitch length, for example, to the right and bringing it up an equal distance to the left. However, the stitching 155 does not extend to the tops . 149 of posts 134 , leaving a space of approximately 1 mm between the top 149 of post 134 and the stitching 155 . After stitching the upper edge 153 of support members 130 , 132 , the cloth 144 then can be stitched in a similar manner at 156 along the lower edge 150 of support members 130 , 132 . The last stitch is then locked by tying a slip knot, which may be performed up to three times to lock the stitching securely in place.
Referring now to FIGS. 21-26, cloth 144 as now attached to support members 130 , 132 is trimmed to conform to the shape of support members 130 , 132 and, if desired, to provide a gasket-like sewing edge. To accomplish this, outer cloth layer 157 can be sliced downwardly from a top edge thereof to a distance approximately 5 mm to 6 mm above the top edge 153 of inner support member 130 . In a similar manner, inner cloth layer 158 can be sliced downwardly from a top edge thereof to a distance approximately 2 mm to 3 mm above the bottom of the slice in outer cloth layer 157 . The slices are made at a location midway between adjacent posts 134 of inner member 130 and are intended to align with one another in the downward direction, as indicated at 160 .
Next, outer cloth layer 157 can be trimmed along the upper edge 153 of inner support member 130 , starting at the bottom of the slice formed in outer cloth layer 157 . In this exemplary embodiment of the present invention the trimming is performed in a manner such that the contour of the cloth 144 extends a distance of approximately 4 mm to 5 mm above the lower curved portions of the upper edge 153 of support member 130 , a distance of approximately 2 mm to 3 mm above portions of support member 130 in the areas at or near the base of posts 134 of support member 130 and a distance of about 0.5 mm to 2 mm above the tops 149 of posts 134 of support member 130 .
As shown in FIG. 22, inner cloth layer 158 is then folded over the tops 149 of posts 134 of inner member 130 and is anchored to posts 134 with a threaded needle stitched through sewing hole 151 in posts 134 in the manner previously described with respect to the upper folded section of cloth 144 . However, after these locking stitches are executed, the needle is passed under the cloth so as to exit from the top of post 134 .
Next, a series of trimming operations can be performed. Referring to FIGS. 22 and 23, a folded portion 162 of inner cloth layer 158 is trimmed around the entire circumference of the cloth so that lower edge 164 of folded portion 162 is approximately 1 mm to 1.5 mm from the stitch in hole 151 of post 134 . A folded portion 168 of outer cloth layer 157 is folded over the tops 149 of post 134 of inner support member 130 . Folded portion 162 of the inner cloth layer 158 is further trimmed so that its remaining edges are flush with the edges of the previously trimmed inner cloth layer 158 . With regard to the non-folded portion of inner cloth layer 158 , this layer is trimmed in a manner such that its edges extend approximately 2 mm beyond the edges of the previously trimmed outer cloth layer 157 . The 2 mm extension of the inner cloth layer 158 beyond the outer cloth layer 157 provides the material desired to form a seating and attachment or sewing surface on the stent.
Each of the trimming operations is performed starting from the central area between posts 134 of inner support member 130 to the tops 149 of posts 134 . The arrangements of inner cloth layer 158 , outer cloth fold 168 , outer cloth layer 157 and inner cloth fold 162 are shown in the enlarged cross-section of FIG. 23 .
The remaining exemplary step to complete the assembly of the stent 56 is to fold and suture the cloth layers to form a sewing edge 169 around the stent 56 . Referring to FIG. 24, inner cloth layer 158 is folded around post 134 and stitched so as to enclose post 134 . More specifically, the thread previously inserted through the top of post 134 when connecting folded outer cloth layer 157 through sewing hole 151 is now used to create first and second locks 172 on the top of post 134 so as to hold inner cloth layer 158 in place on the top of post 134 . A wipstitch 174 may then be utilized to further secure exemplary inner cloth layer 158 downwardly around post 134 approximately 8 mm from the top of post 134 . When the bottom of the post 134 is reached, first and second locks are formed, and the thread is trimmed and discarded. The above-described stitching operation is performed for each of the three posts 134 . However, for the last of the posts 134 to be stitched, instead of trimming the thread after forming the first and second locks 172 , untrimmed thread 176 can be used for performing the stitching of the cloth along the remaining edges of support members 130 , 132 between posts 134 .
In that connection, with reference to FIGS. 25 and 26, inner cloth layer 158 is folded over the outer cloth layer 157 , and an alternating stitching is applied to hold the folded layers in place on the support members and thereby to form the sewing edge 169 on the stent. After completing the stitching around the remaining portions of the support members 130 , 132 , a first and second lock stitch can be formed with the thread, and the excess thread is trimmed and discarded to complete the assembled stent 56 .
Assembly of an Exemplary Suture Ring
Where valve 50 is intended for use in the replacement of a native heart valve, a soft suture ring 60 is contemplated for use in completing the valve structure. For example, referring to FIG. 27, an exemplary ring washer 180 is provided which is preferably made from non-woven polyester, such as a material sold under the trade name REMAY manufactured by Remay, Inc., Old Hickory, Tenn. Also provided is a silicone sponge waffle annulus 182 for mating with washer 180 . In that connection, annulus 182 is configured to have a walled lip 184 configured to be disposed along the inner circumference 185 of washer 180 . Lip 184 is contoured to include three depressions 186 that correspond with the lower curved surfaces between each commissure on valve 50 . Washer 180 mounts on waffle annulus 182 such that washer 180 surrounds the walled lip 184 . This produces a soft, relatively flexible, yet stable suture ring internal structure which, when covered with cloth as discussed below, functions as a compliant, stitchable interface between the natural tissues of the heart and the prosthetic tissue valve 50 .
As shown in FIG. 28, before mounting washer 180 on waffle annulus 182 , a cloth 188 is positioned around washer 180 to extend from the inner circumference 185 to the outer circumference 189 . Washer 180 is then mounted on waffle annulus 182 such that cloth 188 is sandwiched between waffle annulus 182 and washer 180 . Cloth 188 is placed to extend a distance 190 of approximately 3 mm to 5 mm beyond the outer circumferential edge 189 of washer 180 , as shown in FIG. 28 . Washer 180 , cloth 188 and waffle annulus 182 are then sewn together using, for example, in-and-out suturing 192 around the circumference of washer 180 . The exemplary suturing is preferably placed a distance 194 of approximately 1 mm from the outer circumferential edge 189 of washer 180 . If desired, a second suture line (not shown) may be added at the same location as the first suture line, with each stitch of the second suture line placed between the stitches of the first suture line. The resulting suture 192 then appears as a continuous line of stitching. Additionally, as shown in FIG. 29, to further secure cloth 188 and waffle annulus 182 together, back stitching 195 may be applied in the space between the walled lip 184 of annulus 182 and washer 180 , which space is indicated at 196 in FIG. 28 .
Referring now to FIG. 30, cloth 188 can be attached to depressions 186 of the structural assembly of washer 180 and waffle annulus 182 with, for example, a single-threaded needle inserted at one corner 198 of depression 186 (through cloth 188 and annulus 182 ) and then with a double slip knot to secure the thread at corner 198 . In-and-out stitching 200 can be then used to secure cloth 188 to the contour of depression 186 . The same method can be followed for each depression 186 . The excess cloth is then trimmed to the outer edge of washer 180 as indicated at 201 .
With additional reference to FIG. 31, an outer portion 202 of cloth 188 then can be folded around the external surfaces of washer 180 and tucked under washer 180 between washer 180 and waffle annulus 182 . Because of annulus 182 is pliant, annulus 182 deforms and accommodates the outer portion 202 of cloth 188 . Using a single-threaded needle, an alternating stitch 204 can be used to secure folded cloth 188 underneath washer 180 . After completing the stitching of the entire circumference of washer 180 , a double knot can be formed to secure the stitching, yielding a finished suture ring.
Attachment of the Suture Ring to the Exemplary Valve
Referring to FIGS. 32 and 33, to attach suture ring 60 or an alternative structure such as flange 62 (see FIG. 1) to valve 50 , depressions 186 of suture ring 60 are aligned with the descending peripheral cusps 206 of valve 50 and then mated together. More specifically, valve 50 is placed on suture ring 60 such that cloth edge 84 of the wireform 58 on the lower-most portion of each cusp on valve 50 is substantially flush with a top surface of suture ring 60 at corresponding depressions 186 . Care is taken with the placement such that kinking or wrinkling of tissue leaflets 68 is avoided. Valve 50 can be temporarily pinned in place on suture ring 60 with needles 208 to facilitate this procedure.
As shown in FIG. 34, the assembly of pinned valve 50 and suture ring 60 can be flipped over, and suture ring 60 can be stitched to valve 50 along mating edges 209 of ring 60 and valve 50 . More specifically, in the exemplary embodiment a single threaded needle can be used to sew suture ring 60 to the cloth of the stent structure. To facilitate the stitching step, the pieces are held temporarily, yet securely in place with additional needles 208 . The opposite side of ring 60 and valve 50 can be sewn together in a similar manner.
Attachment of Valve to Outflow Conduit
Referring now to FIGS. 35-37, in certain applications, it may be desirable to attach valve 50 to an outflow conduit such as that shown at 66 . For example, in some patients requiring replacement of the aortic valve, a portion of the aorta itself may be damaged or diseased such that it needs replacement as well. Accordingly, consistent with the teachings of the present invention, the adaptable tissue valve structure can be modified to include an outflow conduit 66 that will function to replace the damaged aorta. Alternatively, in some intended mechanical pumping applications the adaptable tissue valve of the present invention may be provided with an outflow conduit to facilitate interfacing with the mechanical pumping structure. In either alternative, this can be accomplished as shown in FIGS. 35 and 36 where an outflow conduit 66 may be attached to wireform 54 at the time that the tissue leaflets 68 are being secured. In particular, referring to FIG. 36, conduit 66 may be secured on a side of wireform 54 opposite to tissue leaflets 68 by, for example, stitching. Alternatively, as shown in FIG. 37, conduit 66 may be stitched and secured to wireform 54 on the same side as tissue leaflets 68 , or sandwiched therebetween. A third option is to simply secure conduit 66 to the periphery of the finished valve (not shown) as a subsequent sewing step. The valve 50 may be attached to an outflow conduit either with or without a sinus.
Alternative Configurations for Inflow Side of Valve
FIG. 38 illustrates additional exemplary alternative options available for modification and attachment of valve 50 . For example, as discussed above, when it is desired to use valve 50 as a conduit valve, suture ring 60 may be attached to valve 50 as previously described. Alternatively, in applications such as artificial hearts or left ventricular assist devices (LVADs), suture ring 60 is not necessarily required; hence, the lower end of stent 56 may be attached to flange 62 for use in mounting the valve in the artificial heart or LVAD.
Yet a further alternative adaptation involves those applications where an inflow conduit 64 is desired. In such applications, inflow conduit 64 may be attached directly to stent 56 of valve 50 . More specifically, inflow conduit 64 may be configured to have a stepped circumference 210 that snugly mates with the outer periphery (or, alternatively, the inner periphery) of stent 56 and which can be sewn thereto. In this configuration, for example, in an artificial heart or an LVAD application, suture ring 60 could be attached to inflow conduit 64 rather than to valve 50 .
Conclusion
In view of the foregoing description of exemplary embodiments of valve 50 and the components thereof, the present invention satisfies the need for improved tissue-type prosthetic heart valves in which stress is reduced on valve leaflets 68 while desirable structural and functional features are maintained. Additionally, valve 50 is adaptable for use in a variety of positions within the natural heart or in mechanical pumps. Further, valve 50 is simpler and easier to manufacture in a more consistent manner than existing valves. The standardized leaflet structure subassembly 52 of the present invention can be modified readily to adapt to different intended applications. Of equal importance, leaflet subassembly 52 uniformly distributes tensile loads along the entire periphery of leaflet cusps 92 , reducing stress points and significantly improving the long-term functionality of valve 50 . As an added benefit of the present invention, the stability and adaptability of the tissue valve subassembly is achieved through simplified manufacturing processes utilizing fewer steps and subassemblies. This manufacturing protocol can be incorporated into branched, adaptable manufacturing techniques for the production of tissue heart valves having a variety of end uses. Further, these improved construction techniques expedite the overall manufacturing process and improve the consistency of valve 50 while simultaneously reducing the need for post-assembly fine tuning and quality-control procedures.
The plurality of tissue leaflets 68 being attached together as described form the dimensionally stable and dimensionally consistent coapting leaflet subassembly 52 . Further, sutures 96 used to attach cusps 92 to wireform 54 act like similarly aligned staples, all of which equally take the loading force acting along the entire periphery of cusp 92 of each pre-aligned, coapting leaflet 68 . The resulting tissue-wireform structural assembly 58 reduces stress and potential fatigue at the leaflet suture interface by distributing stress evenly over the entire leaflet cusp 92 from commissure to commissure. Further, tissue-wireform structural assembly 58 may be attached to cloth-covered stent 56 without disturbing leaflets 68 or disturbing their relative alignment and the resultant coaptation of their mating edges.
Stent 56 as fabricated according to the present invention provides evenly distributed support and dimensional stability for each leaflet 68 of the valve structure 50 from commissure to commissure. This assembly methodology allows the evenly sutured tissue of leaflet cusps 92 to be sandwiched between wireform 54 and stent 56 and to thereby further distribute the loading forces more evenly around the attachment site. Because leaflets 68 experience lower, more evenly distributed stresses during operation, leaflets 68 are less likely to experience distortion in use. Thus, a more stable, long lived, functional closure or coaptation of leaflets 68 is provided by this even distribution of attachment forces.
Furthermore, for each key area of stent 56 , the flexibility can be optimized or customized. If desired, the coapting tissue leaflet commissures 86 can be made more or less flexible to allow for more or less deflection to relieve stresses on the tissue at closing or to fine tune the operation of valve 50 . Similarly, the base radial stiffness of the overall valve structure can be increased or decreased to preserve the roundness and shape of valve 50 . Unlike a rigid mechanical valve, stent 56 does not act as a rigid heart valve structure but as a radially stable, yet axially flexible support. A rigid structure is unnecessary by utilizing the teachings of the present invention because leaflets 68 are dimensionally pre-aligned along their mutually coapting mating or sealing edges 70 prior to being directly attached to cloth-covered wireform 54 . As a result, the entire sealing aspect of valve 50 can be aligned in three dimensions at once without the variability previously experienced in the construction of prior art tissue-type valves. In addition to eliminating the need for post-assembly adjustment, this pre-alignment provides for consistency and simplicity in the manufacture of valve 50 . Further, wireform 54 functions as a template for suturing leaflet cusps 92 to the valve subassembly with uniform stitching from commissure tip 86 to commissure tip 86 . This produces a dimensionally consistent structure that can interface with stent 56 in a previously unobtainable uniform manner. The consistent dimensional integrity of leaflet wireform subassembly 58 enables stent 56 to function as a stress relieving support clamp which further secures leaflet cusps 92 in valve 50 to provide an added degree of stability and stress distribution. If desired, providing the top 99 of the stent 56 with a single, or double fold of covering cloth 144 provides the stent lip with a deformable cloth seat that assists in the distribution of load around leaflet cusps 92 and simplifies sewing stent 56 to tissue-wireform structural subassembly 58 . Those skilled in the art will appreciate that attaching stent 56 to tissue-wireform structural subassembly 58 functions to stabilize the projecting commissure posts of the valve subassembly without stiffening their desirable axial flexibility. This novel construction technique eliminates the need for separate commissure posts at the tissue leaflet commissures and also eliminates multiple tissue and cloth layers at wireform commissures 86 which adds to uniformity and consistency in valve production and eliminates assembly steps. As a result, valve manufacture is not only improved, but simplified and expedited as well.
Stent 56 also functions as an adaptable structural interface, allowing the tissue-wireform-stent structural subassembly to be attached to a variety of additional structures dependent upon intended valve placement and operating environments, including soft suture ring 60 , mechanical flange 62 , inflow conduit 64 , and outflow conduit 66 . Unlike prior art tissue heart valves, the present invention provides this flexibility and adaptability of use because key valve components can be standardized for different types of valves or valve applications. This manufacturing and structural consistency also improves quality control and provides repeatability and consistency in the formation of the valves. It also simplifies final assembly that in turn provides for increased production rates without sacrificing consistent product quality.
As part of the flexibility of the present invention, stent 56 may be designed to be adaptable so that different ways of attaching valve 50 to various intended applications can be accommodated. The novel construction that allows for this universal application results from stent 56 providing a complete uniform support to the dimensionally stable, pre-aligned wireform/leaflet subassembly 58 . Because of this adaptability, valve 50 can function in a variety of applications, including that of a temporary heart valve prosthesis within a circulatory support system using a relatively rigid flange or a conduit assembly rather than a standard soft sewing ring. Alternatively, valve 50 can function as a prosthetic valve having a soft, scallop-shaped sewing ring for aortic positioning or a soft flat sewing ring for mitral positioning, or as a conduit valve by incorporating proximal and distal conduits attached on both the inflow and outflow valve ends. The outflow conduit can have a sinus shape to improve blood flow if desired. Within an artificial heart system, valve 50 mimics the hemodynamic pumping action of the heart while sustaining the patient until a donor heart is located and successfully transplanted. In this application, both blood inflow and outflow functions can be accommodated by valve 50 .
From the foregoing detailed description, it will be evident that there are a number of changes, adaptations and modifications of the present invention which come within the province of those skilled in the art. However, it is intended that all such variations not departing from the spirit of the invention be considered as within the scope thereof as limited solely by the claims appended hereto.
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Improved, adaptable tissue-type heart valves and methods for their manufacture are disclosed wherein a dimensionally stable, pre-aligned tissue leaflet subassembly is formed and its peripheral edge clamped between and attached to an upper shaped wireform and a lower support stent. A variety of adaptable structural interfaces including suture rings, flanges, and conduits may be attached to the support stent with or without an outlet conduit disposed about the wireform to provide a tissue-type heart valve adaptable for use in either a natural heart or in mechanical pumping devices. The methods include forming individual leaflets with a template and using the template to attach the leaflets together to form a tissue leaflet subassembly. The template and leaflets include a straight edge terminating in oppositely directed tabs, and a curvilinear cusp edge extending opposite the straight edge. The template may include a guide slot in its straight edge and the assembly includes aligning two leaflet tabs with the template and passing sutures through the guide slot and through the leaflet tabs. The leaflet subassembly is mated to a wireform with the tabs extending through commissure posts of the wireform. A support stent having an upper surface matching the lower surface of the wireform sandwiches the edges of the leaflet subassembly therebetween. Separated tabs on the leaflet subassembly are passed through the wireform commissures and attached to adjacent stent commissures so as to induce clamping of the leaflet tabs between the stent commissures and wireform commissures upon a radially inward force being applied to the leaflets.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to Taiwanese Patent Application No. 103133181 filed on Sep. 25, 2014, the contents of which are incorporated by reference herein.
FIELD
[0002] The subject matter herein generally relates to an automotive daytime running light.
BACKGROUND
[0003] A conventional automotive daytime running light is a warning light to remind people to pay attention to a running vehicle to decrease accidents. The automotive daytime running light is used to arrange a plurality of LED sources in a line and mounts a reflecting cup to adjust the light. However, the automotive daytime running light has limited visibility.
BRIEF DESCRIPTION OF THE DRAWINGS
[0004] Implementations of the present technology will now be described, by way of example only, with reference to the attached figures.
[0005] FIG. 1 is a cross sectional view of an automotive daytime running light of the present disclosure.
DETAILED DESCRIPTION OF EMBODIMENTS
[0006] It will be appreciated that for simplicity and clarity of illustration, numerous specific details are set forth in order to provide a thorough understanding of the embodiments described herein. However, it will be understood by those of ordinary skill in the art that the embodiments described herein can be practiced without these specific details. In other instances, methods, procedures and components have not been described in detail so as not to obscure the related relevant feature being described. Also, the description is not to be considered as limiting the scope of the embodiments described herein. The drawings are not necessarily to scale and the proportions of certain parts may be exaggerated to better illustrate details and features of the present disclosure. The description is not to be considered as limiting the scope of the embodiments described herein.
[0007] A definition that applies throughout this disclosure will now be presented. The term “comprising” means “including, but not necessarily limited to”; it specifically indicates open-ended inclusion or membership in a so-described combination, group, series and the like.
[0008] Referring to FIG. 1 , an automotive daytime running light includes a light source 10 , a plurality of reflecting plates 20 arranged on a light path of the light source 10 , a substrate 100 paralleled the road of the light path of the light source 10 , a plurality of reflecting cup 30 located above the reflecting plates 20 and a lamp shell 50 located on the substrate 100 .
[0009] In at least one embodiment, the light source 10 is a blue laser light source.
[0010] The reflecting plates 20 are spaced each other and arranged on the light path of the light source 10 . In at least one embodiment, the reflecting plates 20 are total reflection mirrors. Every reflecting plate 20 faces to a corresponding reflecting cup 30 . The reflecting plates 20 are rotatable adjusted by a controller (not shown). The controller may be a motor or an electrical components etc. The reflecting plate 20 may be asynchronized. At the same time, only one reflecting plate 20 reflects light of the light source 10 . The controller controls a frequency of the rotation of the reflecting plates 20 to adjust the light efficiency. If the reflecting plates 20 rotate in a higher frequency, a light with a consistent intensity may be visible for people. If the reflecting plates 20 rotate in a lower frequency, a light with a variational intensity may be visible for people.
[0011] The substrate 100 is made of transparent thermal conductive material and located at top of the reflecting plates 20 . In this disclosure, the substrate 100 is located above the light path of the light source 10 and parallel to the light path of the light source 10 . The substrate 100 includes a first surface 101 and a second surface 102 opposite to the first surface 101 . The first surface 101 is spaced from the reflecting plate 20 . The plurality of reflecting cups 30 and the lamp shell 50 are mounted on the second surface 102 .
[0012] The plurality of reflecting cups 30 faces to the reflecting plates 20 . Each of the reflecting cups 30 includes a top surface 31 and an inner surface 32 extending from the top surface 31 . The inner surface 32 defines a hole therebetween. The diameter of the hole of the reflecting cup 30 is gradually decreasing from the top surface 31 to a bottom of the reflecting cup 30 . The bottom of the hole is filled with a phosphor layer 40 .
[0013] The lamp shell 50 is mounted on the second surface 102 and spaced from and covers the reflecting cup 30 . The lamp shell 50 includes a main portion 51 and a plurality of extending portions 52 . The main portion 51 includes a top surface 511 . The plurality of extending portions 52 is located above the top surface 511 of the main portion 51 . The main portion 51 extends from the second surface 102 . The cross section of the main portion 51 is a rectangular. Each of the extending portions 52 includes a connecting portion 521 protruding from the main portion 51 and a top portion 522 protruding from the center of the connecting portion 521 . Every extending portion 52 faces to a corresponding reflecting cup 30 . The width of the extending portion 52 is equal to or larger than that of the reflecting cup 30 , and each of the extending portions 52 is located above the reflecting cup 30 . The center of the top portion 522 is convex. The extending portions 52 have a function of the convex lens to gather the light.
[0014] In the present disclosure, the light from the light source 10 is reflected by the reflecting plates 20 and the reflecting cup 30 in series and then gathered by the lamp shell 50 . The reflecting plates 20 can rotate fast or slowly. So the frequency of the rotation can be controlled to adjust the light efficiency by the controller.
[0015] It is to be further understood that even though numerous characteristics and advantages have been set forth in the foregoing description of embodiments, together with details of the structures and functions of the embodiments, the disclosure is illustrative only; and that changes may be made in the details, including in matters of shape, size, and arrangement of parts within the principles of the disclosure to the full extent indicated by the broad general meaning of the terms in which the appended claims are expressed.
[0016] The embodiments shown and described above are only examples. Many details are often found in the art such as the other features of an automotive daytime running light. Therefore, many such details are neither shown nor described. Even though numerous characteristics and advantages of the present technology have been set forth in the foregoing description, together with details of the structure and function of the present disclosure, the disclosure is illustrative only, and changes may be made in the detail, including in matters of shape, size and arrangement of the parts within the principles of the present disclosure up to, and including the full extent established by the broad general meaning of the terms used in the claims. It will therefore be appreciated that the embodiments described above may be modified within the scope of the claims.
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Automotive daytime running lights, includes a light source and reflecting plates arranged on a light path of the light source. A substrate is arranged near the reflecting plates. A plurality of reflecting cups is formed on a surface of the substrate. Every reflecting plate faces a corresponding reflecting cup. The reflecting plates can rotate around light source to change the light exiting from the light source. The invention uses a laser source with reflecting plates to make the automotive daytime running lights have high visibility and be aesthetic in appearance.
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FIELD OF THE INVENTION
[0001] The present invention generally concerns payment solutions and commercial incentive mechanisms in the credit card, debit card, and personal check industries, incentivizing both a merchant's acceptance of a payment solution and a customer's preferential use of a payment solution in making purchases. More particularly, the invention concerns processes for automatic generation of discounts when using these methods of payment in purchase transactions.
BACKGROUND OF THE INVENTION
[0002] In the past decades, there has been increased competition among institutions that provide and support payment solutions such as credit cards, debit cards, and personal checks. The type of providers has diversified from only banks to associations, consumer product merchants, and other third-parties. As a way of attracting more clients, institutions have created incentive programs that are associated with these methods of payment, with the goal of incentivizing use of their payment solutions over those of their competitors.
[0003] A type of credit card, often called a “reward card,” illustrates this trend. When using a reward card to pay for a purchase, a customer is rewarded for the use of the credit card by receiving pre-defined amounts of capitalization units, which include “points”, “miles,” or “rewards.” Amounts of these capitalization units are accumulated in a special account and traded later for pre-defined goods and services or, in some instances, for cash.
[0004] On the other hand, merchants that offer products and services for sale also are increasingly competitive in recent years, and offer lower and lower prices and more deals in order to entice customers to shop with them. The options available to merchants seeking to incentivize purchase through them include the offering of coupons and store-branded discount credit cards associated with a merchant that offer various perks in connection with their use (such as, for example, a Macy's® credit card that offers reward points useable only at Macy's® stores). However, one practical problem with these is that, in order to benefit from discounts from several merchants, a user has to subscribe to as many store-branded cards. Having to carry many cards is impractical. In addition, a user who would possess many store-branded credit cards would bear the burden of managing many bank accounts, which is undesirable.
[0005] As a matter of background, and in order to fully comprehend the scope of the disclosed invention, it is useful to understand the operation of methods of payment such as credit cards, debit cards, and personal checks(as well as associated methods of payment) as they are used in a purchase transaction. The purchase transaction begins by the customer paying for an order from a merchant using the method of payment. After scanning of the method of payment using the merchant's point of sale equipment, the merchant sends customer information (such as, for example, a customer's name, address, customer identification information, and the amount of purchase) to a payment gateway which, in turn, checks a payment gateway database to identify a merchant acquiring bank associated with the merchant. The merchant acquiring bank is an actor in a purchase transaction and a bank or financial institution the merchant has an agreement with to process its purchase transactions, and thereby accepts payments on behalf of the merchant.
[0006] After the merchant acquiring bank receives the customer's information, it is forwarded to a payment processor supporting the customer's method of payment, such as, for example, Visa, MasterCard, or American Express if the method of payment is a credit card. The payment processor is another actor in a purchase transaction. The payment processor also has an agreement or contract in place to act as a go between for the merchant acquiring bank and later actors in the purchase transaction.
[0007] The payment processor accesses a computer database to determine which payment issuing bank is associated with the customer information. Each method of payment is associated with a certain payment issuing bank that issues it, another actor in a purchase transaction, and having another agreement or contract to issue payment to other actors in the purchase transaction. Once the correct payment issuing bank is discovered by the payment processor, the customer information is further transmitted there. The payment issuing bank then executes a lookup regarding the customer information on its own computer database to determine whether there are enough funds present or not, whether the billing address with the customer information provided by the merchant matches the billing address in the file, and other pertinent information. Based upon this, if appropriate, an approval message is sent to the payment processor that forwards it to the merchant acquiring bank that again forwards it to the merchant to complete the transaction. Alternately, if the customer's information indicates that the transaction should not be allowed, a denial message is sent along the same path.
[0008] In practice, additional institutions may be receiving, processing and transmitting information on the way from the payment processor to the payment issuing bank, as well as on the way back from the payment issuing bank. However, these additional institutions are not particularly relevant to the present invention. For instance, when the method of payment is a credit card, often the credit card brand (as for instance VISA or MasterCard) receives data, processes it, and sends it to the credit payment issuing bank. Similarly, some of the intermediate roles in the transaction may, in practice, be assumed by a single institution.
[0009] The present invention offers the opportunity for automatic generation of discount transactions by any of the institutions in a purchase transaction with the goal of providing a stronger incentive to the user, while also allowing a large set of institutions to use the present invention as a promotional vehicle. Instantaneous and easy discounts generated automatically encourage the use of a method of payment. The customer benefits by not having to carry a large number of membership cards or clipping and carrying coupons while still receiving discounts.
[0010] The desire to increase the customer base and gain advantage over competitors offering a similar payment solution is not limited, however to the payment issuing bank. In an embodiment of the invention, the merchant benefits by receiving automatically generated discounts on fees owed to the payment issuing bank which encourages merchants to accept a certain method of payment. The merchant does not have to install special payment processing machines and data connections dedicated to a unique method of payment in order to utilize this embodiment of the invention, which greatly enhances membership. Even the market for payment processors has become more competitive and with a desire to increase market share discounts are offered when a payment processor's services are used. In effect, when customers make a payment at the merchant using a method of payment, the payment processor generates a discount transaction payment and sends it to the merchant acquiring bank. This serves to encourage merchants to promote the payment processor's own methods of payment.
[0011] Further facilitating membership in an embodiment of the invention is that the invention does not require an expensive permanent data link to the institution responsible for generation of discount transactions. Instead, in this embodiment the invention acts to supplement existing transaction processing systems. Goals are achieved via an asynchronous connection, whereby data regarding the sales transactions is not necessarily transmitted in real-time but rather at asynchronous intervals and a data set regarding discount transaction data is generated remotely and returned to the merchant.
[0012] Discount transactions are also generated automatically by multiple institutions in the credit card payment process, making it more attractive to make purchases with them.
[0013] An embodiment of the present invention is optimally used by the payment issuing bank, which issues discount transactions to incentivize use of its own payment solutions. The payment issuing bank is responsible for settling requests for payments made directly or indirectly by merchants, when the payment is made by a customer using the method of payment issued by the issuing bank. As such, the bank naturally receives all transaction data associated with the method of payment. Although the payment issuing bank optimally uses the present invention, any institution involved in the processing of transactions, such as the merchant itself, the merchant acquiring bank, or even the payment processor benefits from embodiments of the invention, incentivizing their own financial services over their competitors. The invention also is employed by another party or a “discount processing party,” outside the traditional payment processing method who has data containing the available discounts and who receives at some point in the processing pathway the transaction data. This discount processing party then compares the transaction data with the data representing available discounts and creates a discount data set which it sends to the payment issuing bank for transmission to the merchant acquiring bank. Optionally, this party can send the discount data set to the payment processor or directly to the merchant acquiring bank. In one embodiment of the invention, the discount data set is sent by this discount processing party after the payment issuing bank has sent payment for the amount of the transaction to the merchant acquiring bank. In such embodiment the merchant acquiring bank sends payment representing the amount of the discount back to the payment issuing bank. In another embodiment of the invention the discount processing party sends the discount data set to the payment issuing bank or payment processor prior to the payment issuing bank having sent payment for the transaction to the merchant acquiring bank whereupon the issuing bank sends to the merchant acquiring bank an amount representing the transaction amount minus the discount amount for that purchase.
[0014] Prior art exists in the realm of discount programs. In U.S. Pat. No. 5,056,019, Schultz et al. discloses an “Automated Purchase Reward Accounting System and Method” that requires customers to carry one bar-coded membership card per merchant. Since the number of merchants a customer frequents is typically high (in the order of dozens), it requires a customer to carry a large number of membership cards. Furthermore, modifications to a merchant's existing point of sale equipment are required to take advantage of this invention.
[0015] In U.S. Pat. No. 6,014,635 Harris et al. discloses a “System and Method for Providing a Discount Credit Transaction Network” that again requires modifications to existing point of sale devices to recognize authorizations for sales transactions from a payment issuing bank and authorizations for discounts from a discount credit network. This invention also requires modifications to the chain of transaction processing between a merchant acquiring bank and the payment issuing bank, both differing from the present invention.
[0016] In U.S. Pat. No. 5,689,100 Carrithers et al. discloses a “Debit Card System and Method for Implementing Incentive Award Program.” This invention differs from the present invention in that it discloses a reward system where capitalization units must be put into a separate account which must be used exclusively to buy products or services at certain merchants who accept such capitalization units. This separate account also makes bookkeeping more difficult.
[0017] In U.S. Pat. No. 6,292,786 Deaton et al. discloses a “Method and System for Generating Incentives Based on Substantially Real-Time Product Purchase Information.” This invention, unlike the present invention, requires merchants to install and maintain a connection between the taught system and each point-of-sale. It also requires modifying the chain of transaction processing between the merchant bank and the payment issuing bank.
[0018] In U.S. Pat. No. 6,601,761 Katis discloses a “Method and System for Co-Branding an Electronic Payment Platform such as an Electronic Wallet.” This invention, however, requires merchants (who are possibly in direct competition) to join a common incentive program. Another limitation is that the only way for the customer to redeem the dollar amount that corresponds to the incentives is through buying further products from merchants participating in the common incentive program. If incentives are paper coupons, customers might be required to buy certain products at certain times.
[0019] In U.S. Pat. No. 7,747,524 Brown discloses a “Method and System for Discount Debit Card.” In this invention, the front-end processing is performed the traditional way: with transaction information being transmitted from a merchant to a merchant's acquiring processor and to a discount plan provider system. However, two major aspects of back-end processing, where the settlement occurs, are different in Brown. First, back-end processing does not involve the merchant's acquiring processor. Second, responsibility for distributing fees is given to the discount plan provider system, as opposed to other parties. Furthermore, the acquiring processor of every merchant involved in the discount plan would need to implement the special mode of operation. As discussed earlier, this is a logistical impediment to the actual implementation of the taught invention, and hence a significant limitation.
[0020] While these units may be suitable for the particular purpose employed, or for general use, they would not be as suitable for the purposes of the present invention as disclosed here.
SUMMARY OF THE INVENTION
[0021] The present invention provides methods and systems of payment for automatic generation of discount transactions. Automatic generation of discount transactions incentivizes the use of a certain method of payment or the services of an institution that provides payment services over a competitor. Rather than conventional coupons, discount cards, frequent flier miles, or other perks of limited value, which still involve substantial effort on the part of a customer to use, discounts are generated automatically and effortlessly. Customers prefer discount programs to reward programs (such as reward programs that accumulate points, miles, or rewards) because typical discounts offered by merchants represent a higher percentage of the purchased value than rewards. Thus, the discounts offered are a strong incentive to use a given method of payment over another, or use the products or services offered by a certain merchant, payment issuing bank, merchant acquiring bank, or payment processor over another.
[0022] It is an object of the invention to communicate purchase transaction data regarding a method of payment such as a credit card, debit card, or personal check when data transmission facilities are available, rather than always immediately when a transaction is processed, while still granting automatic discount transactions efficiently. Accordingly, an embodiment of the invention utilizes asynchronous communications where any combination of a merchant acquiring bank, a payment processor, and a credit payment issuing bank are not in constant data communication but instead communicate transaction data or discount data either immediately or at a later time. Thus, in this embodiment if a transaction is processed immediately but data transmission is not available at the time, the full amount of purchase is sent which is later discounted, in part. On the other hand, if data transmission facilities are available immediately the determination of whether there is an available discount on a purchase is made immediately and payment for the discounted transaction is also sent immediately. It is even possible that a subset of a group of purchase transactions have been completed whereas others are still pending.
[0023] It is a further object of the invention to generate discount transactions by matching data on processed transactions with data regarding available discounts. Accordingly, in an embodiment of the invention discount transactions are automatically generated by receiving purchase transaction data then executing a lookup on a computer database containing information on available discounts, which after computer matching the data on available discounts is returned asynchronously, either immediately or a at a later time then data transmission facilities are available.
[0024] It is a further object of the invention to allow a discount transaction to be sent either at the “front-end” of the transaction or during the “back-end” processing. Accordingly, in an embodiment of the invention as a result of the asynchrony when the method of payment offering a discount transaction is used in paying for a transaction the transmission and processing of the discount transaction happens either during the so-called “front-end” processing or during the “back-end” processing. In the “front-end” processing data representing a purchase transaction is compared to a data set representing available discounts in a database by one of the entities in the traditional processing system (e.g. a merchant acquiring bank, a payment processor, a payment issuing bank, etc.) or by a discount processing party to create a data set representing available discounts for that transaction prior to the payment issuing bank sending payment to the merchant acquiring bank. The data set representing available discounts is received by the payment issuing bank which then uses the data set representing available discounts to calculate the payment for the transaction owed to the merchant acquiring bank. Thus, the discount for the particular transaction is determined prior to payment to the merchant acquiring bank and the payment to the merchant acquiring bank is adjusted to take into account any discounts for the transaction. On the other hand, in the “back end” processing the data set representing a purchase transaction is asynchronously compared to data set representing available discounts in a database by one of the entities in the traditional processing system (e.g. the merchant acquiring bank, the payment processor, the payment issuing bank, etc.) or by a discount processing party to create a data set representing a discount for that transaction after the payment issuing bank has sent payment to the merchant acquiring bank. A discount amount is then determined and sent to the merchant acquiring bank which then sends to the payment issuing bank an amount representing the original price minus the discounted amount to the payment issuing bank.
[0025] It is another object of the invention to obviate the need for customers to carry multiple membership cards issued by individual merchants to participate in a discount program. Maintaining one membership card per merchant frequented by a customer is difficult and time consuming, especially when you consider the number of merchants that desire the customer to utilize their unique membership cards. Accordingly, an embodiment of the invention does not rely on membership cards in its generation of automatic discounts, but rather relies on customer information associated with a payment solution.
[0026] It is still a further object of the invention to not require further specialized point of sale equipment other than that typically used to process methods of payment. Accordingly, an embodiment of the invention does not use anything beyond standard customer transaction data transmitted during a purchase transaction, and therefore does not require specialized point of sale equipment other than the merchant's point of sale equipment.
[0027] It is a further object of the invention to avoid the necessity of customers carrying coupons with them where they shop. Accordingly in an embodiment of the invention, discounts with the present invention do not involve utilization of coupons. Instead, the invention determines which discounts are available, then issues discounts based upon these details. Paper coupons are not involved at all.
[0028] It is still a further object of the invention to offer instantaneous return of capitalization units. Prior-art discount systems place capitalization units in a separate account which must later be used at pre-defined merchants and further these accounts require maintenance by the customer of a separate account. Accordingly, an embodiment of the present invention simplifies this process and offers instantaneous discounts on goods or services purchased.
[0029] It is still a further object of the invention to create a method for plan participants to dictate their own discount terms and conditions in an embodiment of the invention. Accordingly, in an embodiment of the invention an internet menu system is available for plan participants to access and define their own available discounts, which are later accessed and matched automatically. Discount terms and conditions are established by the plan participants, including the necessity to purchase a certain amount of goods or services, granting a discount only at certain times, demanding that a certain amount of goods or services are sold before discounts begin to issue, or otherwise.
[0030] It is still a further object of the invention to generate data sets representing purchase transactions automatically and then provide them to merchants via merchant acquiring banks. Accordingly, in an embodiment of the invention data representing available discounts is formed based upon a subset of data representing purchase transactions, and this information is sent by the issuing bank to the merchant acquiring bank for use in promoting sales and in other ways.
[0031] It is still a further object of the invention to increase and incentivize impulse buying by messaging customers in real-time as they are shopping to encourage them to buy more. Accordingly, in an embodiment of the invention purchases are tracked in real-time and compared with available discounts which are then forwarded to customers also in real-time via e-mail, SMS, Facebook®, or some other means. Being offered a sale while shopping capitalizes on human nature, demanding something be purchased only because it is less expensive at that time.
[0032] It is still a further object of the invention to increase and incentivize impulse buying by messaging customers when they are near to being eligible for a discount or further discount. This includes, for example, when the customer's amount of purchases at a merchant is near a level of purchase amount that would entitle the customer to a discount or further discount if the level of purchase is reached. Accordingly, in an embodiment of the invention purchases are tracked and compared with available discounts which are then forwarded to customers via e-mail, SMS, Facebook®, or some other means. Knowing that they are within reach of being entitled to a discount or additional discount at a particular merchant also capitalizes on human nature, incentivizing additional purchases because it will entitle the customer to a discount or additional discounts.
[0033] It is yet a further object of the invention to more strongly incentivize impulse buying. Accordingly, in an embodiment of the invention no pre-planning is necessary before discounts are received (pre-planning could include, for example, clipping coupons before shopping).
[0034] It is yet a further object of the invention to be able to ascertain which discount transactions are most useful and which the least in attracting customers while tracking locations where sales are made. Accordingly, in an embodiment of the invention, data representing issued discounts is stored and used in generating further discounts, along with data regarding locations of sales to customers.
[0035] One efficient way to determine such location is to obtain the location of each merchant and then to deduce the location of the sale from the identification of the merchant that is available on documents and data generated during the transaction. However, other ways to determine the location of the sale are acceptable as well. This information is later used in generating data representing available discounts or in other business research.
[0036] To the accomplishment of the above and related objects, the invention 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 invention, limited only by the scope of the claims.
BRIEF DESCRIPTION OF THE DRAWINGS
[0037] In the drawings, like elements are depicted by like reference numerals. Various embodiments of the present invention are illustrated by way of example, and not by way of limitation, in the figures of the accompanying diagrams. The drawings are briefly described as follows:
[0038] FIG. 1 is a flowchart illustrating the operational flow of a method of payment and process for automatic generation of discounts in an embodiment of the invention.
[0039] FIG. 2 is a flowchart illustrating the operational flow of a further embodiment of the invention displaying a method of payment and process for automatic generation of discounts.
[0040] FIG. 3 is a flowchart illustrating a process of matching of purchase transactions with available discounts in an embodiment of the invention.
[0041] FIGS. 4A and 4B are together a flowchart displaying the operational flow of selecting admissible discounts based upon certain criteria in an embodiment of the invention.
[0042] FIGS. 5A and 5B illustrate another flowchart displaying the process of generation of a message discussing the discount transactions in an embodiment of the invention.
[0043] FIG. 6 is a flowchart illustrating the process of generating discount transactions in an embodiment of the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
[0044] FIG. 1 is a flowchart illustrating the operational flow of a process for automatic generation of discounts in an embodiment of the invention executing on a local data processor associated with a computer database. Flow begins in block 105 . At 110 , data representing a purchase transaction between a merchant and a customer (paid for with a method of payment such as a credit card, debit card, personal check, or associated method of payment) is received asynchronously. The purchase transaction may or may not have already completed, and therefore data is received “asynchronously” to the purchase transaction itself 110 . The data representing a purchase transaction may include (but is not limited to) identification of merchant, identification of customer, credit card number, amount of purchase and location of purchase. Flow continues to block 120 , where data representing available discounts on the computer database are accessed by the local data processor. Flow continues in block 130 , where the data representing the purchase transaction is matched with the data representing the available discounts to define a set of discounts on the purchase transaction. If there are conditions precedent to the receipt of the available discount, they are analyzed at step 130 by the local data processor's logic circuits. Examples of conditions include a condition that the purchase transaction is issued after a prescribed start date and time and before a prescribed end date and time, or a condition that the purchase transaction must be valued under or over a certain dollar value. Flow of the provided embodiment continues again in block 140 , where a transaction data set is generated in-part from the data resulting from the set of discounts matched with the purchase transaction in block 130 .
[0045] The transaction data set generated at step 140 may include, but is not limited to data identifying the merchant, data identifying the customer, the amount of the discount, and data allowing the merchant to check the validity of the discount. The generated data set is then sent directly or indirectly to the merchant's acquiring bank, initiating a new transaction. Actual encodings for the transaction data are obvious to one of skill in the art.
[0046] At 150 a monetary amount for the discount is computed and totaled with monetary amounts for prior discounts and a data set representing the transaction that applied the discount is generated.
[0047] The form taken by a payment the discount transaction in block 140 is obvious to the skilled in the art. At present, we believe that one good form for the transaction data generated in block 140 is in the form of an ACH transfer, for its low, fixed cost. The typical cost for an ACH transfer is in the order of half a cent. However, other forms are also satisfactory. ACH transfer stands for “Automatic Clearinghouse” or “Automatic Check Handling” transfer. ACH transfers are a standard protocol for transferring money from one bank to another.
[0048] Execution continues through the decision at step 160 and back to start 105 if there are more transactions to process. Otherwise, execution completes 170 .
[0049] FIG. 2 represents flow of another process for generating a commercial discount transaction in a further embodiment of the present invention. Flow begins again in block 105 . Data representing a purchase transaction between a customer and a merchant is received at step 110 . Data representing available discounts is accessed on a local data processor associated with a computer database 120 . At step 230 data representing available discounts (previously accessed at step 120 ) is compared to data representing the purchase transaction (previously received asynchronously at step 110 ). A pair is then formed from the data set representing available discounts and data representing the purchase transaction 240 . The monetary amount for this discount is then computed and totaled with prior calculated discounts 150 . If there are more transactions to process, execution of the program proceeds from step 160 back to step 105 . Otherwise execution goes to step 165 where a commercial discounts transaction total is sent to asynchronous discount transaction program participant 165 , then termination ends 170 .
[0050] Mechanisms for performing the matching process of FIG. 2 , step 240 are obvious to one of skill in the art. Typical implementations use a computer database managed by a structured query language like SQL. SQL provides structured queries formulated in the SQL language, or one of its existing extensions, to facilitate easy, efficient, and economical returns of requested data from the database. Examples of brand names for database systems that support SQL and its extensions include, but are not limited to, Oracle, PostgreSQL, and MySQL. However, other ways of forming a pair as required in step 240 are also satisfactory, such as hash functions. Hash functions are mappings that take a dataset and produce a simple index, allowing efficient comparison and matching of data sets.
[0051] FIG. 3 represents a flow of another process for generating a commercial discount transaction in yet another embodiment of the present invention. Flow begins at step 105 . The invention asynchronously receives data representing a purchase transaction between customer and merchant 110 . In this embodiment a data set of all available discounts is received as well 321 . A set of admissible matching criteria is inferred from the information available in the purchase transaction data set 322 . A subset of available discounts that involve the admissible matching criteria is extracted 323 from the whole data set of available discounts. After step 323 and from step 130 and beyond, execution of FIG. 3 continues as with FIG. 1 .
[0052] In a further embodiment displayed as FIGS. 4A and 4B , flow begins at step 105 . Data representing a purchase transaction between a customer and a merchant is received asynchronously in step 110 . Data representing available discounts is accessed on a local data processor associated with a computer database 120 . At step 230 data representing the available discounts from step 120 is compared with data representing the purchase transaction from step 110 . Currently matched transaction data is stored in a database 410 . A set of previously stored matched transaction data sets involving both user and merchant of currently matched data set within a prescribed period of time are collected 415 . A sum of purchase amounts in collected transaction data sets is computed 420 . At step 425 a decision must be made whether the sum of purchase amounts is greater than a prescribed minimum purchase amount that the customer must have spent in purchases from the merchant within a prescribed period of time. If yes, execution continues in FIG. 4B , otherwise execution completes 430 . In FIG. 4B , a pair of data sets from the currently matched transaction data set and the matched discount data set is formed 440 . A monetary amount for a discount is computed and totaled with prior discounts calculated 150 . If there are more purchase transactions to process execution returns to start 105 in FIG. 4A . Otherwise, a commercial discounts transaction total is sent to an asynchronous discount transaction program participant 165 . Execution is now complete 170 .
[0053] FIGS. 5A and 5B display another embodiment of the invention. Flow starts at step 105 . Execution is as before with FIGS. 4A and 4B until step 510 on FIG. 5B . At step 510 a value for the difference between the prescribed amount and sum is calculated. In this embodiment a message is generated containing a description of the matched discount 520 . The message is then sent via a messaging system accessible by the user. The contents of the message may include, but are not limited to, text identifying the merchant, the amount associated with the discount, the period of time for the discount and the computed difference, or other items. However, contents containing more or less information are also satisfying. Exemplars of such a messaging system are well known to the skilled in the art. The messaging systems include but are not limited to e-mail servers, webmail, web-based messaging, Short Message Service (SMS), fax, and integrated messaging systems such as available through Facebook, Google+, and the like. Other messaging systems are also appropriate. At steps 425 and beyond, execution of this embodiment continues as with FIG. 4B .
[0054] FIG. 6 represents the flow of another embodiment of the present invention. In this embodiment execution commences at step 610 and a customer purchases a product from a merchant using a method of payment in step 615 . The merchant then collects information associated with the method of payment in step 620 , and produces an original transaction data set. The information associated with the original transaction data set includes but is not limited to the item purchased, the amount paid, the name of the customer, the date of the transaction, and the location of the transaction. The flow continues in step 625 , where the original transaction data set is sent to a merchant acquiring bank associated with the merchant. This bank may be either the merchant acquiring bank, or another bank serving as merchant acquiring bank for the purposes of processing the merchant acquiring bank's financial transactions. The flow then continues in step 630 , where the merchant acquiring bank receives the original transaction data set from the merchant, processes it, if required, and sends a new transaction data set to a payment processor for the method of payment. The payment processor for the method payment is a bank or similar institution responsible for processing and dispatching transactions. In this embodiment, the flow continues in step 635 , where the payment processor receives the new transaction data set from the merchant acquiring bank, processes it if required, and sends a further new transaction data set to the payment issuing bank. The further new transaction data set is received by the payment issuing bank in step 640 , where it is verified and approved. Flow continues to step 640 , where execution continues simultaneously to steps 650 (where the payment issuing bank produces a discount transaction data set by processing further new transaction data set) and 670 (where the issuing bank sends approval data to the payment processor). These steps and those following indicate the asynchrony of the execution of this embodiment of the invention as two paths proceed simultaneously. The flow proceeds from step 650 to 655 where the issuing bank sends the discount transaction data set to the merchant acquiring bank. At 660 the merchant acquiring bank receives the discount transaction data set. The merchant acquiring bank asynchronously sends payment for the amount of discount to the issuing bank 665 . While steps 650 through 665 are proceeding, the issuing bank sends approval data to the payment processor 670 . The payment processor then receives issuing bank approval data, processes it if required, and sends processor approval data to merchant acquiring bank 675 . The merchant acquiring bank receives processor approval data 680 .
[0055] At step 685 the issuing bank asynchronously sends payment for original transaction to the payment processor. The payment processor then receives payment, optionally pays portion of original transaction amount to zero or more parties, and sends payment of remaining amount to merchant acquiring bank 690 . At step 697 , the merchant acquiring bank receives payment for the original transaction from payment processor. From both steps 697 and 665 execution of the simultaneous paths completes 699 .
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Due to increased competition in the financial services market for merchants, merchant acquiring banks, payment processors, and card-issuing banks, a method and system of payment for automatic generation of discount transactions is offered. Any actor in the purchasing process generates discounts automatically by receiving a purchase transaction dataset, comparing available discount datasets, and asynchronously generating a discount in a manner more accessible than coupons or reward cards.
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This is a division of application Ser. No. 448,621, filed Dec. 10, 1982, now abandoned.
BACKGROUND OF THE INVENTION
I. Field of the Invention
This invention relates to the securement of glass in fire doors and the like. More particularly, the invention relates to such securement avoiding the use of visible metal parts.
II. Description of the Prior Art
The use of windows or lights in fire doors is advantageous because a person escaping from a fire can immediately see whether it is safe to open the door or whether the fire is worse on the other side. Furthermore, as fire doors usually have to be kept closed at all times, the presence of windows or lights provides a building with a less claustrophobic appearance.
The disadvantage of the use of windows or lights in fire doors is that they can reduce the ability of the door to prevent the spread of fire. Heat-resistant glass can be employed, but the frame around the glass is susceptible to burning. To overcome this, metal frames are often provided around the windows or lights, but when the fire door itself is made of wood, this significantly reduces the attractiveness of the door. The use of metal frames can also be expensive.
It is therefore an object of the present invention to provide an alternative to the use of metal frames without reducing the fire retardancy of the door below specified levels.
SUMMARY OF THE INVENTION
According to one aspect of the invention there is provided a glazing strip for fire barriers comprising an elongated strip made of a wood-like material formed from a slurry mixture of wood fibers and a fire retardant chemical through the use of heat and pressure.
The elongated strip is preferably made of a plurality of layers of the wood-like material of uniform thickness that are adhered to one another.
According to another aspect of the invention there is provided a clip for mounting heat-resistant glass in an opening in a fire barrier, comprising a thin, flat base of rigid heat-resistant material and a pair of projections upstanding from said base arranged parallel to each other and separated by a distance corresponding to the width of glass to be mounted.
According to yet another aspect of the invention there is provided a fire barrier having a glass panel therein, said glass panel being secured in said barrier by means of at least one clip comprising a thin flat base of heat-resistant material and a pair of projections upstanding from said base arranged parallel to one another and separated by a distance corresponding to the width of the glass panel, and elongated glazing strips on opposite sides of said panel at the edges thereof, said strips being made of a wood-like material formed from a slurry mixture of wood fibers and a fire retardant chemical through the use of heat and pressure.
The novel clips may be used in combination with the novel glazing strips at any time, but are preferably required when the glazing strips are thinner than 3/4 inch in front of the glass. The clips can, of course, be used with other types of glazing strips.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front elevation of a fire barrier to which a preferred form of the present invention has been applied;
FIG. 2 shows the steps in preparing the material for the glazing strips used in one form of the invention;
FIGS. 3 to 6 are cross-sections of various parts of the fire barrier of FIG. 1;
FIGS. 7 to 9 are perspective views of various clips used in the invention;
FIGS. 10 and 11 show a glazing bar in greater detail; and
FIG. 12 shows the manner in which a clip and glazing bar can be attached to the fire barrier.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS
A typical application for the present invention is the fire barrier shown generally at 10 in FIG. 1. This barrier consists of a fire door 11 and a floor to ceiling, immovable side light 12.
The door 11 is mounted within a suitable fire-resistant frame 13, which may be a conventional fire-resistant door frame.
The side light 12 is also formed by a suitable fire-resistant frame 14, preferably of the same material as the door frame 13.
The door 11 may have any conventional fire-retardant structure and has a glass panel 16 made of a heat-resistant glass, e.g. one quarter inch thick wired glass. The side light 12 has two glass panels 17, 18 made of the same or similar heat-resistant glass. The two panels are mounted one above the other as shown and are separated by a cross-member 19 of the frame.
The difficulty in the past has been to mount the various glass panels within the door or frame in such a manner that the desired fire retardancy of the barrier 10 is maintained. This has been achieved by the use of metal glazing bars or stops to shield the junction between the glass and frame material and to fix the glass firmly in place. The mounting of the glass panels can now be carried out without the use of visible metal parts.
This is achieved by making the glazing bars or stops of a particular fire retardant material resembling wood. This material is made of pressed wood fibers containing a fire retardant additive, and is preferably used in the form of a plurality of thin sheets of such material laminated together. The material is formed by subjecting wood chips to either pressurized steam or a chemical bath to break the wood down into its individual fibers in the form of a wet slurry. This wet slurry is then reformed by spreading it onto the open screened surface mat where it is subject to pressure and heat. A natural chemical component of wood then flows to hold the wood fibers together in their new form. A fire retardant material is conveniently added during the manufacturing process while the fibers are still in a wet slurry in such a manner that the material is dispersed throughout the resulting wood product substantially uniformly. The amount of the fire retardant chemical is preferably in excess of 30% by weight of the sheet material. The fire retardant material may alternatively be impregnated into the individual fibers themselves. An aluminum compound, for example alumina, aluminum hydroxide or aluminum silicate, is a suitable fire retardant. Boron compounds are also known fire retardants and can be utilized. Preferably, the fire retardant compound is other than a salt as salts may leach out, but salts can be employed if desired. The specific gravity of the resulting fibre board is preferably greater than 0.80.
The material is preferably produced as thin (eg. quarter inch thick) sheets which can then be laminated together to any desired total thickness. This is preferable to forming a sheet of the total desired thickness because thicker sheets may have reduced internal strength, i.e., the fibers may tend to pull apart. Further, the laminated structure may also provide greater rigidity and improved ability to hold screws, nails and other fasteners.
The sheets can be adhered together using any suitable glue, but a glue sold under the trade mark UF 109 by Borden Chemicals Ltd. has been found especially advantageous because of its resistance to heat. The adhering of the sheets may be achieved by applying a layer of wet glue to both faces of alternate layers of the material, leaving the intervening layers dry. The layers are then built up to the desired total thickness and the combination is subjected in a press to pressure until the glue is cured.
The lamination technique is shown in FIG. 2, in which part (a) shows a single sheet of fiber board 21, part (b) shows four such boards laminated together to form a composite board 22, and part (c) shows a glazing bar or stop 23 made by cutting the composite sheet 22 to the required size. A veneer (if required) can be provided either on the composite sheet 22 or on the glazing bar or stop 23 after cutting.
A commercially available wood fiber board that is satisfactory for this application is one designated as X-90®-FT sold under a Flame Test® panel brand by the Masonite Corporation. This material is obtained in wall panel sheets of typical thickness of 0.245 inch, with a specific gravity typically of 1.10, and includes an aluminum compound as a fire retardant in the proportion of approximately 35% of its weight. For use in the preferred forms of the present invention, such sheets are glued together to form a composite or laminated structure. Any number of sheets may be laminated in this way, but four such laminations usually provide the desired thickness.
This material was developed to prevent flame spread along the surface of the material when installed as wall paneling in buildings and mobile homes. However, it has been found that such material has improved fire penetration characteristics.
The composite material is highly resistant to burning and has a texture and appearance similar to wood. Further, the material retains nails, screws and other fasteners in much the same way as wood. As mentioned above, in order to improve the appearance of the product further, it may be provided with a wood veneer on the visible surfaces, which makes it virtually indistinguishable from wood.
The laminated wood fiber board is used to hold the glass panels in place and to shield the glass/frame junctions from heat and flame. FIGS. 3 to 6 show how the composite, fire-retardant material can be used in the fire barrier 10 shown in FIG. 1.
FIG. 3 is a cross-section of the barrier 10 taken on the line III--III in FIG. 1. The composite, fire-retardant material is used for the glazing strips, i.e., for the glazing bars 24 for the glass panel 16 in door 11, and in glazing stops 26 for the glass panel 17 (and similarly for panel 18) in the side light 12.
FIGS. 4 to 6 are, respectively, cross-sections taken along the lines IV--IV, V--V and VI--VI of FIG. 1 to show the glazing strips in greater detail.
The glazing strips can be fixed in position by any suitable conventional means, e.g. by nails, screws, glue, etc. By themselves these strips are suitable for holding the glass panels in position when their thickness in front of the glass surface is at least 3/4 inch and their fire retardancy then prevents penetration by flame around the edges of the glass panels. The dimensions of the strips can be chosen according to the design of the fire barrier and according to the degree of fire retardancy required. Naturally, the strips should be present all around the glass panels on both sides to form an effective fire seal.
When the thickness of the strip in front of the glass is less than 3/4 inch it is desirable, in order to maintain adequate fire retardancy, to use novel clips to fix the glass panels in position in addition to the fire retardant glazing strips themselves. When this is done, the glass panels remain in place even when the strips are burnt away, so that the panels can still resist pressure differences on opposite sides of the barrier and even the force of fire hoses directed against the barrier.
Examples of the novel clips are shown in FIGS. 7 to 9, the clips being indicated by the reference numerals 27, 28 and 29 respectively. Basically, each clip comprises a flat base plate 31 and a pair of uprights 32. The uprights 32 are separated by a distance corresponding to the width of the glass panel with which they are to be used. The uprights engage each side of the glass panel adjacent an edge and the flat base 31 is nailed, screwed, glued or otherwise attached to the opening for the glass in the door or frame. A number of such clips are used for each glass panel, and preferably they are spaced about twelve inches apart (and about 6 inches from each corner) to provide adequate support for the panel. Glazing bars or stops of the type described above are then secured against the panel edges to hide the clips and provide the desired fire retardancy. In this way, no metal parts are visible in the finished barrier which appears to be constructed entirely of wood.
Clip 27 consists of a channel member 33 soldered, welded or otherwise attached to the mid-line of the flat base 31. The sides of the channel member form the uprights 32.
Clip 28 has a pair of L-shaped members attached to the flat base 31, the angled parts forming the uprights 32.
Clip 29 is made from a single plate bent to form the flat base 31 and uprights 32.
The clips can be made from any rigid, heat-resistant material, but metal is preferred and galvanized steel sheet is ideal. The clips may be made of any suitable size to suit any application. The most usual size for the flat base is 1×15/8 inches, the uprights usually extend 1/4 inch from the base and are usually separated by a distance of 1/4 inch, although this depends entirely on the thickness of glass to be employed.
The clips 27 may be positioned as shown in FIG. 1. In this case, no clips are provided on the lower panel 18 of the side light 12. This is because the lower panel would be subjected to less heat and flame during a normal fire, as heat rises, and therefore does not need the additional support. The clips may however be provided if desired.
FIGS. 10 and 11 show an example of a glazing bar 36 according to one form of the invention. This is L-shaped in cross-section so that it can be used in the manner shown in FIG. 6 for similar bars 24. The four layers 37, 38, 39, 40 are shown in FIG. 11 together with wood veneer layers 42, 43, 44. If just a paint grade product is required, the layers of veneer can be omitted. The bar 36 differs in shape from the glazing stops, e.g. as shown at 26 in FIG. 3, which are rectangular in cross section, but they are otherwise the same. The bars and stops can be made in any desired cross-sectional shape and length. Standard lengths can be produced and cut to size on site, or lengths designed to fit particular standard doors can be made.
FIG. 12 shows more clearly the way in which the clips and glazing strips may be secured to a door or door frame. The clip 27 is first secured to door 11 by means of nails 45 (the glass panel--not shown--may be manoeuvered into position with the clips attached to it and then the clips may be nailed in place). A layer of double-sided adhesive tape 47 is then attached to the glazing bar 24, which is then located in the position shown by an adhesive or by nailing or the like. A similar glazing bar with double-sided adhesive tape is attached on the other side of the glass panel. The adhesive tape acts as a seal between the glazing bars and the glass and temporarily secures the glazing bars in place while they are being permanently attached.
When the glazing strip is to be attached by nails or screws, it is preferable to ensure that they pass through the laminate material at right angles to the laminations. For example, the nails or screws would be introduced into the upper surface of the bar 24 shown in FIG. 12. The laminate material has an improved ability to retain nails and screws when they traverse the laminations rather than extend parallel to them.
The following Example illustrates one preferred form of the present invention.
EXAMPLE
A fire barrier of the design shown in FIG. 1 (45 inches high by 52 inches wide) was manufactured using glazing strips comprising four laminations of X-90®FT wood fiber material. These strips were of the shape shown in FIG. 12, the outer dimension being 1 inch by 11/4 inches and the cut-out portion being 1/2 by 3/4 inch. The visible faces were veneered. Metal clips were used where shown in FIG. 1.
The barrier was subjected to a fire test by an independent laboratory (Warnock Hersey Professional Services Ltd., Vancouver, Canada). Five burners were each placed six inches from the barrier and the average temperatures that the exposed face of the barrier was subjected to were as follows:
5 minutes: 1036° F.
10 minutes: 1301° F.
15 minutes: 1390° F.
20 minutes: 1474° F.
The barrier contained the fire for 20 minutes. The burners were then turned off and the barrier was subjected to a hose stream against the exposed (burnt) face from a hose having a 28 mm discharge tip. The hose produced a pressure of 207 Kpa and the barrier was sprayed in a zig-zag pattern for an average of 6.7 seconds per square meter (32 seconds in total).
The barrier stood up to the fire test and the hose stream test adequately, i.e., there were no visible openings through the barrier.
The invention is not limited to the details of the preferred embodiment referred to above and includes modifications that would be apparent to a person skilled in this art and that fall within the scope of the following claims.
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Apparatus for securing glass panels in fire barriers comprises an elongated glazing strip made of layers of sheet material adhered together. The sheet material is formed from a slurry mixture of wood fibers and a fire retardant chemical by the use of heat and pressure. The panels are also preferably secured by metal clips having a flat base of thin sheet material and upstanding, elongated projections from the base that are parallel to each other and spaced apart by a distance corresponding to the width of the glass panel to be secured. This arrangement makes it possible to locate glass panels in fire barriers without substantial reduction in the ability of the barrier to contain a fire.
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This application is a division of prior application Ser. No. 10/097,832, filed Mar. 15, 2002, now U.S. Pat. No. 6,566,766 which is the division of prior grandparent application Ser. No. 09/690,023, filed on Oct. 17, 2000, now U.S. Pat. No. 6,404,076.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention relates to a DC-DC converter circuit for converting DC voltage to another DC voltage, a power supply selection circuit for selecting one of a plurality of power supplies, and an apparatus provided with such a DC-DC converter circuit.
2. Description of the Related Art
Many of portable type of electronic apparatuses such as a note personal computer and the like are so arranged that they operate from electric power obtained from a commercial power supply and a battery incorporated therein as well.
Usually, such an apparatus incorporates therein a circuit for changing over as to which source of electric power, the commercial power supply or the battery, is used to operate the apparatus (for example, Japanese Patent Laid Open Gazette Hei.9-182288, and Japanese Patent Laid Open Gazette Hei.9-308102). According to such type of circuit, when electric power obtained from the commercial power supply is supplied to the apparatus, this electric power takes precedence in use, and when the circuit detects that the supply of power from the commercial power supply stops, the supply of power changes to the supply of power from the battery. As another type of the power supply switching circuit, a circuit is arranged in such a manner that, in view of the fact that electric power obtained from the commercial power supply is generally higher in voltage than that from the battery, the supply of power selected is from the electric power of the highest voltage of the plurality of electric powers.
Incidentally, the voltage of a battery decreases as the battery discharges. Thus, an apparatus is provided with a DC-DC converter circuit for maintaining the voltage of electric power used in the apparatus.
FIG. 7 is a circuit diagram showing a first example of a linear regulator. The linear regulator is one type of a DC-DC converter circuit, and it is generally widely used.
A linear regulator section 10 is loaded on an LSI having an input terminal IN through which electric power of input voltage Vin is applied. The linear regulator section 10 converts the electric power of the input voltage Vin to electric power of output voltage Vout (Vin>Vout) lower than the input voltage Vin, and outputs electric power of the output voltage Vout through an output terminal OUT.
Between the input terminal IN and the output terminal OUT, an NPN transistor 11 for output voltage control is disposed, and between the input terminal IN and a base of the NPN transistor 11 , a constant current source 12 is disposed. A current outputted from the constant current source 12 flows through the base of the NPN transistor 11 in the form of a base current thereof, and further flows through a collector of an additional NPN transistor 13 in the form of a collector current thereof. An emitter of the NPN transistor 13 is connected to a ground terminal GND, which is grounded. The output voltage Vout of the output terminal OUT is fed to a plus input terminal of a differential amplifier 16 in the form of a potential division by two resistances 14 and 15 , while a reference voltage generated by a reference voltage source 17 is fed to a minus input terminal of the differential amplifier 16 . An output terminal of the differential amplifier 16 is connected to a base of the NPN transistor 13 .
In the event that the output voltage Vout of the output terminal OUT is biased with a voltage higher than a predetermined reference output voltage, the output voltage of the differential amplifier 16 increases, so that a collector current of the NPN transistor 13 increases. That is, of the current outputted from the constant current source 12 , one used as the collector current of the NPN transistor 13 increases, and as a result, the base current of the NPN transistor 11 for output voltage control decreases and thereby the output voltage Vout of the output terminal OUT decreases.
Conversely, in the event that the output voltage Vout of the output terminal OUT is biased with a voltage lower than a predetermined reference output voltage, the output voltage of the differential amplifier 16 decreases, so that the collector current of the NPN transistor 13 also decreases. That is, the base current of the NPN transistor 11 increases and thereby the output voltage Vout of the output terminal OUT increases.
In this manner, the electric power of a constant output voltage Vout is outputted from the output terminal OUT.
FIG. 8 is a circuit diagram showing a second example of a linear regulator. The following description sets forth the differences from the first example of the linear regulator shown in FIG. 7 , hereinafter.
A linear regulator 10 ′ shown in FIG. 8 is provided with a PNP transistor 18 for output voltage control, instead of the NPN transistor 11 for output voltage control in the linear regulator 10 shown in FIG. 7 . As a result, the output voltage Vout of the output terminal OUT is fed to the minus input terminal of the differential amplifier 16 in form of a potential division by two resistances 14 and 15 , while the reference voltage generated by the reference voltage source 17 is fed to the plus input terminal of the differential amplifier 16 .
In the event that the output voltage Vout of the output terminal OUT is biased with a voltage higher than a predetermined reference output voltage, the output voltage of the differential amplifier 16 decreases, so that a collector current of the NPN transistor 13 also decreases. That is, of the current outputted from the constant current source 12 , one used as the collector current of the NPN transistor 13 decreases, and as a result, the base current of the PNP transistor 18 decreases and thereby the output voltage Vout of the output terminal OUT decreases.
Conversely, in the event that the output voltage Vout of the output terminal OUT is biased with a voltage lower than a predetermined reference output voltage, the output voltage of the differential amplifier 16 increases, so that the collector current of the NPN transistor 13 also increases. That is, the base current of the PNP transistor 18 increases and thereby the output voltage Vout of the output terminal OUT increases.
In this manner, an electric power of a constant output voltage Vout is outputted from the output terminal OUT.
FIG. 9 is a circuit diagram showing a third example of a linear regulator.
A main difference from the second example of the linear regulator shown in FIG. 8 is that the PNP transistor 18 is replaced by P channel MOS transistor 19 . With respect to circuit operation, it is the same as that of the second example shown in FIG. 8 , and thus a redundant explanation will be omitted.
FIG. 10 is a circuit diagram showing an example of a switching regulator. The switching regulator 20 is also a type of DC-DC converter circuit, and it is generally widely used.
An electric power of voltage Vin is fed through an input terminal IN of the switching regulator, and an electric power of output voltage Vout (here dealing with a step-down type and thus Vin>Vout) is outputted from a second output terminal OUT 2 , of first and second output terminals OUT 1 and OUT 2 . Between the first and second output terminals OUT 1 and OUT 2 , an outside coil 31 is connected. Between the second output terminals OUT 2 and the ground, an outside capacitor 32 is connected.
Elements of the switching regulator 20 , except outside coil 31 and outside capacitance 32 , are loaded on an LSI.
Between the input terminal IN and the output terminal OUT 1 , P channel MOS transistor 21 is disposed. An output of a PWM comparator 26 is connected to a gate of the P channel MOS transistor 21 . An output of a differential amplifier 24 and an output of a triangle wave generator 27 are fed to the PWM comparator 26 . The PWM comparator 26 will be described later.
The voltage Vout of the second output terminal OUT 2 is fed to a minus input terminal of the differential amplifier 24 in form of a potential division by two resistances 22 and 23 , while a reference voltage generated by a reference voltage source 25 is fed to a plus input terminal of the differential amplifier 24 . Between the first output terminal OUT 1 and a ground terminal GND which is grounded, a diode 28 is connected. A cathode of the diode 28 is connected to the first output terminal OUT 1 , and an anode of the diode 28 is connected to the ground terminal GND.
The PWM comparator 26 compares an output voltage of the differential amplifier 24 with a triangle wave signal outputted from the triangle wave generator 27 . When the output voltage of the differential amplifier 24 is lower in voltage than the triangle wave signal, the PWM comparator 26 generates a pulse signal of ‘H’ level. When the output voltage of the differential amplifier 24 is higher in voltage than the triangle wave signal, the PWM comparator 26 generates a pulse signal of ‘L’ level. Such a pulse signal is fed to the gate of the MOS transistor 21 , so that the MOS transistor 21 turns on or off in accordance with the variation between the ‘H’ level and the ‘L’ level of the pulse signal. That is, the MOS transistor 21 switches the input voltage Vin at the same repetitive frequency as that of the triangle wave signal.
The diode 28 , the coil 31 and the capacitor 32 smooth the input voltage Vin after the switching and generate the output voltage Vout.
When the output voltage Vout slightly exceeds a set up voltage, the output voltage of the differential amplifier 24 decreases, so that a pulse width (a pulse width of the ‘L’ level) of the pulse signal generated by the PWM comparator 26 narrows slightly and thereby the output voltage Vout decreases. Conversely, when the output voltage Vout decreases, the output voltage of the differential amplifier 24 increases, so that a pulse width (a pulse width of the ‘L’ level) of the pulse signal generated by the PWM comparator 26 expands and thereby the output voltage Vout increases. Thus, the switching regulator 20 controls the electric power of a constant voltage Vout to be outputted.
SUMMARY OF THE INVENTION
In an electronic apparatus, for example, a personal computer, there is frequently a case that a plurality of circuit units, operative with mutually different DC voltages, exist in the apparatus. Such an apparatus has a plurality of DC-DC converter circuits which output electric powers of individual voltages, respectively. A DC-DC converter circuit is associated with such disadvantages that a great deal of useless electric power is consumed for conversion of DC voltage, and as a result, the consumption of battery charge is hastened, and also this is associated with a temperature rise of the apparatus. For example, in case of the DC-DC converter circuit of the linear regulator scheme shown in FIGS. 7 to 9 , for conversion from the input voltage of 16 volts into the output voltage of 3.3 volts, the conversion efficiency is 20%, and the remaining 80% is a power loss. Particularly, in an apparatus in which a plurality of mutually different DC voltages are used and a plurality of DC-DC converter circuits are needed in order to generate the plurality of mutually different DC voltages, it is a problem as to how the conversion efficiency is improved in the DC-DC converter circuits.
In view of the foregoing, it is an object of the present invention to provide a DC-DC converter circuit improved in conversion efficiency, a power supply selection circuit in which an existing DC-DC converter circuit is used to perform a voltage conversion improved in conversion efficiency, and an apparatus incorporated thereinto such a DC-DC converter circuit improved in conversion efficiency.
To achieve the above-mentioned objects, the present invention provides a first DC-DC converter circuit having a plurality of input terminals connected to a plurality of DC power supplies, respectively, and an output terminal. This DC-DC converter circuit has a power supply selection section for selecting the DC power supply of the lowest voltage on the condition that the voltage is not less than a predetermined voltage. This DC-DC convertor circuit also has a step-down type of regulator section for converting the voltage of the DC power supply selected by the power supply selection section into a predetermined voltage lower than the voltage of the DC power supply selected by the power supply selection section, and outputting the converted voltage through the output terminal.
As mentioned above, in case of the DC-DC converter circuit according to the linear regulator scheme, the conversion efficiency is 20% for a conversion of 16V to 3.3V. Conversely, in a case where a power supply of 5V exists, the conversion efficiency is 66% for the same conversion. In this manner, when an output voltage is obtained from an input voltage which is close to the output voltage as much as possible, it is possible to greatly improve the conversion efficiency. This is applicable also to the switching regulator scheme as well as the linear regulator scheme.
The first DC-DC converter circuit according to the present invention utilizes this principle as mentioned above.
That is, the power supply selection section selects a DC power supply of the lowest voltage from among a plurality of DC power supplies, and transmits the selected DC power supply to the regulator section. However, in this case, in order to avoid such a situation that the lowest detected voltage is when no power supply is connected, or the connected power supply is not operative, so that the lowest voltage is 0V, there is a requirement that the lowest voltage is not less than a predetermined voltage. The regulator section converts the voltage of the DC power supply thus selected to a DC voltage lower than the voltage of the selected DC power supply. Thus, it is possible to implement high efficiency voltage conversion wherein the optimum power supply is selected in accordance with the state of the power supplies.
To achieve the above-mentioned objects, the present invention provides a second DC-DC converter circuit having a first input terminal connected to a predetermined first DC power supply, a second input terminal connected to a predetermined second DC power supply of a voltage lower than that of the first DC power supply, and an output terminal. This DC-DC converter circuit has a power supply selection section for selecting the first DC power supply connected to the first input terminal and the second DC power supply connected to the second input terminal, the voltage of the second DC power supply being less than a predetermined voltage or is not less than the predetermined voltage, respectively. This DC-DC converter circuit also has a step-down type of regulator section for converting the voltage of the DC power supply selected by the power supply selection section into a predetermined voltage lower than the voltage of the DC power supply selected by the power supply selection section, and outputting the converted voltage through the output terminal.
In the event that it is decided that, as compared with the voltage of the first DC power supply entered through the first input terminal, the voltage of the second DC power supply entered through the second input terminal is lower, or it is arranged in such a manner as mentioned above on a connection basis, it is possible to simplify the power supply selection section in structure taking into account the idea of the first DC-DC converter circuit of the present invention.
In either of the first and second DC-DC converter circuits according to the present invention, it is acceptable that the regulator section have a linear regulator. In this case, it is preferable that the power supply selection section and the regulator section having the linear regulator are arranged in a chip of an integrated circuit. Or alternatively, it is preferable that the power supply selection circuit and portions of the regulator section having the linear regulator, except for an output voltage control transistor, are arranged in a chip of an integrated circuit.
In any of the first and second DC-DC converter circuits according to the present invention, it is acceptable that the regulator section have a switching regulator. In this case, it is preferable that the power supply selection section and portions of the regulator section having the switching regulator, except for a voltage smoothing circuit portion which is to be disposed outside, are arranged in a chip of an integrated circuit.
Arrangement in a chip of an integrated circuit makes possible a more stable operation, cost-reduction, and space saving.
To achieve the above-mentioned objects, there is provided a first power supply selection circuit having a plurality of input terminals connected to a plurality of DC power supplies; a power supply selection section for selecting a DC power supply of the lowest voltage, on the condition that the voltage is not less than a predetermined voltage, from among the plurality of DC power supplies; and an output terminal for outputting the voltage of the DC power supply selected by the power supply selection section.
To achieve the above-mentioned objects, there is provided a second power supply selection circuit having a first input terminal connected to a predetermined first DC power supply; a second input terminal connected to a predetermined second DC power supply of which the voltage is lower than the voltage of the first DC power supply; a power supply selection section for selecting the first DC power supply connected to the first input terminal and the second DC power supply connected to the second input terminal according to the voltage of the second DC power supply being less than a predetermined voltage or is not less than the predetermined voltage, respectively; and an output terminal for outputting the voltage of the DC power supply selected by the power supply selection section.
The first and second power supply selection circuits correspond to the power supply selection sections of the first and second DC-DC converter circuits, respectively. The DC-DC converter circuits corresponding to the regulator sections of the first and second DC-DC converter circuits are connected to the later stages of the first and second power supply selection circuits, respectively. This feature makes it possible to perform a highly efficient DC-DC conversion for the DC-DC converter circuits.
To achieve the above-mentioned objects, there is provided an apparatus operative upon receipt of an electric power having a step-down type of first DC-DC converter for converting a first DC voltage of a predetermined first DC power supply into a predetermined second DC voltage lower than the first DC voltage of the first DC power supply; a first operating circuit operative upon receipt of supply of an electric power of the second DC voltage obtained by the first DC-DC converter; a second DC-DC converter having a step-down type of regulator section for converting a received DC voltage into a predetermined third DC voltage lower than the received DC voltage, and a power supply selection section responsive to both the first DC voltage of the first DC power supply and an output of the first DC-DC converter for selectively transmitting to the regulator section the output of the first DC-DC converter and the first DC voltage of the first DC power supply according as the output of the first DC-DC converter is not less than a predetermined voltage or is less than the predetermined voltage, respectively; and a second operative circuit operative upon receipt of electric power supplied by the third DC voltage obtained by the second DC-DC converter.
The apparatus of the present invention as mentioned above is provided with two DC-DC converters of the first and second DC-DC converters. The second DC-DC converter, which outputs the lower DC voltage, is arranged with the first or second DC-DC converter circuit. This feature makes it possible to perform a DC-DC conversion excellent in efficiency, and also to implement a reduction of the consumed power and a suppression of temperature increase of the apparatus.
Generally, power supply systems are wired within apparatuses beforehand, and therefore the arrangement of the second DC-DC converter circuit of the present invention is generally used as the second DC-DC converter. However, it is acceptable that the first DC-DC converter circuit of the present invention is used as the second DC-DC converter. At that time, the power supply selection section of the second DC-DC converter serves to block both the path for transmitting the output of the first DC-DC converter to the regulator section and the path for transmitting the voltage of the first DC power supply to the regulator section, when the first DC power supply is less than a predetermined voltage, in the event that the output of the first DC-DC converter is less than a predetermined voltage.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a circuit diagram of a first embodiment of a DC-DC converter circuit according to the present invention, including a first embodiment of a power supply selection circuit according to the present invention.
FIG. 2 is a circuit diagram of a second embodiment of a DC-DC converter circuit according to the present invention, including a second embodiment of a power supply selection circuit according to the present invention.
FIG. 3 is a circuit diagram of a third embodiment of a DC-DC converter circuit according to the present invention.
FIG. 4 is a circuit diagram of a fourth embodiment of a DC-DC converter circuit according to the present invention.
FIG. 5 is a circuit diagram of a fifth embodiment of a DC-DC converter circuit according to the present invention.
FIG. 6 is a block diagram showing an embodiment of an apparatus according to the present invention.
FIG. 7 is a circuit diagram showing a first conventional example of a linear regulator.
FIG. 8 is a circuit diagram showing a second conventional example of a linear regulator.
FIG. 9 is a circuit diagram showing a third conventional example of a linear regulator.
FIG. 10 is a circuit diagram showing a conventional example of a switching regulator.
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
Embodiments of the present invention will be described with reference to the accompanying drawings.
FIG. 1 is a circuit diagram of a first embodiment of a DC-DC converter circuit according to the present invention, including a first embodiment of a power supply selection circuit according to the present invention.
A DC-DC converter circuit 100 shown in FIG. 1 comprises an input selection circuit 110 and a linear regulator 10 . The DC-DC converter circuit 100 is loaded onto a one LSI chip 190 in its entirety. The input selection circuit 110 is an embodiment of a power supply selection circuit of the present invention.
The input selection circuit 110 is provided with two input terminals IN 1 and IN 2 to which DC supplies are connected, respectively. Input voltages Vin1 and Vin2 are applied through the input terminals IN 1 and IN 2 , respectively.
Between the input terminals IN 1 and IN 2 and a node TML for transferring signals from the input selection circuit 110 to the linear regulator section 10 , wherein in the event that the input selection circuit 110 is constructed in the form of a circuit separated from the linear regulator section 10 (for example, only the input selection circuit 110 is loaded onto an LSI), the node TML is an output terminal of the input selection circuit 110 , diodes 111 and 112 of which anodes are connected to the input terminals IN 1 and IN 2 , respectively, and P channel MOS transistors 113 and 114 are disposed. Input sides of the P channel MOS transistors 113 and 114 are connected via resistances 115 and 116 to their gates, respectively. Between the gates of the P channel MOS transistors 113 and 114 and a ground terminal GND, N channel MOS transistors 117 and 118 are disposed, respectively. The ground terminal GND is grounded.
The input selection circuit 110 is further provided with first, second and third comparators 121 , 122 and 123 , and a reference voltage source 124 . A plus input terminal of the first comparator 121 is connected to a cathode of the diode 111 , and a minus input terminal of the first comparator 121 is connected to the reference voltage source 124 . A plus input terminal of the second comparator 122 is connected to a cathode of the diode 112 , and a minus input terminal of the second comparator 122 is connected to the cathode of the diode 111 . A plus input terminal of the third comparator 123 is connected to the reference voltage source 124 , and a minus input terminal of the third comparator 123 is connected to the cathode of the diode 112 .
Outputs of those three comparators 121 , 122 and 123 are transmitted via a first logical circuit 133 comprising an AND gate 131 and an OR gate 132 to the N channel MOS transistor 117 , and further transmitted via a second logical circuit 136 comprising an OR gate 134 and a NAND gate 135 to another N channel MOS transistor 118 .
The first comparator 121 compares voltage Vin1 of the first input terminals IN 1 with the voltage of the reference voltage source 124 , and determines whether the voltage Vin1 of the first input terminals IN 1 is higher than the voltage of the reference voltage source 124 . In other words, it is determined whether the reference voltage source 124 is connected to the first input terminals IN 1 .
In a similar fashion to that of the first comparator 121 , the third comparator 123 compares voltage Vin2 of the second input terminals IN 2 with the voltage of the reference voltage source 124 , and determines whether the voltage Vin2 of the second input terminals IN 2 is higher than the voltage of the reference voltage source 124 . In other words, it is determined whether the reference voltage source 124 is connected to the second input terminals IN 2 .
The second comparator 122 is different from the first comparator 121 and the third comparator 123 , and compares the voltage Vin1 of the first input terminal IN 1 with the voltage Vin2 of the second input terminal IN 2 .
When the voltage Vin1 of the first input terminal IN 1 exceeds the reference voltage and Vin1<Vin2, the first logical circuit 133 generates an ‘H’ level of signal, so that the NMOS transistor 117 conducts and the potential of the gate of the PMOS transistor 113 decreases to the potential of the ground side. Thus the PMOS transistor 113 turns on, so that the voltage Vin1 of the first input terminal IN 1 is transmitted via the node TML to the linear regulator section 10 . At that time, the output (the gate of the NMOS transistor 118 ) of the second logical circuit 136 transitions to the ‘L’ level, so that the NMOS transistor 118 turns off. Thus the PMOS transistor 114 also turns off, so that the voltage Vin2 of the second input terminal IN 2 is not transmitted to the linear regulator section 10 .
For example, it is assumed that Vin1=5.0V, Vin2=16.0V. In the event that the linear regulator section 10 outputs voltage of 3.3V, the input selection circuit 110 selects Vin1=5.0V. Thus, the efficiency of the linear regulator section 10 is 66%.
On the other hand, in the case of Vin2<Vin1, when Vin2 exceeds the reference voltage, the output of the first logical circuit 133 transitions to the ‘L’ level, and the second logical circuit 136 transitions to the ‘H’ level. Thus, the NMOS transistor 117 and the PMOS transistor 113 turn off, so that transfer of Vin1 to the linear regulator section 10 is inhibited, and the NMOS transistor 118 and the PMOS transistor 114 turn on, so that Vin2 is transferred to the linear regulator section 10 . In this case, for example, assuming that Vin1=16.0V, Vin2=5.0V and the linear regulator section 10 outputs voltage of 3.3V, the input selection circuit 110 selects Vin2=5.0V. Thus, the efficiency of the linear regulator section 10 is 66%.
In the event that Vin2 is less than the reference voltage (typically the input terminal IN 2 is disconnected with the source), while Vin1 is not less than the reference voltage, the first, second and third comparators 121 , 122 and 123 transition to the ‘H’ level, ‘L’ level, and ‘H’ level of signals, respectively, so that the first logical circuit 133 generates an ‘H’ level of signal, and the second logical circuit 136 generates an ‘L’ level of signal. Thus, the NMOS transistor 117 conducts and the PMOS transistor 113 also conduct. On the other hand, the NMOS transistor 118 turns off and the PMOS transistor 114 also turns off. Consequently, in this case, the voltage Vin1 entered through the first input terminal IN 1 is transmitted to the linear regulator section 10 . In the event that the linear regulator section 10 outputs a voltage of 3.3V, the efficiency of the linear regulator section 10 is 66% when Vin1=5.0V, and is 20% when Vin1=16.0V.
On the other hand, in the event that Vin1 is less than the reference voltage (typically the input terminal IN 1 is disconnected with the source) while Vin2 is not less than the reference voltage, the first, second and third comparators 121 , 122 and 123 transition to the ‘L’ level, ‘H’ level, and ‘L’ level of signals, respectively, so that the first logical circuit 133 generates an ‘L’ level of signal, and the second logical circuit 136 generates an ‘H’ level of signal. Thus, the NMOS transistor 117 turns off and the PMOS transistor 113 also turns off. On the other hand, the NMOS transistor 118 turns on and the PMOS transistor 114 also turns on. Consequently, in this case, the voltage Vin2 entered through the second input terminal IN 2 is transmitted to the linear regulator section 10 . In the event that the linear regulator section 10 outputs voltage of 3.3V, the efficiency of the linear regulator section 10 is 66% when Vin2=5.0V and 20% when Vin2=16.0V.
The linear regulator section 10 has the same structure as the linear regulator shown in FIG. 7 , and it generates in accordance with the principle explained referring to FIG. 7 the stabilized output voltage Vout (Vout<Vin1, Vin2) lower than voltages Vin1 and Vin2 of the input terminals IN 1 and IN 2 . For example, Vout=3.3V, and the output is the same through the output terminal OUT.
In this manner, in case of the DC-DC converter circuit 100 shown in FIG. 1 , of two input voltages Vin1 and Vin2, the smaller one is transmitted to the linear regulator section 10 so as to be used for generating the output voltage Vout, on the condition that it is not less than the reference voltage. Thus, it is possible to perform a DC-DC conversion improved in conversion efficiency.
FIG. 2 is a circuit diagram of a second embodiment of a DC-DC converter circuit according to the present invention, including a second embodiment of a power supply selection circuit according to the present invention.
A DC-DC converter circuit 200 shown in FIG. 2 comprises an input selection circuit 210 which is more simplified in structure as compared with the input selection circuit 110 according to the first embodiment shown in FIG. 1 , and a linear regulator section 10 which has the same structure as the linear regulator section 10 according to the first embodiment shown in FIG. 1 . In a similar fashion to that of the first embodiment shown in FIG. 1 , the DC-DC converter circuit 200 is loaded onto a one LSI chip 290 in its entirety.
The DC-DC converter circuit 200 is a circuit wherein it is intended to receive input voltages Vin1 and Vin2 through the input terminals IN 1 and IN 2 , respectively, ensuring Vin1>Vin2. Assuring that Vin1 is greater than Vin2 may be implemented by means of, for example, differentiating types of connectors, or fixedly wiring the respective connectors in an apparatus beforehand.
Between the first input terminal IN 1 of the two input terminals IN 1 and IN 2 and a node TML coupling between the input selection circuit 210 and the linear regulator section 10 , there are disposed a diode 211 of which an anode is connected to the input terminal IN 1 and a PMOS transistor 213 . Here, in the event that the input selection circuit (an example of the power supply selection circuit referred to in the present invention) is arranged in form of a circuit separated from the linear regulator section 10 (for example, only the input selection circuit 210 is loaded on a one LSI chip), the node TML is an output terminal of the input selection circuit 210 . The gate of the PMOS transistor 213 is connected via a resistance 215 to the diode 211 . Between the gate of the PMOS transistor 213 and the ground terminal GND, an NMOS transistor 217 is disposed. The ground terminal GND is grounded.
Between another input terminal IN 2 and the node TML, a diode 212 is disposed, an anode of which is connected to the input terminal IN 2 . A cathode of the diode 212 is connected to a minus input terminal of a comparator 221 . A reference voltage source 224 is connected to a plus input terminal of the comparator 221 . An output of the comparator 221 is connected to a gate of the NMOS transistor 217 .
The comparator 221 compares the voltage Vin2 of the input terminal IN 2 with a reference voltage obtained by the reference voltage source 224 . This comparison is for a determination as to whether the reference voltage source 224 is surely connected to the second input terminal IN 2 .
When the voltage Vin2 is higher than the reference voltage, the output of the comparator 221 offers ‘L’ level, so that the NMOS transistor 217 turns off. Thus, the PMOS transistor 213 also turns off. As a result, the voltage Vin1 of the first input terminal IN 1 is not transmitted to the linear regulator section 10 , but the voltage Vin2 of the second input terminal IN 2 is transmitted to the linear regulator section 10 . On the other hand, in the event that the voltage Vin2 of the second input terminal IN 2 transitions to a voltage (typically 0V) lower than the reference voltage, for example, such cases that the source is not connected to the second input terminal IN 2 , or that the source connected to the second input terminal IN 2 is in condition of turn-off, the output of the comparator 221 transitions to an ‘H’ level, so that the NMOS transistor 217 turns on. Thus, the PMOS transistor 213 also turns on. As a result, the voltage Vin1 of the first input terminal IN 1 is transmitted to the linear regulator section 10 .
As mentioned above, the input selection circuit 210 shown in FIG. 2 is effective in the event that the condition of Vin1>Vin2 is satisfied. When the voltage Vin2 is effective, the voltage Vin2 is transmitted to the linear regulator section 10 . When the voltage Vin2 is not effective (e.g. 0V), the voltage Vin1 is transmitted to the linear regulator section 10 .
The linear regulator section 10 is the same as the linear regulator section shown in FIG. 1 in structure, and generates the stabilized output voltage Vout lower than voltages Vin1 and Vin2 of the input terminals IN 1 and IN 2 , and outputs the same through the output terminal OUT.
In this manner, also in the case of the DC-DC converter circuit 200 , when the voltage Vin2 of the voltages Vin1 and Vin2 (voltages Vin1>Vin2) is sufficient, the voltage Vin2 is transmitted to the linear regulator section 10 to be used for generation of the output voltage Vout. Thus, it is possible to perform a DC-DC conversion improved in conversion efficiency.
FIG. 3 is a circuit diagram of a third embodiment of a DC-DC converter circuit according to the present invention. Described now are features different from those of the second embodiment shown in FIG. 2 .
A different feature of a DC-DC converter circuit 300 from the second embodiment shown in FIG. 2 resides in that a portion, not an NPN transistor 11 , of the output voltage control section constituting the linear regulator section 10 is loaded onto an LSI chip 390 , and the NPN transistor 11 is disposed outside the LSI chip 390 . Thus, the LSI chip 390 needs two output terminals OUT 1 and OUT 2 in addition to an output terminal OUT 3 corresponding to the output terminal OUT in the second embodiment shown in FIG. 2 .
The operation of the circuit is the same as that of the second embodiment shown in FIG. 2 , and thus redundant explanation will be omitted. The reason why the transistor 11 is disposed outside the LSI chip 390 is as follows. The DC-DC converter circuit 300 is of a large current capacity so that the secondary end thereof is permitted to consume a very large electric power, and thus as the transistor 11 , there is a need to use a transistor which is capable of withstanding consumption of the large electric power. In view of the above-mentioned matter, a large capacity of transistor is needed as the transistor 11 , and in addition, there is a need to perform a heat radiation by installing, for example, a heat sink and the like. That is, the transistor 11 is not suitable for incorporation into the LSI chip.
Thus, in a DC-DC converter circuit of a linear regulator scheme, it happens that a transistor for the output voltage control is mounted outside.
FIG. 4 is a circuit diagram of a fourth embodiment of a DC-DC converter circuit according to the present invention.
A DC-DC converter circuit 400 shown in FIG. 4 also comprises an input selection circuit 110 , which is the first embodiment of the power supply selection circuit of the present invention also shown in FIG. 1 , and a switching regulator section 20 which is the same as the switching regulator shown in FIG. 10 . The circuit operation of the input selection circuit 110 and the switching regulator section 20 has been already explained, and thus redundant explanation is omitted. The DC-DC converter circuit 400 shown in FIG. 4 is loaded on an LSI chip 490 , except for a coil 31 and a capacitor 32 , which are part of the switching regulator 20 . The coil 31 and the capacitor 32 are considerably large and are not suitable for placement on the LSI chip.
The input selection circuit 110 receives two input voltages Vin1 and Vin2 (it is acceptable that either of the input voltages Vin1 and Vin2 may be a low voltage) applied through the two input terminals IN 1 and IN 2 , respectively. Of the two input voltages Vin1 and Vin2, the lower voltage is applied to a switching regulator section 20 on the condition that the lower voltage is not less than the reference voltage. The switching regulator section 20 is of a step-down type of regulator for generating an output voltage Vout which is lower than the voltages Vin1 and Vin2. Thus, it is preferable for conversion efficiency that the output voltage Vout is generated in accordance with the lower input voltage (if, of course, it is not less than the output voltage Vout). In this manner, also in the embodiment shown in FIG. 4 , there is adopted a scheme wherein of the input voltages Vin1 and Vin2, the lower voltage is applied to generate the output voltage Vout, and thereby implementing the more efficient DC-DC conversion.
FIG. 5 is a circuit diagram of a fifth embodiment of a DC-DC converter circuit according to the present invention.
A DC-DC converter circuit 500 shown in FIG. 5 comprises the input selection circuit 210 corresponding to the second embodiment of the power supply selection circuit of the present invention shown in FIG. 2 , and the switching regulator section 20 which is the same as the switching regulator section 20 shown in FIG. 20 . The circuit operation of the input selection circuit 210 and the switching regulator section 20 have already been explained, and thus redundant explanation is omitted. The DC-DC converter circuit 500 shown in FIG. 5 is loaded on an LSI chip 590 , except for a coil 31 and a capacitor 32 , which are part of the switching regulator section 20 , in a manner similar to that of the fourth embodiment shown in FIG. 4 .
In the input selection circuit 110 , when the sources are both of the two input terminals IN 1 and IN 2 , the inequality Vin1>Vin2 is always satisfied. In the event that the input voltage Vin2 is not less than a predetermined reference voltage, the input voltage Vin2 is transmitted to the switching regulator section 20 . And on the other hand, in the event that the input voltage Vin2 is not more than the predetermined reference voltage, the input voltage Vin1 is transmitted to the switching regulator section 20 . Therefore, in the switching regulator section 20 , it is possible to perform a more efficient DC-DC conversion.
FIG. 6 is a block diagram showing an embodiment of an apparatus according to the present invention.
An apparatus 600 , for example, a personal computer, is supplied with DC power of 16.0 V generated from a commercial power supply in an external AC adapter (not illustrated), and DC power of 12 to 9 V generated from an internal battery 611 , through diodes 612 and 613 , respectively. Since the DC power (16.0 V) from the external AC adapter is higher than the voltage (12 to 9 V) of the battery, when the DC power is supplied from the AC adapter, the power from the battery is not supplied to the apparatus due to operation of the diode 613 . On the other hand, when no power is supplied from the AC adapter, and the apparatus 600 is operating, power is supplied from the battery 611 . The power from the AC adapter or the battery 611 is fed to a DC-DC converter 614 (for example, the first DC-DC converter referred to in the present invention) and a regulator 615 (for example, the second DC-DC converter referred to in the present invention).
The DC-DC converter 614 supplies 5.0V of electric power to a first operating circuit 616 . The first operating circuit 616 is driven by the power of 5.0V generated from the DC-DC converter 614 . The DC-DC converter 614 receives a control signal (an on/off signal) for turning on and off the DC-DC converter, so that the DC-DC converter 614 may stop operating for the purpose of saving power when there is no need for the first operating circuit 616 to operate.
The regulator 615 receives power of 5.0V from the DC-DC converter 614 received from either the AC adapter or the battery 611 , and supplies power of 3.3V in accordance with lower power of the received two types of power. The power of 3.3V from the regulator 615 is supplied to a second operating circuit 617 . The second operating circuit 617 is activated by the power of 3.3V supplied from the regulator 615 . The second operating circuit 617 comprises circuits and the like which are needed to be kept operating on an interruptible power supply basis.
While it is acceptable that as the regulator 615 , any one of the above-mentioned embodiments of DC-DC converter circuit may be adopted, typically, the DC-DC converter circuit shown in FIG. 2 is adopted because it is wired beforehand, since it is incorporated into the apparatus.
When the DC-DC converter 614 operates, and the power of 5.0V generated from the DC-DC converter 614 is fed to the regulator 615 , the regulator 615 generates power of 3.3V from an input power of 5.0V. When the DC-DC converter 614 stops operating, the regulator 615 generates power of 3.3V in accordance with the power of 16.0V from the AC adapter or the power of 12 to 9V from the battery 611 when the AC adapter is not connected.
In this manner, the regulator 615 is so arranged that when the DC-DC converter 614 operates, the power of 3.3V is generated from the power of 5.0V generated from the DC-DC converter 614 . Thus, as compared with the case where, regardless of the fact that the DC-DC converter operates, the power from the AC adapter or the battery is used, it is possible to save more power.
Incidentally, as the regulator 615 , it is acceptable to use the DC-DC converter circuit shown in FIG. 1 . In this case, it is acceptable to connect the input and the output of the DC-DC converter 614 to either of the two input terminals of the regulator 615 . This feature simplifies the wiring work, and also may prevent the miswiring that may otherwise occur when the two wires are erroneously connected.
As mentioned above, the present invention makes possible higher efficiency of DC-DC conversion.
While the present invention has been described with reference to the particular illustrative embodiments, it is not to be restricted by those embodiments but only by the appended claims. It is to be appreciated that those skilled in the art can change or modify the embodiments without departing from the scope and sprit of the present invention.
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In a DC-DC converter circuit having a plurality of input terminals connected to a plurality of DC power supplies, and an output terminal, the DC-DC converter circuit includes a power supply selection section for selecting a DC power supply of lowest voltage on the condition that the voltage is not less than a predetermined voltage, and a step-down type of regulator section for converting the voltage of the DC power supply selected by the power supply selection section into a predetermined voltage lower than the voltage of the DC power supply selected by the power supply selection section, and outputting the converted voltage through the output terminal.
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FIELD OF THE INVENTION
The present invention relates generally to communication networks, and specifically to methods and systems for bridging in virtual private LAN services (VPLS) and other distributed bridging systems.
BACKGROUND OF THE INVENTION
Local Area Networks (LANs) connect computing systems together at the Layer 2 level. The term “Layer 2” refers to the second layer in the protocol stack defined by the well-known Open Systems Interface (OSI) model, also known as the logical link, data link, or Media Access Control (MAC) layer. Each computing system connects to a LAN through a MAC device. Multiple LANs can be connected together using MAC bridges, as set forth in the IEEE Standard for Information Technology, Telecommunications and Information Exchange between Systems, Local and Metropolitan Area Networks, Common Specifications, Part 3 : Media Access Control ( MAC ) Bridges , published as ANSI/IEEE Standard 802.1D (2004), which is incorporated herein by reference. (The 802.1D standard, as well as other IEEE standards cited herein, is available at standards.ieee.org/catalog/.) MAC bridges that implement the 802.1D standard allow MAC devices attached to physically separated LANs to appear to each other as if they were attached to a single LAN. The bridge includes two or more MAC devices that interconnect the bridge ports to respective LANs.
MAC bridges maintain a forwarding database (FDB) to map destination MAC addresses of the packets they receive to bridge ports. The bridge builds the forwarding database by means of a learning process, in which it associates the source MAC address of each incoming packet with the port on which the packet was received. When the bridge receives an incoming packet whose destination address is not found in the database, it floods (i.e., broadcasts) the packet through all its available ports, except the one through which the packet arrived. Other MAC bridges that do not recognize the destination address will further flood the packet to all the relevant ports. Through the flooding mechanism, the packet will eventually traverse all interconnected bridges at least once, and will ultimately reach its destination.
Recently, various means have been proposed and developed for transporting Layer-2 packets, such as Ethernet frames, over high-speed, high-performance Layer-3 packet networks. Methods for this purpose are described, for example, by Martini et al., in “Encapsulation Methods for Transport of Ethernet Frames Over IP/MPLS Networks” (IETF draft-ietf-pwe3-ethernet-encap-11.txt, November, 2005), which is incorporated herein by reference. This draft, as well as other Internet drafts cited herein, is available from the Internet Engineering Task Force (IETF) at www.ietf.org/internet-drafts. The draft defines mechanisms for encapsulating Ethernet traffic for transportation over Internet Protocol (IP) networks using Multi-Protocol Label Switching (MPLS) or other tunneling methods, such as Generic Routing Encapsulation (GRE), as are known in the art.
According to the model proposed by Martini et al., native Ethernet LANs are connected to the IP network by provider edge (PE) devices, which are linked one to another by tunnels through the IP network. As a result of the encapsulation of Ethernet frames and associated processing functions, the IP network emulates Ethernet trunking and switching behavior and can thus be treated as an Ethernet “Pseudo-Wire” (PW). In other words, from the point of view of native Ethernet LANs that are connected to tunnels through the IP network, each PW is a virtual Ethernet point-to-point connection, emulating a physical connection between two Ethernet ports. Martini's encapsulation method may also be used in conjunction with virtual LANs (VLANs), as defined in IEEE standard 802.1Q.
Taking this functionality a step further, a number of authors have described methods for creating a virtual private LAN service (VPLS), which links different LANs together over an IP network. Such methods are described, for example, by Kompella et al., in “Virtual Private LAN Service” (IETF draft-ietf-12vpn-vpls-bgp-06.txt, December, 2005) and by Lasserre et al., in “Virtual Private LAN Services over MPLS” (IETF draft-ietf-12vpn-vpls-1dp-08.txt, November, 2005), which are incorporated herein by reference.
A VPLS (also known as a transparent LAN service—TLS) provides bridge-like functionality between multiple sites over a large network. Users connect to the VPLS via regular Ethernet interfaces. PWs between the nodes to which the users are connected form the VPLS entity itself. Every node in a VPLS acts as a virtual bridge. A virtual bridge node has “virtual ports,” which are the endpoints of PWs that are part of the VPLS. The interfaces to which the users are actually connected are physical ports at the network edges. Both virtual and physical interfaces are treated identically from the point of view of frame forwarding and address learning. A single provider node can participate in multiple VPLS instances, each belonging to a different user. From the perspective of the end-user, the VPLS network is transparent. The user is provided with the illusion that the provider network is a single LAN domain. User nodes on different physical LANs can thus be joined together through VPLS connections to define a Layer 2 virtual private network (VPN), which appears to the users to be a single Ethernet LAN.
Link aggregation (LAG) is a technique by which a group of parallel physical links between two endpoints in a data network can be joined together into a single logical link (referred to as the “LAG group”). Traffic transmitted between the endpoints is distributed among the physical links in a manner that is transparent to the clients that send and receive the traffic. For Ethernet networks, link aggregation is defined by Clause 43 of IEEE Standard 802.3 , Carrier Sense Multiple Access with Collision Detection ( CSMA/CD ) Access Method and Physical Layer Specifications (2002 Edition), which is incorporated herein by reference. Clause 43 defines a link aggregation protocol sub-layer, which interfaces between the standard Media Access Control (MAC) layer functions of the physical links in a link aggregation group and the MAC clients that transmit and receive traffic over the aggregated links. The link aggregation sub-layer comprises a distributor function, which distributes data frames submitted by MAC clients among the physical links in the group, and a collector function, which receives frames over the aggregated links and passes them to the appropriate MAC clients.
SUMMARY OF THE INVENTION
Embodiments of the present invention provide improved methods for MAC learning and network nodes that implement such methods. These methods are useful especially in the context of nodes that are configured to serve as virtual bridges in Layer 2 virtual private networks, as well as in distributed bridge nodes of other types, particularly when multiple ports of the node are conjoined in a LAG group. The principles of the present invention, however, may be applied, mutatis mutandis, to facilitate MAC learning in any distributed MAC learning environment.
In some embodiments of the present invention, a network node comprises multiple line cards having respective ports, and is configured to operate as a virtual MAC bridge in a Layer 2 virtual private network (VPN). (One example of such a VPN is a VPLS, as described above). Each of the line cards may typically serve as both ingress and egress for data packets and has a respective MAC forwarding database (FDB) that is shared by the ingress and egress functions. When an ingress line card receives an incoming data packet over the VPN on one of its ports, it consults the FDB in order to choose the line card and port through which the packet should be forwarded based on the MAC destination address (or floods the packet through the ports in the VPN when the MAC destination address does not appear in the FDB).
The egress line card (or line cards) that is to transmit the packet onward checks the MAC source address of the data packet against the records in its own FDB. If the FDB of the transmitting line card does not contain a record associating the MAC source address with the port of the ingress line card on which the data packet was received, the transmitting line card adds the record to its FDB. At an appropriate time, the line card sends a synchronization message to the remaining line cards, informing them of the association of the MAC source address with the ingress port. Typically, all line cards send their synchronization messages at certain predefined times, although under some circumstances, a synchronization message may be sent immediately upon entry of a new association in the FDB. Upon receiving the synchronization message, the other line cards update their own MAC FDBs as appropriate.
When the forwarding destination of a packet is a link aggregation group (LAG), LAG member selection (i.e., selection of the link over which the packet is to be forwarded) is typically performed on the ingress line card. In the absence of the synchronization method described above, other members in the LAG may not receive such packets for transmission, so that the FDB of the corresponding line cards will not be updated. When these line cards receive incoming packets, the result may be constant flooding, since the FDB is incomplete. The synchronization mechanism described herein avoids this problem by updating the FDB in all line cards in the LAG group (or across the entire VPN instance) within the node. Typically, when the transmitting line card transmits the data packet via a port that belongs to a LAG group, the synchronization message sent by the line card identifies the VPN instance and the incoming port. The other line cards in the same LAG group (as well as all the other line cards serving this VPN instance) can use this information to learn the MAC address association even when these other line cards have not yet received packets from the MAC address in question.
There is therefore provided, in accordance with an embodiment of the present invention, a method for communication, including:
configuring a network node having at least first and second line cards, the line cards having respective ports, to operate as a distributed media access control (MAC) bridge in a Layer 2 network;
providing for each of the line cards a respective forwarding database (FDB) to hold records associating MAC addresses with the respective ports of the network node;
receiving a data packet on one of the ports of the network node from a MAC source address, the data packet specifying a MAC destination address on the network;
conveying the received data packet in the network node to at least the first line card for transmission to the MAC destination address;
checking the MAC source address of the data packet against the records in the FDB of the first line card; and
if the FDB of the first line card does not contain a record of an association of the MAC source address with the one of the ports on which the data packet was received, adding the record to the FDB of the first line card and sending a message to at least the second line card informing at least the second line card of the association.
In one embodiment, sending the message includes sending messages periodically at predefined times to inform at least the second line card of new associations between the MAC addresses and the respective ports.
Typically, the method includes receiving the message at the second line card, and responsively to the message, adding the record of the association to the FDB of the second line card if the record does not already exist in the FDB of the second line card. In a disclosed embodiment, the method includes marking the records in the respective FDB of each line card to distinguish a first type of the records, which are added in response to data packets transmitted via a port of the line card, from a second type of the records, which are added in response to messages received from another of the line cards. The method may further include associating a respective aging time with each of the records, refreshing the records in the FDB responsively to further packets transmitted by the line cards, and removing the records from the respective FDB if the records are not refreshed within the respective aging time.
In some embodiments, sending the message includes transmitting a synchronization packet from the first line card via a switching core of the network node to at least the second line card. In one embodiment, sending the synchronization packet includes, if the record in the FDB associates the MAC source address with a port different from the one of the ports on which the data packet was received, changing the record in the FDB of the first line card and sending a synchronization update packet to at least the second line card to indicate that the record has been changed.
In a disclosed embodiment, the first and second line cards have respective first and second ports, which are conjoined in a link aggregation (LAG), and conveying the received data packet includes transmitting the data packet to the MAC destination address via the first port, and wherein sending the message includes identifying the LAG group in the message so as to inform all the line cards that are members of the LAG group of the association. Typically, transmitting the data packet includes, when the MAC destination address does not appear in the FDB, flooding the data packet via the ports of the line cards, wherein the data packet is flooded via only a single one of the ports in the LAG group.
In some embodiments, the network node is configured to operate as multiple virtual MAC bridges in a Layer 2 virtual private network (VPN), wherein each virtual MAC bridge is configured to serve a respective VPN instance, and wherein the records associating the MAC addresses with the respective ports are maintained independently for each of the VPN instances. In a disclosed embodiment, the VPN instance is a VPLS instance among multiple VPLS instances served by the network node, and sending the message includes identifying the VPLS instance in the message so as to inform all the line cards that serve the VPLS instance.
Typically, the method includes conveying a further data packet, received from a further MAC source address, to the second line card for transmission over the network, checking the further MAC source address against the records in the FDB of the second line card, and responsively to the further data packet, adding a further record with respect to the MAC source address to the FDB of the second line card and sending a further message to inform at least the first line card of the further record.
There is also provided, in accordance with an embodiment of the present invention, a node for network communication, including:
a switching core;
a plurality of line cards configured to forward packets through the switching core so that the node operates as a virtual media access control (MAC) bridge in a Layer 2 network, the plurality of line cards including at least first and second line cards, each line card including respective ports and having a respective forwarding database (FDB) to hold records associating MAC addresses with the respective ports of the line cards,
wherein the line cards are arranged so that upon receiving a data packet on one of the ports of one of the line cards from a MAC source address, the data packet specifying a MAC destination address, the one of the line cards conveys the data packet via the switching core to at least the first line card for transmission to the MAC destination address, whereupon the first line card checks the MAC source address of the data packet against the records in the FDB of the first line card and if the MAC database of the first line card does not contain a record of an association of the MAC source address with the one of the ports on which the data packet was received, adds the record to the FDB of the first line card and sends a message to at least the second line card informing at least the second line card of the association.
The present invention will be more fully understood from the following detailed description of the embodiments thereof, taken together with the drawings in which:
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a block diagram that schematically illustrates a communication system, in accordance with an embodiment of the present invention;
FIG. 2 is a block diagram that schematically shows details of a line card in a network node, in accordance with an embodiment of the present invention; and
FIG. 3 is a flow chart that schematically illustrates a method for MAC learning, in accordance with an embodiment of the present invention.
DETAILED DESCRIPTION OF EMBODIMENTS
FIG. 1 is a block diagram that schematically illustrates a communication system 20 , in accordance with an embodiment of the present invention. A Layer 2 VPN, in the form of a VPLS, is provisioned in system 20 so as to connect MAC user terminals in different parts of the network, including exemplary terminals 22 and 24 . In the scenario shown in the figure, terminal 22 is connected to a LAN, such as an Ethernet LAN, while terminal 24 is connected to a wide area network (WAN) 28 , such as the Internet or another Layer 3 network. The VPLS, however, permits the users of terminals 22 and 24 to communicate with one another as though they were connected to the same LAN domain.
Although for the sake of simplicity, only two user terminals are shown in FIG. 1 , a given VPLS may typically connect a large number of users at various different locations. Furthermore, although the embodiments described hereinbelow relate only to a single VPLS instance, multiple, different VPLS instances may be provisioned in system 20 so as to serve different groups of users and organizations. The specific configuration of LAN 26 and WAN 28 is shown in FIG. 1 purely by way of illustration, and the principles of the present invention may be applied in substantially any network configuration that supports the provisioning of Layer 2 virtual private networks.
In the exemplary configuration shown in FIG. 1 , a network node 30 links LAN 26 and WAN 28 . Node 30 comprises multiple line cards 32 , linked by a switching core 34 . Line cards 32 have ports 36 , which connect to other nodes in LAN 26 and WAN 28 (and possibly in other networks, as well). Typically, each line card comprises multiple ports, although only a few ports are shown in FIG. 1 . In the description that follows, ports 36 are assumed to be Ethernet ports, for the sake of simplicity of explanation. Alternatively, some or all of the line cards may comprise ports of other types, and may connect to other types of networks, such as Internet Protocol (IP) networks. For example, in an alternative embodiment (not shown in the figures), WAN 28 comprises a Resilient Packet Ring (RPR) network, and some of line cards 32 thus comprise RPR interfaces. Features of a network node that may be used to connect an Ethernet network to a RPR network are described, for example, in U.S. patent application Ser. No. 10/993,882, filed Nov. 19, 2004, which is assigned to the assignee of the present patent application and whose disclosure is incorporated herein by reference. Additionally or alternatively, line cards 32 may connect to tunnels, such as Multi-Protocol Label-Switching (MPLS) tunnels, through WAN 28 via appropriate label-switched routers in the WAN.
In the embodiment shown in FIG. 1 , certain ports 36 of line cards 32 are connected by respective physical links to a switch 40 in WAN 28 , and these ports are conjoined in a LAG group 38 . Such a LAG group may serve one or more VPLS instances. From the point of view of the VPLS, the LAG group is a single logical link having an aggregated bandwidth (i.e., capacity) equal to the sum of the bandwidths of the individual physical links. At the physical level, for example, when a line card receives an incoming packet from LAN 26 that is to be transmitted to WAN 28 , the line card chooses one of the ports in the LAG group for outgoing transmission of the packet. The port is typically chosen so as to satisfy load balancing considerations. For example, the line card may apply a hash function to certain fields in the header of each incoming packet in order to choose the port through which to send that packet. The LAG group also provides built-in protection in case one of the physical links in the group fails or otherwise becomes unavailable.
FIG. 2 is a block diagram that schematically shows details of one of line cards 32 in node 30 , in accordance with an embodiment of the present invention. The line card comprises multiple ports 36 , each associated with a corresponding processing channel 50 . (Although each channel 50 is shown, for the sake of conceptual clarity, as a distinct functional block, in practice the channels may not be distinct physical devices, but may rather be implemented as threads or process carried out by a processing device that serves multiple ports.) In the example shown in FIG. 2 , port 36 of the first channel (labeled CHANNEL 1 ) is assumed to be linked to switch 40 as part of LAG group 38 , along with one or more ports on other line cards (not shown in this figure). The ports and associated channels that are linked to LAN 26 or to other nodes and media are similar in design and operation. Channel 50 comprises a packet processor 52 , which comprises an ingress path 54 and an egress path 56 . Packet processor 52 uses a MAC FDB 58 for MAC learning and forwarding functions. The FDB is shared among the processing channels on line card 32 . It is built and maintained in accordance with a method described hereinbelow with reference to FIG. 3 .
In the VPLS environment, each record in FDB 58 corresponds to a particular MAC address belonging to a particular VPLS instance. Optionally, a given VPLS instance may be partitioned into a number of virtual LANs (VLANs), which generally operate in the manner defined in the above-mentioned IEEE Standard 802.1Q. Thus, each record in the database is typically identified by a key that includes the MAC address, VPLS identifier and, optionally, the VLAN identifier or VLAN grouping identifier (known as FID). When the header parameters of an incoming packet are found to match the key, the corresponding record in the database indicates the output interface and other transmission parameters necessary for node 30 to forward the packet on to its destination. For simple Ethernet interfaces, for example, the record may simply identify the line card and port through which the packet should be transmitted. If the packet is to be forwarded via a LAG group, the record identifies the LAG group. The record also contains a “SELF” flag indicating whether the contents of the record were learned by a packet processor on this line card itself from a data packet, or whether the contents were received in a synchronization (“SYNC”) packet from another line card, as described hereinbelow.
Upon receiving an incoming packet from switch 40 , port 36 passes the packet to ingress path 54 . Packet processor 52 identifies the VPLS (typically by a lookup and classification process based on certain packet header fields), extracts the other key parameters from the incoming packet (including the MAC destination address (DA), and optionally, the VLAN identifier), and uses the key to query database 58 . If the record is found, the packet processor adds a tag to the packet indicating the egress port through which the packet should be forwarded, as well as the ingress port through which the packet was received. If the output interface indicated by the record is a LAG group, the packet processor selects one of the physical ports in the LAG group (using a hash function, for example), and tags the packet for transmission via the selected port. The packet processor then passes the tagged packet to switching core 34 , which conveys the packet to egress path 56 of the appropriate port.
When packet processor 52 receives a packet on ingress path 54 for whose key there is no a corresponding record in database 58 , however, it tags the packet for flooding. In this case, switching core 34 will pass the packet for transmission via all the ports (other than the ingress port through which the packet was received) that are used by this VPLS instance. For each LAG group serving the VPLS instance, however, the flooded packet is transmitted via only one port in the group.
Other aspects of MAC database 58 and learning processes that may be applied in building the database, particularly for nodes operating in RPR environments, are described in the above-mentioned U.S. patent application Ser. No. 10/993,882.
FIG. 3 is a flow chart that schematically illustrates a method for MAC learning that is applied by line cards 32 in node 30 , in accordance with an embodiment of the present invention. The method is carried out by packet processor 52 as it processes packets on egress path 56 , at a forwarding step 60 . Learning on egress is advantageous particularly with respect to flooded packets, since in this case multiple line cards receive the packet and are able to learn the interface association of the MAC source address (SA) and VPLS instance.
Packet processor 52 refers to FDB 58 in order to look up the key parameters (MAC SA, VPLS instance and, optionally, VLAN tag) of the packet on egress path 56 , at a key checking step 62 . If a record with this key does not yet exist in the database, the packet processor creates a new record corresponding to this key, at an entry writing step 64 . The record indicates the interface through which subsequent packets received on ingress path 54 with this key should be forwarded, based on the input interface through which the current packet was received. If the packet that generated the new record is a data packet, the packet processor marks the record with the SELF flag, to indicate that it learned the forwarding parameters from a packet forwarded through egress path 56 of its own channel 50 . Otherwise, it indicates that this is a SYNC record.
The packet processor then decides what to do with the packet that generated the new record, at a forwarding decision step 66 . If the packet is a data packet, it is forwarded to the appropriate output port, at a forwarding step 68 . Otherwise, the packet is simply discarded, at a discard step 70 .
At certain regular intervals (which should desirably be shorter than the FDB aging time), packet processor 52 sends a synchronization (“SYNC”) message to report each SELF entry that it has created in FDB 58 to the other line cards 32 in node 30 . This message typically comprises a message packet, having the same headers as the data packets forwarded by node 30 , but with a special header field indicating that it is a synchronization message. Switching core 34 conveys this SYNC packet to the other line cards in the same way as it forwards ordinary data packets. The line cards receiving the packet, however, recognize it as a synchronization message and therefore process it internally at step 64 (or step 84 , as explained hereinbelow) without forwarding it further.
In order to process a SYNC packet with a new SA at step 64 , each line card checks the VPLS instance identified in the packet. If the line card is not configured to serve this VPLS instance, it simply discards the synchronization message. Otherwise, if an entry does not exist for the key fields extracted from the SYNC packet, the line card adds the record to its own FDB. In this case, as noted above, the record has an indication that this is a SYNC entry, which was received from another line card.
Thus, for example (referring back to FIG. 1 ), when a VPLS packet from terminal 22 is forwarded by node 30 to terminal 24 via switch 40 , the packet is forwarded through only one of ports 36 in LAG group 38 . All three line cards 32 having ports in the LAG group learn the port association of the MAC address of terminal 22 , however, by means of the SYNC packets sent out by the line card through which the packet is forwarded. As a result, when terminal 24 sends a packet back to terminal 22 , the line cards associated with LAG group 38 will all be able to forward the packet to the appropriate interface for terminal 22 without flooding. Other line cards that are configured to support this VPLS instance (even if not in the same LAG group) also learn the interface association of the MAC source address from the SYNC packet.
The use of packets to distribute SYNC messages in the manner described above is advantageous in that it makes use of existing forwarding mechanisms within node 30 , without the need for an additional control channel in hardware. Alternatively, the synchronization messages may be distributed among the line cards using a dedicated control channel. Further alternatively or additionally, the line cards may distribute each synchronization message only to those other line cards that are registered as serving the VPLS instance in question. The inventors have found, however, that sending SYNC packets indiscriminately to all the line cards simplifies the operation of the MAC learning mechanism while incurring only a moderate additional communication burden. Additional savings can be made by sending multiple synchronization entries within a single packet. In this case, the processing described above is simply repeated for multiple records within the same packet.
An aging mechanism is applied in MAC database 58 in order to remove records that are no longer in effect and free space for new records. For this purpose, each record in the database has a timestamp indicating the time at which it was created or most recently updated. A record with a given key is removed from the database if a predetermined aging time elapses following the timestamp without a further packet having been received with the same key. Aging applies to both SELF and SYNC records, typically having the same aging time for both. To prevent aging of “live” records, line cards 32 refresh the timestamps of the records in the manner described below.
Referring again to FIG. 3 , when packet processor 52 determines at step 62 that FDB 58 already contains a record corresponding to the key of the packet currently in its egress path 56 , the packet processor decides on how to handle the packet at a decision step 72 . If the packet is a data packet, the packet processor checks the record in the FDB to determine whether the current packet matches the record, at a record checking step 74 . In other words, the packet processor determines whether the current packet would, if there were no record in the FDB, generate the same record as already exists (i.e., whether the existing record is a SELF record with the same port as the ingress port as the current packet). If so, the packet processor refreshes the timestamp of the record, at a refresh step 76 , and then forwards the packet to the appropriate output port at step 68 .
On the other, if the packet processor determines at step 74 that the entry in FDB 58 that matches the key of the current packet is a SYNC record, it updates the record appropriately at an update step 78 . As part of the update process, the packet processor changes the SYNC indication to SELF in the record. It may also occur at step 78 that upon looking up the key given by the packet in egress path 56 , packet processor 52 finds that the ingress port of the packet is different from the interface currently recorded for this key in database 58 . This sort of discrepancy may occur, for example, if terminal 24 moves to a different location or if the network configuration changes due to a fault or new installation. In this case, the packet processor writes the new parameters into the SELF record overwriting the old record.
The packet processor determines whether it must inform the other line cards of the change it has made in the FDB record, at an update decision step 80 . If there was no change in the interface listed in the record, the packet processor simply forwards the data packet to the appropriate output port at step 68 . If the interface has changed, however, the packet processor sends a special SYNCUPDATE packet to the other line cards, at an update step 82 . This packet is similar to the SYNC packets described above, but contains an additional “UPDATE” indication. Typically, the SYNCUPDATE packet is sent immediately upon updating the FDB record at step 76 , rather than waiting for the scheduled time for transmitting SYNC packets. The data packet that prompted the SYNCUPDATE is forwarded to the appropriate output port at step 68 .
Sending the specially-marked SYNCUPDATE packet in this manner ensures that the MAC databases of all the line cards are updated promptly when changes occur, while avoiding race conditions between SYNC packets that may already have been sent between line cards with old information. Packet processors receiving the SYNCUPDATE packet with a result that is different from their own record data, regardless of whether the record is a SYNC or SELF entry, will change the record and set the entry status to SYNC, as described hereinbelow.
Returning now to step 72 , if packet processor 52 determines that the current packet is not a data packet (i.e., it is a SYNC or SYNCUPDATE packet), it checks to determine whether the existing record in FDB 58 that corresponds to the key of the current packet is a SYNC or SELF entry, at a record checking step 84 . In the case of a SYNC entry, the packet processor updates the record if necessary, at a SYNC update step 86 . In other words, if the interface indicated in the packet is different from that indicated in the existing record, the packet processor updates the record in accordance with the packet. The packet processor refreshes the timestamp of the record whether or not the record is changed. It then discards the packet at step 70 .
If the packet processor determines at step 84 that the existing record in FDB 58 corresponding to the key of the current packet is marked as a SELF record, it checks the type of the packet at a type checking step 88 . If the current packet is a SYNC packet, the packet processor discards the packet at step 70 , since SYNC packets do not overwrite SELF entries. On the other hand, If the current packet is a SYNCUPDATE packet, the packet processor overwrites the SELF record in FDB 58 and marks the record as a SYNC entry, at a SYNC update step 90 . The packet is then discarded at step 70 .
In other embodiments of the present invention (not shown in the figures), redundant links between node 30 and other network elements, such as the parallel links between line cards 32 and switch 40 , may be used not only in LAG, but also for protection in case of failure of one of the links. Such embodiments may also benefit from the methods described above for MAC database updating and synchronization. In particular, a standby line card, when activated to provide substitute service in case of failure, can use the synchronized MAC database in order to generate and transmit dummy data packets over each new active link. Upon receiving these packets, other devices in the network learn to use the new active port. This mechanism of dummy packet transmission is described in detail in U.S. patent application Ser. No. 10/036,518, filed Jan. 7, 2002, and published as US 2003/0208618 A1, whose disclosure is incorporated herein by reference. In order to support this protection function, the FDB 58 is updated not only for VPLS instances, as described above, but also for point-to-point services that are terminated over the protected links. In this latter case, the FDB record contains the MAC address and the connection ID, rather than the VPLS ID.
Although the embodiments described above relate specifically to a certain exemplary network and equipment topology and refer to certain specific communication protocols, the principles of the present invention may similarly be applied in other types and topologies of Layer 2 virtual private networks, using different kinds of equipment and protocols. It will thus be appreciated that the embodiments described above are cited by way of example, and that the present invention is not limited to what has been particularly shown and described hereinabove. Rather, the scope of the present invention includes both combinations and subcombinations of the various features described hereinabove, as well as variations and modifications thereof which would occur to persons skilled in the art upon reading the foregoing description and which are not disclosed in the prior art.
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A method for communication includes configuring a network node having at least first and second line cards, the line cards having respective ports, to operate as a distributed media access control (MAC) bridge in a Layer 2 network. Each of the line cards has a respective forwarding database (FDB). Upon receiving a data packet on a port of the network node from a MAC source address, the data packet is conveyed to at least the first line card for transmission to the MAC destination address. The MAC source address of the data packet is checked against the records in the FDB of the first line card. If the FDB does not contain a record of an association of the MAC source address with the port on which the data packet was received, the record is added to the FDB of the first line card, which sends a message to at least the second line card informing the second line card of the association.
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FIELD OF THE INVENTION
This invention relates to a mechanical tube expander and, more particularly, to a mechanical tube expander having structure thereon for facilitating a quick adjustment in order to accommodate coil constructions of differing heights.
BACKGROUND OF THE INVENTION
Tube and fin type heat exchangers employing hairpin tubes (U tubes) or straight tubes are assembled into a mechanical tube expander by expanding the tubes into interference fit with the fins and end sheets of the heat exchanger. The hairpin tubes (U tubes) are comprised of two straight legs and a bend which is bent through an arc of 180°. The length of the two straight legs determines the finished coil height and the number of fins that are to be stacked one on top of the other and laced through holes provided in the fins. Finished coil assemblies come in a variety of heights and widths. During assembly of the coil constructions, it is oftentimes necessary to shift assembly operations from one coil construction to another. As a result, an operator must climb on a ladder to access the various adjustment features on the machine and, in some instances, the operator will need to move up and down the ladder several times at differing locations on the machine just to effect a repositioning of the various control elements on the machine. Movements of the operator up and down ladders is both time consuming and, in some instances, an occupational hazard. It is, therefore, desirable to provide a construction which will quickly accommodate a switch over from one coil assembly to another with a differing height in a most expeditious manner.
Accordingly, it is an object of this invention to provide a mechanical tube expander having structure thereon for facilitating an adjustment of the expander to accommodate differing coil heights without necessitating the operator moving up and down ladders to access the various adjustment features on the expander.
It is a further object of the invention to provide a mechanical tube expander, as aforesaid, which has a control panel having controls thereon enabling the operator to set up the machine for differing coil heights while remaining at the control panel.
It is a further object of the invention to provide a mechanical tube expander, as aforesaid, which is easy to operate and which eliminates the hazards of the working environment associated with a set up operation for the mechanical tube expander.
SUMMARY OF THE INVENTION
The objects and purposes of the invention are met by providing a mechanical tube expander for expanding hairpin tubes or straight tubes into interlocked relationship with fins, which expander includes a frame, a receiver mounted on the frame and adapted to support the bent portions of the hairpin tubes. An assembly of fins is loosely stacked on the hairpin tubes and supported on the receiver. A pressure plate carrying a plurality of expander rods which are aligned with the hairpin tubes, which expander rods include tube-expanding bullets at one end thereof, is driven toward and away from the assembly of fins in order to effect a driving of the bullets into the tubes to expand them and to effect an interlocked relationship of the fins to the exterior surface of the tubes as well as retracting the bullets from within the tubes. A stripper plate having a plurality of guide openings therethrough through which extend the expander rods is provided for engaging the assembly of fins on an end thereof remote from the receiver, the stripper plate being moveable relative to the frame toward and away from the receiver by the drive mechanism for the pressure plate. A pair of laterally spaced internally threaded nuts are provided on an expander plate and elongated pressure screws are threadedly received in each of the threaded nuts. A drive mechanism is provided for simultaneously rotating each of the screws relative to the nuts to, therefore, cause the screws to be adjusted vertically relative to a bolster plate on which the receiver is mounted. A pair of fluid cylinders are provided on opposite sides of the frame, which fluid cylinders each have a main chamber and a piston dividing the main chamber into first and second chambers. A piston rod is secured to each piston. A source of pressurized compressible fluid and a connection therefor is provided for facilitating a connection of each of the second chambers to the fluid source and a continuous urging of the pistons toward one end of the main chamber. First and second block members are slidably mounted on each of the piston rods for movement longitudinally thereof, the first block member being also mounted on and moveable with the stripper plate and is oriented on a side of the stripper plate remote from the receiver. Additional support means are provided for suspending the second block member from the stripper plate and providing a limit distance that each second block member is suspended along the piston rods away from the first block members and the stripper plate. Releasable clamping structure is provided on each of the first and second block members for fixedly clamping the first and second block members to the piston rod. Control means are provided for effecting a complete cycle of operation to cause the hairpin tubes to be expanded into interlocked relationship with the fins as well as facilitating an initial setup of the mechanical tube expander to accommodate a desired height of an assembly of fins.
BRIEF DESCRIPTION OF THE DRAWINGS
Other objects and purposes of this invention will be apparent to persons acquainted with apparatus of this general type upon reading the following specification and inspecting the accompanying drawings, in which:
FIG. 1 is a front view of a conventional mechanical tube expander in a first position of operation;
FIG. 2 is a front view of a mechanical tube expander illustrated in FIG. 1, but moved to a second position of operation thereof;
FIG. 3 is a fragmentary enlargement of an assembly of fins mounted on a hairpin tube supported on a receiver;
FIG. 4 is an isometric view of a mechanical tube expander embodying the invention;
FIG. 5 is a front view of the mechanical expander illustrate in FIG. 4;
FIG. 6 is a front view of the mechanical expander illustrated in FIG. 5, but with the component parts thereof in a position whereat the final coil height is set;
FIGS. 7A-7F illustrate a sequence of movements of component parts of the mechanical tube expander during a coil assembly task; and
FIG. 8 is a schematic illustration of a control panel for controlling the operative sequences of the mechanical tube expander embodying the invention.
Certain terminology will be used in the following description for convenience in reference only and will not be limiting. The words "up", "down", "right" and "left" will designate directions in the drawings to which reference is made. The words "in" and "out" will refer to directions toward and away from, respectively, the geometric center of the device and designated parts thereof. Such terminology will include derivatives and words of similar import.
DESCRIPTION OF KNOWN PRIOR ART
FIGS. 1-3 of this application illustrates known prior art relating to a mechanical tube expander. Devices of this type can be oriented both vertically and horizontally. The type of construction illustrated in FIGS. 1-3 relate to a vertically oriented device wherein the overall height is approximately that of a two story building. In order to accommodate coil constructions of differing heights, such as will occur when a changeover is to take place from one coil construction to another coil construction, ladders employed by the setup people are required in order to make the appropriate adjustments to the machine. In order to better understand the nature of the adjustments that need to be made in the prior art machine, it will be necessary to describe the prior art machine and such description is set forth in the next preceding paragraphs.
Referring to FIG. 1, there is illustrated a vertical tube expander 10 comprising a frame 12 (See FIG. 4) on which a hairpin supporting receiver 11 is mounted. The tubes T and the fins F to be interlocked with the tubes (see FIG. 3) are disposed in a fixture 13. The tubes T are oriented vertically and the fins F are loosely stacked thereon. The hairpin supporting receiver 11 supports the reversely curved (hairpin bent) lower ends of the tubes. The receiver 11 is supported on a receiver support plate 14 mounted on [the frame 12] a bolster plate 21.
A plurality of expander rods 16 corresponding in number and arrangement to the number and arrangement of tubes T, is provided for expanding the tubes. At their lower ends, the expander rods carry expander bullets 17 (see FIG. 3) which are effective to expand the tubes into interlocked engagement with the fins when the expander rods are moved vertically downwardly through the tubes. The expander rods 16 extend through plural, vertically movable, guide plates 18, suspended from a pressure plate 22 by not illustrated tie rods, so that the lower ends of the expander rods will remain vertically aligned with the tubes T. Vertical guide rods 19 are provided for guiding the reciprocating. movement of the reciprocal parts of the mechanical tube expander such as the pressure plate 22 and the guide plates 18. The vertical guide rods 19 are mounted on the sturdily constructed bolster plate 21 part of the frame 12. The receiver support plate 14 is mounted on the upper surface of the bolster plate 21. The pressure plate 22 is provided for supporting the expander rods 16 for vertical reciprocating movement. The pressure plate 22 is vertically slidably guided by the rods 19. The pressure plate 22 is connected to a ram piston rod 23 of a piston and cylinder assembly schematically indicated by the reference character 24 so that the pressure plate 22 can be driven toward and away from the receiver 11.
A final expander plate 26 is vertically slidably movable on the guide rods 19 and, like the guide plates 18, are suspended from the pressure plate 22, but by tie rods 20. The expander plate has not illustrated structure thereon for flaring the upwardly facing open ends of the tubes T, particularly during the final stages of the stroke from the piston and cylinder assembly 24. The expander plate 26 has on laterally opposite sides thereof projections 27. A pair of internally threaded nuts 28 are mounted on the upper surface of the expander plate 26 and threadedly receive therein an elongated screw 29. Each screw 29 has an elongated rod 31 extending upwardly therefrom through openings provided in the guide plates 18 and the pressure plate 22. A motorized drive arrangement (not illustrated) is provided for driving the rods 31 for rotation and, consequently, the screws 29 for rotation within the stationary nuts 28. Both of the screws 29 are oriented so that the upper ends 32 are coplanar and remain coplanar as the motorized drive means alters the vertical position thereof.
A stripper plate 36 is slidably mounted on the guide rods 19 and are suspended by stripper bolts 34 (FIG. 2) a predetermined distance from the expander plate 26. The stripper plate 36 has a plurality of stripper posts 37 projecting downwardly therefrom, only one of which is illustrated in FIGS. 1 and 2. The stripper posts 37 are intended to engage the upper fin F of an assembly of fins AF for the purpose of facilitating a removal of the bullets 17 from within the tubes T following an expansion of the tubes T into interlocking relation with the fins F.
A pair of brackets 38 are provided on opposite lateral sides of the stripper plate 36. Each bracket 38 includes a guide block 39 extending horizontally outwardly in a plane generally parallel to the plane of the stripper plate 36. The brackets 38 each include a downwardly extending arm 41 to which is pivotally secured a two arm latch mechanism 42. Each latch mechanism 42 includes an elongated lever arm 43 extending away from the pivot axle 44 on one side thereof. The outermost end of the lever arm 43 has a projection 46 thereon adapted to operatively engage and disengage from the projection 27 on the expander plate 26. A spring mechanism (not illustrated) is provided for continually urging the left lever arm 43, as viewed in FIG. 1, clockwise about the pivot axle 44 therefor and the right lever arm 43 counterclockwise about the pivot axle 44 therefor. The latch mechanism 42 includes a latch projection 47, the purpose of which will be set forth in more detail below.
A holding block 48 is slidably movably oriented on each of the guide rods 19 and is positioned between the bolster plate 21 and the underside of the stripper plate 36. Each holding block includes a manually operable knob 49 for facilitating a manipulation of a hook-like member 64 into engagement with a pin 66. In order to permanently affix the holding block 48 to the guide rod 19, a plurality of screws 51 are provided, it being recognized that the holding block 48 is somewhat C-shaped and encircles the guide rod 19 with the free ends of the C-shaped construction being connected together by the aforementioned screws 51. A projection 52 is provided on the holding block 48 and is adapted to operatively engage the latch projection 47 on the latch mechanism 42.
A pair of piston and cylinder assemblies 53 are mounted on laterally opposite ends of the bolster plate 21 and are oriented so that each piston rod 54 thereof extends vertically upwardly parallel to the guide rods 19. Each piston rod 54 extends through a guide opening 56 in the guide block 39. A pre-sizer actuator block 57, the position of which can be vertically adjusted along the length of the piston rod 54 by loosening and tightening a clamp actuated by a lever arm 58, is provided on each of the piston rods 54 at a location that is beneath the guide blocks 39.
A source P of pressurized fluid, here air, is connected via pipes 59 or the like to the bottom end of the cylinder part of each of the piston and cylinder assemblies 53 to continually urge the pistons therein and associated piston rods 54 vertically upwardly. A pipe 61 is connected to the upper end of the cylinder part of each of the piston and cylinder assemblies 53 in order to connect the upper end of the piston and cylinder assemblies 53 to the atmosphere. A valve V is provided in the pipe 59 to bleed off to the atmosphere any excess pressure that may develop inside the piston and cylinder assembly 53 when the pistons therein are urged toward the bottom end of the piston and cylinder assemblies 53.
In order to adjust the mechanical tube expander 10 to accommodate coil constructions of differing heights at the point in time where a changeover from one coil construction to another one is to occur, the first thing that the operator needs to do is to lower the stripper plate 36 until the downwardly facing surface 62 of the guide structure therefor around the guide rods 19 engages the upper surface 63 of the holding blocks 48 as shown in FIG. 2. Thereafter, the operator will need to climb up on a ladder (for tall coil heights--a ladder would probably not be required for short coil heights) and secure by means of a hook 64 and knob 49 (FIG. 2) pivotally secured to the holding block 48, the holding block 48 to a pin 66 provided on the guide structure for the stripper plate 36. This action will be required on both lateral sides of the machine and, therefore, the operator will need to move up and down ladders, if necessary, at two separate locations in order to accomplish this task. Thereafter, the operator will need to loosen each of the screws 51 to effect an unclamping of the holding block 48 from its fixably clamped relation with the guide rod 19. Following an unclamping of the holding blocks 48, the piston and cylinder assembly 24 can then be actuated in order to cause the pressure plate 22 to move either upwardly or downwardly to a desired location to orient the upper surface 63 of each of the holding blocks 48 to a finished coil height for the next coil structure to be assembled. Prior to this step, however, it will be necessary for the pre-sizer actuator blocks 57 to be lowered out of the way of movement of the brackets 38 provided on the stripper plate 36. Assuming that the holding blocks 48 have been moved to the proper finished coil height location, it will be necessary for the operator to again climb up on a ladder and retighten the screws 51 to fixedly orient the holding block 48 to the associated guide rod 19 (meaning that the operator will need to move up and down ladders at two separate locations). The hooks 64 can then be removed [by loosening knob 49] from engagement with the pins 66 by loosening knob 49 to allow the pressure plate as well as the expander plates and all plates 18 oriented thereabove to move vertically away from the newly positioned holding blocks 48. Since no coil is now present in the machine during an adjustment, there is no force being applied to the stripper plate.
In situations where a totally new coil construction is to be assembled, the aforementioned adjustment procedure can be quite cumbersome due to the fact that multiple repositionings of the holding block 48 will be necessary by trial and error until the final position of the upper surfaces 63 of the holding blocks 48 is appropriately determined. In other words, the operator will need to move up and down ladders at two separate locations a multiple number of times and effect tightenings and loosenings of screws using, in this particular embodiment, an allen wrench. In other words, a considerable amount of time is spent effecting a readjustment of the machine. During this time of adjusting the position of the holding blocks 48, the pre-sizer actuator blocks 57 are also moved so that the upper surfaces 67 thereof are oriented a certain specified distance above the upper surfaces 63 of the adjusted position of the holding blocks 48, thus, further movement of the operator up and down ladders.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The mechanical tube expander 10 shown in FIGS. 1 and 2 is similar in many respects to a modified mechanical tube expander 10A illustrated in FIG. 4. Yet, the differences are subtle and important. The mechanical tube expander illustrated in FIGS. 4-6 includes an alternate holding block and pre-sizer actuator block construction which makes it wholly unnecessary to utilize the afore-described complicated latch mechanism 42, holding blocks 48 and manually manipulatable pre-sizer actuator blocks 57.
Referring now to FIG. 4, there is illustrated a vertical modified tube expander 10A. The reference characters for the components that are the same as the components in the embodiment of FIGS. 1-2 will remain the same.
The expander comprises a frame 12 on which a hairpin supporting receiver 11 is mounted. The tubes T and the fins F to be interlocked with the tubes are disposed in a fixture 13. The tubes T are oriented vertically and the fins F are loosely stacked thereon. The hairpin supporting receiver 11 supports the reversely curved (hairpin bent) lower ends of the tubes. The receiver 11 is supported on a receiver support plate 14 mounted on the bolster plate 21.
A plurality of expander rods 16 corresponding in number and arrangement to the number and arrangement of tubes T, is provided for expanding the tubes. At their lower ends, the expander rods carry expander bullets 17 (see FIG. 3) which are effective to expand the tubes into interlocked engagement with the fins when the expander rods are moved vertically downwardly through the tubes. The expander rods 16 extend through plural, vertically movable, guide plates 18, suspended from a pressure plate 22 by not illustrated tie rods, so that the lower ends of the expander rods will remain vertically aligned with the tubes T. Vertical guide rods 19 are provided for guiding the reciprocating movement of the reciprocal parts of the mechanical tube expander such as the pressure plate 22 and the guide plates 18 expander plate 26 and stripper plate 36. The vertical guide rods 19 are mounted on a sturdily constructed bolster plate 21 part of the frame 12. The receiver support plate 14 is mounted on the upper surface of the bolster plate 21. The pressure plate 22 is provided for supporting the expander rods 16 for vertical reciprocating movement. The pressure plate 22 is vertically slidably guided by the rods 19. The pressure plate 22 is connected to a ram piston rod 23 of a piston and cylinder assembly schematically indicated by the reference character 24 so that the pressure plate 22 can be driven toward and away from the receiver 11.
An expander plate 26 is vertically slidably movable on the guide rods 19 and, like the guide plates 18, suspended from the pressure plate 22, but by tie rods 20. The expander plate has not illustrated structure thereon for flaring the upwardly facing open ends of the tubes T, particularly during the final stages of the stroke from the piston and cylinder assembly 24. A pair of internally threaded nuts 28 are mounted on the upper surface of the expander plate 26 and threadedly receive therein an elongated screw 29. Each screw 29 has an elongated rod 31 extending upwardly therefrom through openings provided in the guide plates 18 and the pressure plate 22. A motorized drive arrangement (not illustrated) is provided for driving the rods 31 for rotation and, consequently, the screws 29 for rotation within the stationary nuts 28. Both of the screws 29 are oriented so that the upper ends 32 are coplanar and remain coplanar as the motorized drive means alters the vertical position thereof.
A stripper plate 36 is slidably mounted on the guide rods 19 and suspended by stripper bolts 34 (FIG. 2) a predetermined distance from the expander plate 26. The stripper has a plurality of stripper posts 37 projecting downwardly therefrom, only one of which is illustrated in FIGS. 1 and 2. The stripper posts 37 are intended to engage the upper fin F of an assembly of fins AF for the purpose of facilitating a removal of the bullets 17 from within the tubes T following an expansion of the tubes T into interlocking relation with the fins F.
In this particular embodiment, it will be noted that the projections 27 on opposite lateral sides of the expander plate 26 are missing. Further, the brackets on opposite lateral sides of the stripper plate 36 are also missing.
The piston and cylinder assemblies 53 described in FIGS. 1 and 2 above have been replaced with different piston and cylinder assemblies 71, each having a piston moveable therein, to which piston is secured a piston rod 72 extending vertically generally parallel to the guide rods 19. A source P of compressed air is connected through piping or the like 73 to the cylinder port oriented beneath the pistons in each of the piston and cylinder assemblies 71. A valve V 1 is provided for bleeding off any excessive pressure that may build up inside the piston and cylinder assembly 71 as the pistons therein are urged toward the bottom of the respective stroke for the pistons. The upper end of the cylinder port above the pistons in each of the piston and cylinder assemblies 71 is, in this particular embodiment, connected through piping 74 to a valve V 2 which in turn is connected through piping 76 to a reservoir R of oil or the like. As the pistons in each of the piston and cylinder assemblies 71 is moved downwardly, oil will be drawn through the valve V 2 into the upper end of the piston and cylinder assemblies 71 as air is urged out of the lower end of the piston and cylinder assemblies through the relief valve V 1 to the atmosphere while retaining in the lower end of the piston and cylinder assemblies the requisite pressure determined by the setting on the relief valve V 1 .
A combination of pre-size clamp 77 and strip clamp 78 are mounted on opposite lateral sides of the stripper plate 36 and are moveable relative to the piston rods 72. The strip clamp 78 is fixedly secured to the upper surface of a lateral extension 79 of the stripper plate 36. The strip clamp 78 encircles the piston rod 72 and has a hydraulic structure therewithin, schematically shown in broken lines at 68 in FIGS. 5 and 6, for constricting around and effecting a clamp of the strip clamp 78 to the piston rod 72. Suspended from the lateral extension 79 and the strip clamp 78 is a pre-size clamp 77 identical in construction to the strip clamp 78, it, too, having a hydraulically operated structure 68 therewithin constricting around the piston rod 72 to fixedly clamp the pre-size clamp 77 to the piston rod 72. In this particular embodiment, a post 81 is secured to the upper end of the pre-size clamp 77 and projects through an opening provided in the lateral extension 79 of the stripper plate 36 and through the mounting plate 82 for the strip clamp 78 to an enlarged cap retained by a not illustrated screw at the upper end of the post 81. The pre-size clamp 77 is capable of moving relative to the strip clamp 78 a prescribed distance X 1 illustrated in FIG. 7A. In one exemplary embodiment, the dimension X 1 is equal to 9.5 inches.
As shown in FIG. 4, a control panel CP is provided which has a plurality of control buttons B thereon and two small screens S for displaying numerical data indicating the position of the screws 29 relative to the nuts 28. The control panel CP includes all of the requisite control buttons B for effecting a coil height setup operation for the mechanical tube expander 10A without necessitating the operator leaving the control panel. For example, FIG. 8 illustrates a highly simplified schematic electrical control diagram enabling a manual operation of the control buttons B to effect a coil height setup of the mechanical tube expander as well as activating an automated operation control system to allow coil assembly, tube expansion, to occur in an automated manner following the setup operation.
Referring to FIG. 8, electrical lines 91 and 92 are provided and electrical power is supplied thereto in a conventional manner. An ON-OFF switch 93 is connected in series with the line 91 to control the application of electrical power to the circuit components. In order to, for example, activate the pre-size clamp 77, switch 94 is closed to activate a control relay CR1 and, simultaneously therewith, the clamp. A relay contact CR1-1 of the control relay CR1 changes state from normally open to closed to lock in the activation of the control relay CR1 and the clamp. To deactivate the pre-size clamp, a STOP switch 96 is activated. Similarly, a switch 97 is closed to activate the stripper clamp 78. This causes an activation of the control relay CR2 so that a contact thereof, namely, contact CR2-1 to change state from a normally open condition to a closed condition to result in a locked in activation of not only the control relay CR2 but also the stripper clamp 78. To deactivate the stripper clamp, the STOP switch 97A is activated.
The ram drive cylinder 24 is controlled by two control relays CR3 and CR4. For example, a switch 98 is capable of moving back and forth between two sets of contacts 99 and 101. If it is desired to move the ram up, the switch 98 is moved to contact the set of contacts 99 to effect an activation of the control relay CR3. Activation of the control relay CR3 causes the contacts thereof CR3-1 and CR3-2 to become closed and the ram will continue to move upwardly until contact with a limit switch LS-1 which will become open to stop the upward movement of the ram. Stopping at intermediate points can be accomplished by activating the STOP switch 102. When it is desired to move the ram down, the switch 98 can be moved to a set of contacts 101 to accomplish that objective as well. The limit switch LS-2 and the STOP switch 102A serve the purpose of limiting the downward movement of the ram.
When it is desired to move the screws 29 to differing positions, a switch 103 is moveable to select one of the sets of contacts 104 and 106. The limit switches LS-3 and LS-4 and the stop switches 105 and 105A serve to limit the upward and downward movement of the screws, respectively. The control relays CR5 and CR6 operate in the same manner as has been described above with respect to the control relays CR1-CR4 and the sets of contacts thereon, namely, CR5-1, CR5-2, CR6-1 and CR6-2, respectively, operate also in the same manner.
When the set of contacts, for example, CR3-2 become closed, the ram drive cylinder will be driven upwardly. If it is desired to jog the ram drive cylinder for movement in small increments, a JOG-UP switch 107 can be activated. Similarly, a JOG-DN switch 108 can be activated to jog the drive cylinder through incremental small steps in a downward direction. In a similar fashion, the screw motor M can be driven in a clockwise direction, namely, causing the screws to move in an upward direction when the contact CR5-2 of the control relay CR5 become closed. Similarly, a JOG-UP switch 109 can be activated to increment the screw in a clockwise direction. A JOG-DN switch 111 can be used to effect the reverse rotation of the screw, namely, a counter clockwise direction causing the screw to be moved intermittently in a downward direction. The position display for the screw is displayed on a screen S 1 through conventional transducer circuitry. Similarly, the position of the stripper plate to which the ram drive cylinder is connected is displayed on a screen S 2 through conventional transducer circuitry.
An automated operation control system is also provided and can be activated by moving a switch 112 between a MANUAL and an AUTO set of contacts. Similarly, the automated operation control system can be activated by opening the switch 113.
The valve V 2 is a normally open valve which, when activated, becomes closed to prevent the flow of fluid therethrough. If desired, a switch can be provided for manually controlling the valve V 2 . However, in this particular embodiment, the automated operation control system effects a timely control of the valve V 2 to cause the valve V 2 to become closed when the ram drive cylinder reaches its bottom most stroke and the limit switch LS-2 becomes open. The valve V 2 becomes opened again when the ram has been raised to a predetermined height relative to the receiver 11.
Broken lines are shown in FIG. 8 and extend between the automated operation control system and the aforementioned valve V 2 and the control relays CR2, CR3 and CR4. Proper sequencing of the control relays CR2, CR3 and CR4 will enable an assembly of fins to be properly assembled into a finished coil construction.
In order to effect a setup operation of the mechanical tube expander illustrated in FIGS. 4-6, the press drive cylinder, namely, the piston and cylinder assembly 24 is retracted so that the pressure plate 22 is first moved to the uppermost limit position. This is caused by a moving of the selector switch 98 to the upper contact to activate a control relay CR3 which becomes locked on by the closing of a normally open relay contact CR3-1 on the control relay CR3. Similarly, normally open contacts CR3-2 on the control relay CR3 will also close thereby activating the press drive cylinder 24 to retract the ram until the normally closed limit switch LS-1 is opened thereby deactivating the control relay CR3 and causing the contacts thereof CR3-1 and CR3-2 to open. Thereafter, the screws 29 can be rotated by activating a drive motor 86 (FIG. 4) therefor and, through an appropriate transmission mechanism 87, causing both screws 29 to synchronously rotate and be moved upwardly or downwardly relative to the nuts 28 at the same rate thereby keeping the upper ends 32 of the screws in a coplanar arrangement. An encoder 88 is provided to monitor the number of rotations of the screws 29 and to thereby indicate the distance that the lower end of the screw 29 is from the expander plate 26. The screws will be adjusted either up or down until the correct screw position is displayed on the screen S 1 . Assume, for the moment, that the dimension for the finished coil is known to be 50 inches. Thus, the display on the screen S 1 will be adjusted to 50.000 inches. Careful play with the switches, including the selector switch 103 and the JOG-UP switch 109 and the JOG-DN switch 111 will enable an accurate positioning of the screw until the Y dimension is at the appropriate distance for a 50 inch finished coil (See FIG. 5) and the display in S 1 is at the desired 50.000 inches. Thereafter, the ram 23 can be driven downwardly through an appropriate activation of the selector switch 98 as well as intermittent operation of the ram JOG-UP and ram JOG-DN switches 107 and 108, respectively to position the stripper plate at the coil pre-size location which, for a 50.000 inch finished coil height and assuming about a 3% shrink, is 51.546 inches in this particular embodiment. A transducer (not shown) will provide at all times the position X 2 -X 1 , or Z or pre-size height so that the dimension Z is properly displayed on the screen S 2 . The transducer has a 9.500 offset, hence when the screen S 2 displays 51.546, then X 2 (FIG. 7A) would be 61.046. This is when the pre-size clamp 77 should be locked. Thus when the ram is lowered from the FIG. 7A position to the FIG. 7B position or 9.500, then Z=51.546, namely, the pre-size height. Screen S 2 is only used for setting up in FIG. 7A. After the pre-size clamps are locked, the screen data is unimportant until the next height change X 2 -X 1 =Z=SH. Since the dimension X 1 is 9.500 inches, the pre-size clamp 77 will always be 9.500 inches below the stripper plate 36, at which time the pre-size clamp 77 can be activated and the letter "C" appearing in FIG. 7A designates that the clamp 77 is in the "clamped" condition. The screen S 2 display is not, as stated above, important from here on. The stripper clamp 78 remains unclamped and the "U" symbol designates such in FIG. 7A. The aforementioned adjustments were all made without the operator needing to leave the control panel CP. Once an assembly of fins has been placed on to the receiver 11, the operator can thereafter activate the automated control system and a coil assembly operation will take place automatically with the pre-size clamp 77 and stripper clamp 78 operating in the manner illustrated in FIGS. 7A-7F. If, on the other hand, the Z and FC dimensions in FIGS. 7B and 7C or the Z dimension in FIG. 5 or the FC dimension in FIG. 6 needs to be determined by trial and error to accommodate a coil of a different size, such manipulation of the screws and pre-size clamp 77 can be easily and quickly accomplished.
The automated operation control system will first bring the stripper plate 36 from the position illustrated in FIG. 7A to the position illustrated in FIG. 7B wherein the stripper plate 36 rests on the upper surface of the pre-size clamp 77. Dimension Z is the pre-size size dimension for a 50 inch coil and is 51.546 inches. It is to be noted that dimension X 1 substrated from dimension X 2 will equal dimension Z. The press drive cylinder 24 will continue to drive the piston rod 23 downwardly to force the bullets 17 through the tubes T to cause the fins to become interlocked with the tubes T. During this process, shrinkage of the assembly of fins and tubes from a starting height SH or pre-size height will occur, as depicted in FIG. 5. As the ram drive cylinder 24 continues urging the pressure plate 22 downwardly, the pressure plate 22 contacts the surfaces 32 to cause the expander plate 26 to push the stripper plate 36, which causes the lateral extension 79 to force the pre-size clamp 77 down. Since the pre-size clamp 77 is clamped to the piston rod 72, the piston rod 72 is also urged downwardly. The pre-size clamps 77 clamped to the piston rods 72 will be pushed downwardly to cause the piston rods 72 to be retracted within the piston and cylinder assemblies 71 until the finished coil size FC is reached as illustrated in FIG. 7C and as determined by the bottom end of each screw 29 nearing the upper surface of the bolster plate 21. It is preferable that the limit switch LS-2 open when the bottom end of the screws 29 are spaced about 1 mm from the bolster plate 21. This can be accomplished, for example, by the utilization of a proximity switch on the bolster plate 21, serving the limit switch LS-2, which proximity switch would detect the presence of the lower end of the screws 29 to halt further downward movement of the ram 23. Other suitable locations of the limit switch LS-2 are also possible. Thereafter, the automated control system effects an activating of the stripper clamp control relay CR2 to activate the stripper clamp 78 as schematically illustrated by the C in FIG. 7D and close the valve V 2 . While the stripper clamp and pre-size clamp 77 both remain in the clamped condition illustrated in FIG. 7D, the press drive cylinder 24 will retract the ram or piston rod 23 as well as the expander rods 16 and bullets 17 thereon from the tubes T until the bullets 17 are positioned adjacent the upper open ends of the tubes T. All during a retraction of the bullets 17 from the tubes T, the closed valve V 2 prevents the escape of oil from the upper end of the piston and cylinder assembly 71 to fixedly position the piston rods 72 in their lowered position illustrated in FIGS. 7C-7E. As shown in FIG. 7E, the stripper clamp 78 is unclamped and the press drive cylinder 24 is allowed to continue to retract the ram 23 to eventually cause the stripper plate 36 to rise from the position illustrated in FIG. 7E. Shortly after the stripper plate rises off of the pre-size clamps 77, the valve V 2 is opened to allow the pressurized air from the source P to push the pistons upwardly in the piston and cylinder assembly 71 to drive the oil back into the reservoir R through the now opened valve V 2 . The ram cylinder continues to retract to allow the pressure plate 22 to lift the expander plate 26 and stripper plate 36. The limit switch LS-1 will open to halt further upward movement of the ram 23 after sufficient space has been provided to allow for removal of an assembled coil and inserting an assembly of fins to be finished. As a result of this last mentioned step, the stripper plate 36 and the pre-size clamp as well as the stripper clamp are oriented to the FIG. 7F position at which time the mechanical tube expander is ready for the next cycle of operation.
It is conceivable, and within the purview of a person skilled in the art of machine control, that an operator could know in advance from experience the finished coil height, the pre-size coil dimension (SH) and the amount of shrink for a particular coil model. All that the operator would need to do is to input the coil model number into a control module on the control panel (not illustrated) preprogrammed with the above information so as to enable the control module to set the parameters on the expander automatically.
Although a particular preferred embodiment of the invention has been disclosed in detail for illustrative purposes, it will be recognized that variations or modifications of the disclosed apparatus, including the rearrangement of parts, lie within the scope of the present invention.
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A mechanical tube expander having a construction which facilitates a machine setup prior to coil assembly without necessitating the machine operator to leave a control panel, this being due to all setup and locking features being accomplished from the control panel. Thus, an operator climbing on ladders to various and remote locations on the machine are not necessary. This feature is accomplished by orienting a pre-size clamp and a strip clamp on opposite sides of the stripper plate and tracking the position of the stripper plate relative to the receiver in order to enable the pre-size clamp to be correctly positioned and clamped to a piston rod driven upwardly by pressurized air. Any retraction of the piston rod will cause oil to be drawn into the upper end of the piston and cylinder assemblies so that at the bottommost stroke of the mechanical tube expander, a valve will be activated to block outflow of oil at the same time that the stripper clamp is clamped to allow bullets to be removed from the tubes in an assembly of fins, after the withdrawal of such bullets the stripper clamp is unclamped to allow the mechanical tube expander to return to a predetermined position to enable another operative sequence to take place.
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RELATED APPLICATIONS
[0001] This application claims under 35 U.S.C. §120 the benefit of the filing date of prior U.S. application Ser. No. 08/929,752, now pending, which in turn claims under 35 U.S.C. §120 the benefit of the filing date of prior U.S. application Ser. No. 08/661,836, now abandoned, which in turn claims under 35 U.S.C. §120 the benefit of the filing date of U.S. application Ser. No. 08/100,037, now abandoned.
FIELD OF THE INVENTION
[0002] This invention relates to a communication system, and more particularly to a communications system that is operative at the sub-orbital level yet well above any system which is connected to the ground.
BACKGROUND OF THE INVENTION
[0003] Long distance telecommunications systems currently use space satellite transmission or ground based systems that rely upon towers, tall buildings, tethered balloons and the like.
[0004] Satellite systems have been used for many years with a high degree of reliability. They are particularly advantageous since due to their altitude one satellite can send and receive signals from an area encompassing hundreds of thousands of square miles. However, satellites are expensive to manufacture and are expensive to launch and place in position. Further, because of the costs associated with their manufacture and launch, and the great difficulty in servicing them, extraordinary care must be taken to assure their reliability. Notwithstanding this, when a satellite fails, as assuredly they all—must do, either electronically, or by degradation of orbit, substantial expense is incurred in replacing it and the equipment it carries.
[0005] Ground based systems do not have the high costs that are associated with satellite systems. However, because they are low, a particular relay station may only be able to send and receive signals over a few hundred square miles. Thus, to cover a large area, many such relay stations must be provided. Further, ground based systems suffer from line-of-sight problems in that mountains, tall trees, tall buildings and the like interfere with the propagation of telecommunications signals. Still further, it may not be possible to install a telecommunications relay station at a particular site where one is needed due to geographic or political factors, or merely because of the inability to obtain permission from a land owner or government.
[0006] To some extent these problems are alleviated by using tethered balloons. However, tethered balloons are subject to the atmospheric conditions that exist at lower altitudes and are likely to be damaged as they are subject to weather conditions thereby requiring frequent replacement. Also, if they are flown at altitudes that enable them to relay telecommunications signals over a large enough area to make them economically feasible, the tethers become hazardous to aircraft.
[0007] It would be advantageous to provide a stable, long duration, telecommunications system which is based on a sub-orbital, high altitude device which has the ability to receive telecommunication signals from a ground station and relay them to another similar device or to a further ground station.
[0008] If the relay stations were made of high altitude, long duration lighter than air devices whose location could be controlled so as to be over a particular location on the earth, a means will have been created for providing relatively low cost telecommunication service such as a telephone service for remote areas without incurring the expense associated with satellite based communication systems, and without the disadvantages of a ground system or a tethered balloon system.
SUMMARY OF THE INVENTION
[0009] Accordingly, with the foregoing in mind the invention relates generally to a telecommunications system that comprises at least two ground stations. Each of the ground stations includes means for sending and means for receiving telecommunication signals. At least one relay station is provided. The relay station includes means for receiving and sending telecommunication signals from and to the ground stations and from and to other relay stations.
[0010] The relay stations are at an altitude of about 15 to 25 miles (i.e., within a portion of the stratosphere) and, thus, are capable of transmitting signals to a point on the earth directly below a relay station with a transmission time of about 80 μsec. Means are provided for controlling the lateral movement of the relay stations so that once a pre-determined altitude is reached, a predetermined location of each of the relay stations can be achieved and maintained.
BRIEF DESCRIPTION OF THE DRAWINGS
[0011] The invention can be further understood by referring to the accompanying drawing of a presently preferred form thereof, and wherein
[0012] [0012]FIG. 1 is a schematic showing a communications system constructed in accordance with a presently preferred form of the invention.
[0013] [0013]FIG. 2 is a side elevation view of one of the relay stations comprising the invention.
[0014] [0014]FIG. 3 is a view of a portion of FIG. 2 showing a propulsion system.
[0015] [0015]FIG. 4 is a view of a portion of FIG. 2 showing another form of propulsion system.
[0016] [0016]FIG. 5 is a view of a portion of a relay station.
[0017] [0017]FIG. 6 is a view of a second embodiment of the portion of the relay station shown in FIG. 5.
[0018] [0018]FIG. 7 is a view of a relay station being recovered.
DETAILED DESCRIPTION
[0019] Referring now to FIG. 1, the system 10 comprises a ground based portion 12 and an air based portion 14 .
[0020] The ground based portion 12 may comprise conventional telephone networks 16 with branches that are connected to a ground station 18 having suitable long distance transmitting and receiving means such as antenna 20 . The ground based portion 12 may also comprise mobile telephones of well known types such as cellular telephones that may be carried by individuals 22 or in vehicles 24 . The microwave antennae 20 are operative to transmit and receive a telecommunication signal to and from a sub-orbital, high altitude relay station 28 which is located at an altitude of between about 15 to 25 miles.
[0021] Preferably, there are a plurality of relay stations 28 ; each one being at a fixed location over the earth.
[0022] Each relay station 28 contains means for receiving a telecommunication signal from a ground station 20 , individual 22 or vehicle 24 and then transmitting it to another ground station 118 , individual 122 or vehicle 124 either directly or by way of another relay station 130 . Once the signal returns to the ground based portion 12 of the system 10 , the telecommunication call is completed in a conventional manner.
[0023] The relay station 28 may comprise a lighter than air device 32 . A suitable device could be an inflatable device such as a high altitude super-pressure balloon of the type developed by Winzen International, Inc. of San Antonio, Tex. The superpressure balloon 32 is configured so that it floats at a predetermined altitude. The configuring is accomplished by balancing inflation pressure of the balloon and the weight of its payload against the expected air pressure and ambient temperatures at the desired density altitude. It has been observed that devices of this character maintain a high degree of vertical stability during the diurnal passage notwithstanding that they are subject to high degrees of temperature fluctuation.
[0024] A plurality of tracking stations 36 are provided. The tracking stations include well known means which can identify a particular relay station 28 and detect its location and altitude.
[0025] As will be explained, a thrust system is provided for returning a relay station 28 to its pre-assigned location should a tracking station 36 detect that it has shifted.
[0026] Referring to FIG. 2, each of the- relay stations 28 includes a housing 40 which is supported by device 32 . The housing 40 contains a telecommunication signal transmitter and receiver 44 and a ground link antenna 48 . Antenna 48 is for receiving and sending telecommunications signals between ground stations 20 and the relay station 28 . The relay station 28 also includes a plurality of antennas 52 which are adapted to receive and transmit telecommunications signals from and to other relay stations. The housing 40 also contains a guidance module 56 that transmits the identity and location of the relay station to the tracking stations 36 . It receives instructions from the tracking station for energizing the thrust system. A guidance antenna 58 is provided to enable communication between the tracking station 36 and the guidance module 56 .
[0027] A suitable re-energizable power supply Go is mounted on housing 40 , the power supply 60 may comprise a plurality of solar panels 64 . In a well known manner the solar panels capture the sun's light and convert it into electricity which can be used by the telecommunications equipment as well as for guidance and propulsion.
[0028] In addition the power supply could also comprise a plurality of wind vanes 68 . The wind vanes may be arranged to face in different directions so that at least some of them are always facing the prevailing winds. The wind vanes 68 can be used to generate electric power in a well known manner which also can be used by the telecommunication equipment as well as for guidance and propulsion.
[0029] As seen in FIG. 4, an alternate power supply 66 may be provided in the form of a microwave energy system of similar to that which has been developed by Endosat, Inc. of Rockville, Md. The microwave energy system includes a ground based microwave generator (not shown) that creates a microwave energy beam of about 35 GHz. This beam is directed to receptors 80 on the relay 28 and there converted to direct current.
[0030] In a manner similar to the solar energy system, the microwave energy system could supply power sufficient to operate the telecommunications system on the relay station as well as provide power for guidance and propulsion. Further, the relay stations 28 may be provided with at least one microwave transmitter and suitable means for aiming the microwave transmitter at a microwave receiving means on another relay station 28 so that a source other than the ground based microwave generator is available to provide microwave energy to the relay stations.
[0031] As seen in FIGS. 3 and 4 the navigation/thrust system for the relay station 28 may comprise a plurality of rockets or jets 90 or propellers 94 . The jets 90 and propellers 94 are arranged in a horizontal plane along mutually perpendicular axes which are supported by pods 100 on the housing 40 . By selective energization of various ones of the jets or propellers the relay station 28 can be directed to and maintained at a pre-determined location over the earth.
[0032] If desired, additional jets or rockets 108 or propellers 112 could be located on vertical axes to assist in bringing the relay station to its pre-determined altitude on launch or restoring it should its drift from that altitude be more than an acceptable amount.
[0033] The tracking stations 36 and guidance module 56 are operative to energize selected ones of the jets or propellers for selected intervals to return the relay stations 28 to their pre-determined locations.
[0034] When the system 10 , is operating the customer will be unaware of its existence. Thus, when a call is placed, the telecommunications signal will be conveyed from the caller's telephone by way of a conventional network to the ground station 18 associated with that location. The microwave antenna 20 will then beam a telecommunications signal corresponding to that telephone call to the nearest relay station 28 . Switching circuity of a well known type will direct the signal to another ground station 120 near the recipient. If the recipient is further, the signal will be sent to a further relay station 130 from which it will be directed to a mobile telephone carried by an individual 122 or in a vehicle 124 or to a ground station 140 near the recipient. The signal received by the ground station 120 or 140 will be transmitted to the recipient's telephone by way of a conventional telephone network. once a communication link is established between two telephones by way of the ground stations and relay stations, the parties can communicate.
[0035] Drifting of the relay stations 28 from their pre-determined locations will be detected by the tracking stations 36 . The tracking stations 36 will then energize the thrust members on the relay stations 28 to return them to their predetermined locations.
[0036] As best seen in FIGS. 2, 5, 6 and 7 a recovery system 150 for the relay stations 28 is provided. As will be more fully explained, the recovery system includes a deflation device 152 and a remote controlled recovery parachute 154 .
[0037] Referring to FIGS. 2 and 5 one embodiment of the deflation device 152 includes a housing 160 that is formed integrally with the suitable lighter than air device 32 . The housing 160 includes an outwardly extending and radially directed flange 164 that is integrally connected to the device 32 as by welding or by adhesive. The flange 164 supports a downwardly directed, and generally cylindrical wall 168 that supports a bottom wall 172 . As seen in FIG. 5, the bottom wall 172 is defined by an open lattice so that the housing 160 is connected to the interior of the device 32 and is at the same pressure.
[0038] Near its upper end the cylindrical wall 168 supports an inwardly directed flange 176 . A frangible cover 184 is connected to the flange in airtight relation. This can be accomplished by connecting the cover to the flange by an adhesive, or with a suitable gasket between them, or by fabricating the cover as an integral part of the housing 160 .
[0039] The cylindrical wall 168 , bottom wall 172 and cover 184 define a chamber that contains the remote control recovery parachute 154 .
[0040] A small chamber 190 is formed on the underside of the cover 184 by a wall 192 . A small explosive pack 194 which is contained within the chamber 190 is responsive to a signal received by antenna 196 .
[0041] The parachute 154 has its control lines 198 connected to a radio controlled drive member 200 that is contained within the housing 160 . The drive member 200 may include electric motors that are driven in response to signals from the ground to vary the length of the control lines in a well known manner to thereby provide directional control to the parachute.
[0042] To recover the relay station a coded signal is sent to the device where it is received by antenna 196 . This results in the explosive charge 194 being detonated and the frangible cover 184 being removed.
[0043] Since the cover 184 is designed to break, the explosive charge can be relatively light so that it does not damage the parachute 154 .
[0044] In this regard the wall 192 helps to direct the explosive force upwardly against the cover rather than toward the device 32 .
[0045] After the cover has been removed, the gases will begin to escape from the interior of the device 32 through bottom wall 172 and the opening in the top of the housing. The force of air exiting from the device 32 when the cover is first removed will be sufficient to deploy the parachute.
[0046] As seen in FIG. 7, the parachute 154 will support the device 32 by way of its control lines 198 . As explained above, the relay station 28 can be directed to a predetermined location on the ground.
[0047] In the embodiment shown in FIG. 6 flange 164 supports cover 204 with an annular airtight gasket between them. The cover 204 is held against the flange 164 by a plurality of circumferentially spaced clamping brackets 210 . The clamping brackets are retractably held in engagement with the cover 204 by electrically driven motors 212 . The motors are energized in response to signals from the ground to retract the brackets 210 .
[0048] When the brackets 210 are retracted, the pressure of the gases escaping from the device 32 will dislodge the cover and permit the parachute to be deployed.
[0049] After the relay station has been serviced, the recovery system 150 can be replaced and the device 32 can be re-inflated and returned to the service.
[0050] While the invention has been described with regard to particular embodiments, it is apparent that other embodiments will be obvious to those skilled in the art in light of the foregoing description. Thus, the scope of the invention should not be limited by the description, but rather, by the scope of the appended claims.
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A sub-orbital, high altitude communications system that has at least two ground stations and at least one high altitude relay station. Each of the ground stations includes apparatus for sending and receiving telecommunications signals. The relay stations include apparatus for receiving and sending telecommunications signals from and to the ground stations and from and to other relay stations. Apparatus is provided for controlling the lateral and vertical movement of the relay stations so that a predetermined altitude and location of each of the relay stations can be achieved and maintained. Apparatus is provided for retrieving relay stations so that they can be serviced for reuse.
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TECHNICAL FIELD
This invention relates generally to convenience stores, and this invention specifically relates to prefabricated, modular, transportable, drive-thru convenience stores featuring ergonomic layouts allowing for maximum efficiency, profitability, and customer service.
BACKGROUND OF THE INVENTION
In the drive-thru industry, which allows consumers to access a variety of services from the convenience of their vehicles, numerous factors play a role in the design of the structures from which the services are provided. Among the factors considered in designing drive-thru structures are employees' access to products selected by consumers for purchase; storage area available for inventory; security, in terms of protecting both the establishment's inventory, the employees, and the customers from criminal elements; the ability to display a "menu" of available products to consumers as they approach the structure's service facility (the "drive-thru window"); the ability to efficiently rotate inventory supplies; maintaining an efficient flow of customer vehicle traffic; and the ability to fulfill the foregoing goals while lawfully abiding by all relevant government regulations, such as local zoning laws and the federal Americans with Disabilities Act ("ADA").
Additionally, certain factors exist which are peculiar to drive-thru establishments providing convenience store-type services, such as, for example, the need for a large volume of refrigerated storage; the ability to efficiently deliver and rotate short-life perishable supplies, such as dairy products; the ability to display actual products to customers; and the ability to provide efficient service to customers by delivering their purchases to the driver's side of vehicles.
Finally, prefabrication, modularity, and transportability are advantageous features of drive-thru convenience stores, for a number of reasons. First, in situations where convenience store owners do not own the land on which they build their stores, termination of the lease results in the loss of the structure to the landlord, who then may lease the structure to another tenant. If the convenience store owner's structure constitutes proprietary trade dress, the convenience store owner must then ask the landlord or subsequent tenants to alter the structure so as to avoid infringement of the trade dress or, alternatively, the convenenience store owner is placed in the position of having to bring an infringement action in order to protect its trade dress rights. Where the structure is modular and the lease includes the appropriate terminology, the convenience store owner may simply transport the structure to an alternative location upon termination of the lease. Additionally, because federal Department of Transportation regulations come into play when modular structures are transported, certain size limitations apply. For instance, the maximum width of a structure to be transported on federal roadways is 14 feet. Because of such restrictions, modular convenience stores must utilize any available space in the most economical manner feasible.
Previous attempts have been made to design ergonomically designed, prefabricated, modular, transportable buildings, certain features of which are generally described in U.S. Pat. No. 5,285,604, to Carlin; U.S. Pat. No. 5,113,974, to Vayda; U.S. Pat. No. 5,109,956, to Casale et al.; U.S. Pat. No. 5,070,661, to Lo Guidici; U.S. Pat. No. 5,052,519, to Woodham; U.S. Pat. No. 4,733,754, to Acosta; U.S. Pat. No. 4,715,159, to Hijazi; U.S. Pat. No. 4,704,827, to Murphy et al.; U.S. Pat. No. 4,236,359, to Woolford; U.S. Pat. No. 4,006,798, to De Mund; U.S. Pat. No. 3,866,365, to Honigtmm; U.S. Pat. No. 3,866,364, to Pollard; U.S. Pat. No. 3,836,220, to Ishammar; U.S. Pat. No. 3,282,382, to Thompson; and U.S. Pat. No. 2,638,636, to Pool, all of which are incorporated herein by reference. However, none of these references, either alone or in combination with others, describes a modular convenience store with these ergonomic features.
Additionally, Champion Modular Restaurant Corporation has constructed modular drive-thru fast-food restaurants identified by the "CHECKERS" trademark. However, because of the distinct, ergonomic needs of a drive-thru convenience store, none of which are described in the above-listed references, either alone or in combination, the design of the modular drive-thru fast-food restaurants does not fulfill the needs of a design for a modular drive-thru convenience store.
Thus, there is a need in the art for an ergonomically-designed workplace for use in space-constrained convenience stores.
There is an additional need in the art for such convenience stores to feature drive-thru access.
There is an additional need in the art for these drive-thru convenience stores to be modularly constructed.
There is an additional need in the art for modularly constructed drive-thru convenience stores featuring an ergonomically-designed workplace to be transportable from location to location.
SUMMARY OF THE INVENTION
The invention provides a drive-thru convenience store having an ergonomically-designed workspace. The invention further provides a prefabricated, modular convenience store having such a design.
Broadly stated, the present invention provides a convenience store including a floor; a plurality of walls extending substantially vertically from the floor and defining a perimeter of the store, the store having an interior and exterior; a roof covering the interior of the store; at least one access door for ingress to and egress from the interior of the store; a walk-in cooler having an interior, the cooler being located within the interior of the store adjacent at least one of the walls; an exterior cooler-service door for passage between the exterior of the store and the interior of the cooler; an interior cooler-service door for passage between the interior of the cooler and the interior of the store; and at least one display window disposed within at least one of the walls.
In an alternate embodiment, the plurality of walls includes a front wall; a rear wall; a left wall; and a right wall.
In an alternate form of the present invention, the front and rear walls substantially oppose one another, and the left and right walls substantially oppose one another, so that the store is substantially rectangular in shape.
In an alternate form of the present invention, the access doors include a front access door substantially intermediate the front wall and a rear access door substantially intermediate the rear wall.
In an alternate embodiment, the cooler is located left of the rear access door and spaced from the front wall.
In an alternate form of the present invention, the cooler is adjacent the rear and left walls.
An alternate form of the present invention provides the cooler further with a front side substantially parallel to and spaced apart from the rear and front walls; a right side substantially parallel to and spaced apart from the left and right walls; a left side adjacent the left wall; and a rear side adjacent the rear wall.
In an alternate embodiment, the front side substantially opposes the rear side and the right side substantially opposes the left side so that the cooler is substantially rectangular.
In an alternate form of the present invention, the exterior cooler-service door is disposed within the left side of the cooler.
An alternate embodiment further provides a cooler-product door in the right side of the cooler.
In an alternate form of the present invention, the display windows include a front display window disposed within the front wall to the side of the front access door and a rear display window disposed within the rear wall to the side of the rear access door.
An alternate embodiment further provides an employee room within the interior of the store adjacent the front and right walls, the employee room being located right of the front access door, the employee room being spaced from the rear wall; and a restroom within the employee room.
In an alternate form of the present invention, the store is assembleable off-site and transportable as a single unit.
In an alternate form of the present invention, the cooler has a front side substantially parallel to and spaced apart from the rear and front walls; a right side substantially parallel to and spaced apart from the left and right walls; a left side; and a rear side.
An alternate embodiment provides cooler racks in the interior of the cooler adjacent the cooler product doors.
In an alternate embodiment, the front and rear access doors are sliding glass doors.
An alternate embodiment provides a left display window located in the left wall between the cooler and the front wall; and a right display window located in the right wall between the employee room and the rear wall.
In an alternate form of the present invention, the front display window occupies substantially all of the front wall left of the front access door; the rear display window occupies substantially all of the rear wall right of the rear access door; the left display window occupies substantially all of the left wall between the cooler and the front wall; and the right display window occupies substantially all of the right wall between the employee room and the rear wall.
An alternate embodiment provides a cashier stand located within the interior of the store substantially intermediate between and spaced from the front and rear access doors, the stand being located right of and spaced from the cooler; and an inventory storage area located right of the cashier stand and left of the employee room.
An alternate embodiment provides front display racks adjacent the front and left display windows for displaying merchandise to the exterior of the store through the front and left display windows; and rear display racks adjacent the rear and right display windows for displaying merchandise to the exterior of the store through the rear and right display windows; wherein the cooler is spaced from the front wall sufficiently to allow stocking of the front display racks; wherein the employee room is spaced from the rear wall sufficiently to allow stocking of the rear display racks.
An alternate form of the present invention provides a freezer located within the inventory storage area. An alternate embodiment provides inventory shelving located within the inventory storage area.
An alternate embodiment provides a front canopy and a rear canopy extending from the roof over the front and rear access doors, respectively.
In an alternate embodiment, the left and right walls are less than twenty feet long. More specifically, the left and right walls may be less than or equal to fourteen feet long. In an alternate embodiment, the front and rear walls are less than sixty-five feet long. Further, the front and rear walls may be less than or equal to fifty-five feet long.
An alternate form of the present invention provides an exit-only panic door through the front wall located between the front access door and the employee area.
An alternate form of the present invention provides a modular convenience store having a floor; a plurality of walls extending substantially vertically from the floor and defining a perimeter of the store, the store having an interior and exterior; a roof covering the interior of the store; at least one access door for ingress to and egress from the interior of the store; a walk-in cooler having an interior, the cooler being located within the interior of the store adjacent at least one of the walls; an exterior cooler-service door for passage between the exterior of the store and the interior of the cooler; an interior cooler-service door for passage between the interior of the cooler and the interior of the store; and at least one display window disposed within at least one of the walls; wherein the store is assembleable off-site and transportable as a single unit.
An alternate embodiment provides a modular convenience store having a floor; a plurality of walls extending substantially vertically from the floor and defining a perimeter of the store, the store having an interior and exterior; the plurality of walls including a front wall, a rear wall, a left wall, and a right wall; the front wall being less than or equal to sixty feet long; the rear wall being less than or equal to sixty feet long and substantially opposing the front wall; the left wall being less than or equal to fourteen feet long; the right wall being less than or equal to fourteen feet long and substantially opposing the left wall; a roof covering the interior of the store; a front access door substantially intermediate the front wall; a rear access door substantially intermediate the rear wall; a walk-in cooler having an interior, the cooler being located within the interior of the store, left of the rear access door, and spaced from the front wall; an exterior cooler-service door for passage between the exterior of the store and the interior of the cooler; an interior cooler-service door for passage between the interior of the cooler and the interior of the store; wherein the store is assembleable off-site and transportable as a single unit.
Accordingly, it is an object of the present invention to provide a space-constrained convenience store employing an ergonomically designed workspace.
It is a further object of the present invention to provide such a convenience-store featuring drive-thru access.
It is a further object of the present invention to provide such drive-thru convenience stores with modular constructions.
It is a further object of the present invention to provide such modularly constructed drive-thru convenience stores featuring an ergonomically-designed workspace to be transportable from location to location.
These and other objects, features, and advantages of the present invention may be more clearly understood and appreciated from a review of ensuing detailed description of the preferred and alternate embodiments and by reference to the accompanying drawings and claims.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a front view of an embodiment of the present invention.
FIG. 2 is a rear view of an embodiment of the present invention.
FIG. 3 is a side view of an embodiment of the present invention.
FIG. 4 is a side view of an embodiment of the present invention.
FIG. 5 is a cut-away, top view of an embodiment of the present invention along line 5--5 in FIG. 1.
FIG. 6 is a cut-away view illustrating the canopy installation along line 6--6 in FIG. 2.
FIG. 7 is a cut-away view illustrating the canopy installation along line 7--7 in FIG. 6.
FIG. 8 is a cut-away view illustrating the canopy installation along line 8--8 in FIG. 6.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The description of the drawings and the embodiments of the invention is made within the frame of reference established by the drawings. In order to facilitate the understanding of the description and the appended claims, the terms "left", "right", "front", "rear", and the like are used consistently as they apply to this particular frame of reference. In actuality, the invention is not limited to this frame of reference.
The preferred embodiment of this invention is a prefabricated, modular convenience store. However, many of the features of the design are equally applicable to conventional, site-built convenience stores.
FIG. 1 shows the front view of the preferred embodiment of a store 10. Store 10 has a floor 15 and a front access door 50 (also called "front door") located near the middle of a front wall 40. A customer in his or her vehicle approaches the front door 50 in the direction indicated by the arrow A. This allows the customer to interact with the employees in the store 10 through the driver's side of his or her vehicle. The customer leaves in the same direction.
A series of front display windows 45 are disposed in the front wall 40 to the side of the front door 50 from which the customer approaches. This allows the customer to view whatever is displayed behind the front display windows 45 as he or she approaches the front door 50. In this embodiment, a series of front display windows 45 is employed to substantially occupy the entire front wall 40 to that side of the rear door 30. In actual practice, any number of front display windows 45 could be used. Also, in this embodiment, a front display window 45 is disposed in the front wall 40 to the side of the front door 50 to which the customer will exit. This particular front display window 45 allows a view of more of the inside of the store 10.
A panic door 55 is disposed in the front wall 40 next to the front door 50. This allows for emergency exit should the front door 50 become locked shut. The roof 400 covers the store 10, and front canopy 450, extends out from the roof 400 over the front door 50. Canopy 450 provides shelter to customers being served at front door 50, and also helps to shelter the store 10 itself during inclement weather, because front door 50 generally remains open while the store 10 is in operation. Canopy 450 spans from over front door 50 in each direction toward the left and right walls 80, 60. Front canopy 450 can span either more or less distance in each direction toward the left and right walls 80, 60. A longer span toward the left wall 80 could be employed to provide better shade to prevent direct sunlight from hitting front display windows 45, thereby preventing unwanted solar heating.
FIG. 2 shows the rear view of the store 10, and looks very similar to the front view shown in FIG. 1. The similarities reflect the desire to design a store in which both drive-thru lanes can be served equally efficiently. The rear access door 30 (also called "rear door") is located near the middle of rear wall 20. To allow interaction through the driver's side here as well, a customer approaches rear door 30 in the direction indicated by arrow B.
A series of rear display windows 25 are disposed in the rear wall 20 to the side of the rear door 30 from which the customer approaches and substantially occupies the entire rear wall 20 to that side of the rear door 30. Again, any number of rear display windows 25 could be used. Also, in this embodiment, a rear display window 25 is disposed in the rear wall 20 to the side of the rear door 30 through which the customer will exit.
The roof 400 covers the store 10, and rear canopy 452, extends out from the roof 400 over and shelters the rear door 30. As with the front of the store 10, a longer or shorter span toward the right and left walls 60, 80 could be employed.
FIG. 3 shows the right view of the present invention. Right display window 65 is disposed in the right wall 60 in the preferred embodiment of the store 10. The roof 400 covers the store. This figure provides a better view of canopies 450, 452 extending out from the roof.
FIG. 4 shows the left view of the preferred embodiment, looking at the opposite end of the store 10. A left display window 85 and an exterior cooler-service door 125 are disposed in the left wall 80. As discussed later, depending upon the configuration of the cooler (not shown in this figure), the exterior cooler-service door 125 may either be disposed directly in the left wall 80 or nested in an opening therethrough and actually disposed in the cooler itself.
FIG. 5 shows a top, cut-away view, looking down at the floor 15 of the preferred embodiment of the store 10. As can be seen from this view, it is preferred that the front and rear walls 40, 20 and the right and left walls 60, 80 substantially oppose one another to give the store 10 a rectangular shape.
The front door 50 and rear door 30 are located substantially near the middle of the front wall 40 and the rear wall 20, respectively. For reference, arrows A and B again show the direction customer traffic flows past the front and rear door 50, 30, respectively. Locating the doors 50, 30 thusly allows equally efficient service for each customer lane from a single, central location. In order to minimize the space needed and maximize the display functions, it is preferred that the doors 50, 30 be sliding glass doors. The cashier stand 300, is located substantially in this central location between the front and rear doors 50, 30. The cashier stand 300 can have extensions 310, 312 to allow placement of cash registers (not shown) at an angle, so that the employees can operate the registers while facing generally toward the front or rear doors 50, 30, respectively.
The walk-in cooler 100 is refrigerated by any of a number of means known in the art and located in the corner formed by the intersection of rear and left walls 20, 80. The cooler 100 has a right side 110, left side 120, front side 130, and rear side 140, in the preferred embodiment, the sides 110, 120, 130, 140 of the cooler 100 are separate cooler walls 110, 120, 130, 140. In an alternate embodiment, the rear side 140 and the left side 120 of the cooler 100 could be integral with the rear wall 20 and the left wall 80, as long as the walls 20, 80 are properly insulated.
In the preferred embodiment shown, exterior cooler-service door 125 is disposed in left cooler wall 120. Left wall 80 is provided with a corresponding opening. If the left side 120 of the cooler 100 were integral with the left wall 80, the exterior cooler-service door 125 would be disposed in the left wall 80. Deliveries of goods, especially short-life refrigerated items which need to be delivered frequently, to the store 10 can be made through the exterior cooler service-door 125. The exterior cooler-service door 125 could alternatively be located in the rear side 140 of the cooler 100, but this would necessitate delivering goods across the customer service lanes which run along the front and rear walls 40, 20. By locating the exterior cooler-service door 125 as shown, deliveries can be made without interfering with the normal flow of customer traffic.
At least one cooler-product door 115 is disposed in the right cooler wall 110. Cooler racks 150 are just inside the cooler 100 behind the cooler-product doors 115. A full selection of refrigerated goods is stocked on the cooler racks 150 for quick access through the cooler-product doors 115. This minimizes the time it takes to fill a customer order. Refrigerated goods are stored in bulk in the remainder of the cooler 100. As the stock on the cooler racks 150 is depleted, replacement goods are "rotated" from the cooler 100.
The right cooler wall 110 should be as far from the left cooler wall 120 as possible to maximize cooler capacity. At the same time, it should be spaced far enough from the cashier stand 300 to allow the cooler-product doors 115 to be opened and not interfere with efficient operation. The optimum spacing of the right cooler wall 110, the cashier stand 300 and the front door 50 would allow each to fall near the perimeter of a single imaginary circle having a diameter of approximately five feet. The cooler-product doors 115 should be hinged to avoid swinging into this circle as well. This allow employees enough room to move freely while minimizing the distances they must cover.
The interior cooler-service door 135 provides access to the cooler 100 from the interior of the store 10. The interior cooler-service door 135 may be located anywhere along the front or right cooler walls 130, 110. In order to minimize the width of the cooler 100, it is desired that the cooler-service door 135 be in the front cooler wall 130. If the interior cooler-service door 135 is to open into the cooler 100, as shown, then it should be far enough from the right cooler wall 110 to avoid the cooler racks 150 when opened. Locating it as close to the right cooler wall 110 as possible allows for more efficient operation. It minimizes the distance an employee must travel to reach goods inside the cooler 100. Also, because a path must be clear for the interior cooler-service door 135 to swing, it prevents the stacking of goods directly next to the cooler racks 150, which would slow the rotation of goods to the cooler racks 150.
Front cooler wall 130 is spaced from front wall 40. This serves several purposes which improve the operation of the store 10. First, it allows the interior cooler-service door 135 to be disposed in the front cooler wall 130 and the right cooler wall 110 to be devoted almost entirely to cooler product doors 115, the benefits of which have been discussed. Second, it allows front display window 45 to be disposed in the front wall 40, and front display racks 90 to be disposed against front display windows 45.
Non-refrigerated goods are displayed on the front display racks 90 through the front display windows 45. In order to minimize the space taken by the front display racks 90, they can be configured to fit between the mullions separating the windowpanes 45. To maximize cooler capacity, front cooler wall 130 should be as close to the front wall 40 as possible. However, there should be sufficient space between the cooler 100 and the front wall 40 so that, when the front display racks 90 are in place against the front display windows 45, there is sufficient space to stock and retrieve items efficiently from the front display racks 90. Therefore, the distance the cooler 100 needs to be from the front wall 40 will depend upon the distance the front display racks 90 extend into the store 10 from the front display windows 45. If it is desired to meet the present standards set by the ADA, three feet of clearance should be provided between the front display racks 90 and the front cooler wall 130.
An employee room 200 is positioned in the corner formed by the intersection of front wall 40 and the right wall 60. A manager area 205 and a restroom 250 are within the employee room 200. A rear employee-room wall 210 and a left employee-room wall 215 segregate the employee room 200 from the remainder of the interior of the store. An employee-room door 220 provides access to the employee room 200. A restroom wall 260 separates a restroom 250 from manager area 205, and a restroom door 270 provides passage therebetween.
The restroom 250 contains all standard equipment and fixtures (not shown) in any of numerous configurations, such as a toilet, sink, grab bars, soap dispenser, tissue dispenser, hand dryer towel dispenser and mirror. It is preferred that the size of doors 220, 270 and area of the restroom 260 be sufficient to permit wheelchair access under specifications set by the ADA.
The manager area 205 contains several standard items (not shown) as well, such as a desk, shelves, lock boxes for storage of valuable items (such as cigarettes) and mop sink.
This configuration of the employee room 200 is preferred but not necessary. For instance, the doors 220, 270 could be disposed differently. Either or both doors 220, 270 could be located in rear employee-room wall 210. It is not vital that there be access directly between the manager area 205 and restroom 250.
Another alternative configuration could eliminate left employee-room wall 215 and shorten rear employee-room wall 210 so that manager area 205 would not be enclosed. However, it is preferred that manager area 205 be enclosed because it improves the aesthetics of the store 10 and provides an out-of-sight area for tasks that, for security or other reasons, should not be done in plain sight.
Rear employee-room wall 210 is spaced from rear wall 20. This allows rear display windows 25 to be disposed in the rear wall 20, and rear display racks 70 to be disposed against rear display windows 25. The distance the employee room 200 needs to be from the rear wall 20 will depend upon the distance the rear display racks 70 extend into the store 10 from the rear display windows 25, so that there is sufficient space to stock the racks 70, and, if desired, to meet ADA standards.
Between the cashier stand 300 and the employee room 200 is an inventory storage area 75. In area 75 inventory shelving 77 and at least one freezer 76 should be supplied. To improve efficiency, upright freezers 76 are preferred, because employees can retrieve items from them quickly, but any of a number of standard freezer types could be employed. Freezers 76 are placed back-to-back just to the right of the cashier stand 300 to reduce the space needed and facilitate access. Just to the right of the freezers 76 is the inventory shelving 77, for bulk items, and an ice merchandiser 78. It is also preferred that a cigarette dispenser (not shown) be suspended above the cashier stand 300 for easy access.
As the figures show, display windows 25, 45, 65, 85 are disposed in almost all available exterior wall space, except where the cooler 100 and employee room 200 dictate otherwise. This serves many functions. First, from a marketing standpoint, it provides as much display area as possible for displaying merchandise to customers. From an operational standpoint, it allows the customers to watch the employees filling orders, which will encourage efficiency from the employees and keep customers' attention while they wait in line. From a safety standpoint, it provides a view of the majority of the store 10 from a distance, and allows the interior lights to illuminate the nearby surroundings, creating a safer environment for both employees and customers. Safety is further increased by providing ample exterior lighting, especially on the underside of the canopies 450, 452. In addition, for late-night transactions, "security pass-throughs" (not shown) could be provided next to front and rear doors 50, 30. This could be any acceptable mechanism which would allow passage of a small bag of groceries in a secure manner while shielding employees, and would allow the doors 50, 30 to remain closed and locked.
In the preferred embodiment, the store 10 is rectangular in shape. However, this is not necessary to the invention. For example, the portion of the left wall 80 between the cooler 100 and the front wall 40 could be angled inward, creating an additional short wall "cutting" the corner off the building. Left display window 85 could be disposed in the new angled wall portion. A similar alteration could be made to the design at the other end of the store, at the portion of the right wall 60 between the employee room 200 and the rear wall 20.
In the preferred embodiment, the entire store 10 is constructed as a modular unit. Materials and means generally known in the art are used to manufacture the store 10 away from its ultimate use site. Items such as the display racks 70, 90, the cooler racks 150, the freezers 76, and the inventory shelving 77 may be either affixed in position at manufacture, or installed at the site. In order to facilitate shipment of the store 10, the canopies 450, 452 can be installed once the store 10 has been delivered to the site. At the site, the foundation is laid and exterior plumbing, telephone, and electrical hook-ups are readied prior to the delivery of the store 10.
In order to maintain a proper inventory, it is desired that the cooler 100 have a horizontal area of approximately one hundred eighty square feet. However, as a modular unit, the preferred embodiment of the store 10 is subject to certain size constraints. If it is desired that the store 10 be delivered via truck on the highway, current regulations require that the entire store 10 be no wider than fourteen feet. This places serious constraints on the design of the store. In order to fit such a large cooler 100 into such a narrow space, and allow sufficient room for display racks 90 and windows 45, the cooler 100 must be elongated in shape.
There is another advantage to having a cooler 100 with this elongated shape, regardless of whether it is used in a prefabricated, modular store, or a conventional site-built store. With less space between front and rear cooler walls 130, 140, there is less room for stacking rows of refrigerated goods in front of one another along these walls. Because there are fewer rows, less time will be spent finding and retrieving goods from behind other goods, thereby increasing the efficiency of rotation of inventory to the cooler racks 150.
The preferred embodiment takes on the following dimensions. Front and rear walls 40, 20 are approximately fifty-four feet long. Left and right walls 80, 60 are slightly under fourteen feet long. The cooler 100 is approximately twenty-two feet long and approximately eight and two-thirds feet wide. Employee room 200 is approximately eight and two-thirds feet from front wall 40 to rear employee-room wall 210. The restroom 250 is slightly under six feet from right wail 60 to restroom wall 260. Manager area 205 is approximately seven feet from restroom wall 260 to left employee-room wall 215.
Once the modular store 10 is delivered and anchored by conventional means, the canopies 450 and 452 are installed, if they are not already attached. This can be done by means known in the art, an example of which is shown in FIGS. 6-8.
FIG. 6 shows a vertical column 485 supporting a horizontal roof I-beam 475 as part of the main structure of store 10. A channel form 480 is bonded by conventional means to roof I-beam 475. Similarly, a canopy I-beam 470 is bonded to plate 490. To secure the canopies 450, 452 to the store 10, plates 490, 491, and channel form 480 are bonded and bolted together in sequence as shown, by using bolts 495 and nuts 496. It can be seen that the canopy I-beam 470 is bonded to the plate 490 at an angle. This provides the canopies 450, 452 with their angle best seen in FIGS. 3 and 4. In the figures, canopies 450, 452 are shown sloping up away from the store 10. In actual practice, the canopies 450, 452 may be disposed at any desired angle.
FIG. 7 shows the attachment of the canopies 450, 452 from a different perspective, shown by line 7--7 in FIG. 6. The distribution of the nuts 496 about canopy I-beam 470 can be seen better from this view. FIG. 8 is the opposite view, shown by line 8--8 in FIG. 6. This shows the bolts 495, which are mated with the nuts through plates 490, 491, and in some cases through channel form 480. As can be seen from this figure and FIG. 6, column 485 passes through a gap in a lower flange 481 of channel form 480.
A series of canopy I-beams 470 is cantilevered along the roofline of the store 10 in this fashion to form the support for the canopy. The number of canopy I-beams 470 that must be used depends upon the length the canopy 450 (or 452) is desired to be. After the canopy I-beams 470 are in place, any desired form of cover (not shown) can be fastened to them to form the "ceiling" of the canopy; for example, deck pan can be used.
Accordingly, it will be understood that the preferred embodiment of the present invention has been disclosed by way of example and that other modifications and alterations may occur to those skilled in the art without departing from the scope and sphere of the appended claims.
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A modular convenience store. The store has a floor and a plurality of walls extending substantially vertically from the floor, which define a perimeter of the store, which has an interior and exterior. This plurality of walls includes a front wall, a rear wall, a left wall, and a right wall. The front wall is less than or equal to sixty feet long. The rear wall is less than or equal to sixty feet long and substantially opposing the front wall. The left wall is less than or equal to fourteen feet long, and the right wall is less than or equal to fourteen feet long and substantially opposing the left wall. A roof covers the interior of the store. A front door is substantially intermediate the front wall, and a rear door is substantially intermediate the rear wall. A walk-in cooler, with an interior, is located within the interior of the store, adjacent the left and rear walls, left of the rear door, and spaced from the front wall. An exterior cooler-service door is provided for passage directly between the exterior of the store and the interior of the cooler. An interior cooler-service door is provided for passage between the interior of the cooler and the interior of the store. The store is assembleable off-site and transportable as a single unit.
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FIELD OF THE INVENTION
[0001] The invention relates generally to intraluminal devices for containing particulate in the vessels of a patient. More particularly, the invention relates to a catheter having a mechanically actuated fluid-column occluder for containing emboli in a blood vessel during an interventional vascular procedure. Furthermore, the invention concerns a mechanically actuated fluid-column occluder mounted on a guidewire that can also be used to direct an interventional catheter to a treatment site within a patient.
BACKGROUND OF THE INVENTION
[0002] Catheters have long been used for the treatment of diseases of the cardiovascular system, such as treatment or removal of stenosis. For example, in a percutaneous transluminal coronary angioplasty (PTCA) procedure, a catheter is used to insert a balloon into a patient's cardiovascular system, position the balloon at a narrowed treatment location, inflate the balloon to expand the narrowing, and remove the balloon from the patient. Another example is the placement of a prosthetic stent in the body on a permanent or semi-permanent basis to support weakened or diseased vascular walls to avoid closure or rupture thereof.
[0003] These non-surgical interventional procedures often avoid the necessity of major surgical operations. However, one common problem associated with these procedures is the potential release into the bloodstream of atherosclerotic or thrombotic debris that can embolize distal vasculature and cause significant health problems to the patient. For example, during deployment of a stent, it is possible for the metal struts of the stent to cut into the stenosis and shear off pieces of plaque which become embolic debris that can travel downstream and lodge somewhere in the patient's vascular system. Further, particles of clot or plaque material can sometimes dislodge from the stenosis during a balloon angioplasty procedure and become released into the bloodstream.
[0004] Medical devices have been developed to attempt to deal with the problem created when debris or fragments enter the circulatory system during vessel treatment. Practitioners have approached prevention of escaped emboli through use of occlusion devices, filters, lysing, and aspiration techniques. For example, it is known to remove the embolic material by capturing emboli in a filter positioned distal of the treatment area.
[0005] Alternatively, an occlusion device may be deployed distally or proximally of the treatment area to block the flow of contaminated blood, which can then be aspirated along with the embolic debris contained therein. Known occlusion guidewires include an occluder membrane surrounding an expandable mechanical structure that is actuatable by push-pull action of a core wire through an outer tubular member. However, such expandable mechanical structure can be complex to fabricate and can add undesirably to the overall collapsed profile of the occlusion guidewire.
[0006] Other known occlusion catheters or guidewires include an inflatable occlusion balloon located adjacent the distal end of a hollow guidewire. Dilute radiopaque contrast agent is forced through an inflation lumen to inflate and deflate the occlusion balloon. However, operating the balloon may take longer than desired due to the viscosity of the inflation medium, the small size of the inflation lumen, and the requirement to attach, detach and operate one or more inflation accessories at the proximal end of the catheter or guidewire. Accordingly, there is a need for a simplified, low-profile embolic protection device.
BRIEF SUMMARY OF THE INVENTION
[0007] The present invention is a protection device for collecting/containing embolic debris in a body lumen. The protection device includes an outer tubular member, an elongate inner member longitudinally slidable within the outer tubular member, and a mechanically actuated occluder The occluder has a proximal end fixedly sealed about a distal end of the outer tubular member, a distal end axially secured to the elongate inner member and a fixed amount of fluid contained therein. In an embodiment of the present invention, a sliding seal accommodates relative sliding movement between the inner and outer members and prevents leakage of occluder fluid from the occluder. In another embodiment, the occluder has an annular cross-section defined by the coaxial arrangement of an inner and an outer tubular wall. The annular space between the inner and outer walls is filled with a fixed amount of occluder fluid. The inner tubular wall isolates the core wire from occluder fluid. Upon positioning of the occluder within the body lumen distally or proximally of the treatment site, proximal movement of the elongate inner member relative to the outer tubular member forces the ends of the occluder toward each other, thus redistributing the occluder fluid radially outward to deploy the occluder into sealing apposition with a wall of the body lumen.
[0008] In various embodiments of the present invention, the occluder may be comprised of an impervious elastomeric material filled with a biocompatible fluid.
BRIEF DESCRIPTION OF DRAWINGS
[0009] The foregoing and other features and advantages of the invention will be apparent from the following description of the invention as illustrated in the accompanying drawings. The accompanying drawings, which are incorporated herein and form a part of the specification, further serve to explain the principles of the invention and to enable a person skilled in the pertinent art to make and use the invention. The drawings are not to scale.
[0010] FIG. 1 is a side view of a distal protection device in accordance with an embodiment of the present invention.
[0011] FIG. 2 is a partial cross-section of a distal end of the distal protection device of FIG. 1 within a patient's vascular anatomy.
[0012] FIG. 3 is a partial cross-section of a distal end of the distal protection device of FIG. 1 in accordance with another embodiment of the present invention.
[0013] FIG. 3A is a transverse cross-section of the distal protection device of FIG. 3 taken along line A-A.
[0014] FIG. 3B is an enlarged view of a distal end of the distal protection device of FIG. 3 in accordance with another embodiment of the present invention.
[0015] FIG. 4 illustrates a distal end of the distal protection device of FIG. 1 with the occluder in its deployed configuration within the patient's vascular anatomy.
[0016] FIG. 5 is a partial cross-section of a distal end of a protection device within a patient's vascular anatomy according to another embodiment of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
[0017] Specific embodiments of the present invention are now described with reference to the figures, wherein like reference numbers indicate identical or functionally similar elements. The terms “distal” and “proximal” are used in the following description with respect to a position or direction relative to the treating clinician. “Distal” or “distally” are a position distant from or in a direction away from the clinician. “Proximal” and “proximally” are a position near or in a direction toward the clinician.
[0018] While the following description generally refers to a distal protection device, it should be understood that the invention is also applicable to a proximal protection device, wherein the occluder may be deployed proximally of a treatment site to block flow upstream of the site. A treatment apparatus, such as a catheter, may be delivered via a through lumen in the proximal protection device to provide therapy at the site. See lumen 509 in FIG. 5 . Debris generated during the therapy will not move downstream to embolize because of the temporary stasis in the vessel. Fluid that may be contaminated with debris can be aspirated via the through lumen before the occluder is contracted to allow fluid flow to resume.
[0019] The present invention is a temporary distal protection device for use in minimally invasive procedures, such as vascular interventions or other procedures, where the practitioner desires to capture and remove embolic material that may be dislodged during the procedure. As shown in FIGS. 1 and 2 , distal protection device 100 , viz, occluder system 100 , includes an elongate tubular member, or catheter shaft, 102 , a core wire 108 slidably extending there through, and a hub 110 . Core wire 108 extends within a lumen 207 of tubular member 102 from a proximal end 104 to a distal end 101 thereof. A seal 205 is secured to distal end 101 of tubular member 102 and slidingly seals about core wire 108 to retain fluid on the distal, or occluder side of seal 205 , like a rod-type seal for a hydraulic cylinder. Alternatively, seal 205 may take the form of a cap that sealingly fits over distal end 101 of tubular member 102 . A fluid-column occluder 106 for containing a fixed amount of biocompatible fluid 212 is joined to distal end 101 of tubular member 102 and core wire 108 , as described below.
[0020] One alternative to rod-type seal 205 is a seal fixed about core wire 108 to slidingly seal anywhere along the interior surface of tubular member 102 to retain fluid on the distal, or occluder side of the seal, like a piston-type seal (not shown) for a hydraulic cylinder. In another alternative embodiment, a rolling diaphragm-type of seal (not shown) can be disposed between tubular member 102 and core wire 108 . A seal that allows movement between core wire 108 and shaft 102 may be located at distal end 101 , e.g. seal 205 , at proximal end 104 , or anywhere in lumen 207 between shaft ends 101 , 104 . If a seal is located at shaft proximal end 104 or within lumen 207 proximally of shaft distal end 101 , then the portion of lumen 207 distal to the seal will be in fluid communication with the interior of occluder 106 and thus will also contain occluder fluid 212 , which may act as a lubricant between core wire 108 and shaft 102 .
[0021] Fluid-column occluder 106 has a proximal end 214 and a distal end 216 . Occluder distal end 216 is axially secured to core wire 108 and occluder proximal end 214 is attached to distal end 101 of tubular member 102 . Occluder ends 214 , 216 may be fixedly attached to tubular member 102 and core wire 108 , respectively, by use of a bonding sleeve, and/or an adhesive, as would be apparent to one of ordinary skilled in the relevant art. Occluder 106 is filled with occluder fluid 212 in the form of gas, liquid, semisolid, i.e. a gel, or combinations thereof. Non-limiting examples of suitable fluids 212 are carbon dioxide gas, saline and silicone oil. Other amorphous, fluid-like substances may be utilized, as long as the substance is biocompatible and is capable of redistributing, deforming or flowing in response to forces applied thereto during push-pull actuation of occluder system 100 . In a further embodiment, fluid 212 may comprise suspended radiopaque particles or a dilute or undiluted x-ray contrast agent to aid in fluoroscopic observation of the occluder in vivo. Optionally and/or in addition to fluoroscopic material within fluid 212 , radiopaque markers (not shown) may be placed on proximal and distal ends 214 , 216 of occluder 106 to aid in fluoroscopic observation during manipulation thereof.
[0022] Core wire 108 may be made from a metal, such as nitinol, stainless steel, or cobalt-chromium superalloy wire. In an embodiment of the present invention (not shown), core wire 108 may be tapered at its distal end and/or be comprised of one or more core wire sections of different materials. Core wire 108 may be centerless-ground to have several diameters in its profile in order to provide regions of different stiffnesses with gradual transitions there between. Core wire 108 has a proximal end 109 that extends outside of the patient from proximal end 104 of tubular member 102 . Core wire 108 may also include a coiled tip portion, such as, coiled tip portion 326 shown in FIG. 3 , or may include a flexible coil spring that is formed from a round or flat coil of stainless steel and/or one of various radiopaque alloys, such as platinum, as is well known to those of skill in the art of medical guidewires.
[0023] In another embodiment of the present invention, tubular member or catheter shaft 102 may be constructed of multiple shaft components (not shown) of varying flexibility to provide a gradual transition in flexibility. Such a shaft arrangement is disclosed in U.S. Pat. No. 6,706,055, which is incorporated by reference herein in its entirety. In addition, a liner or axial bearings (not shown) as disclosed in the '055 patent may be utilized between core wire 108 and outer shaft 102 in order to facilitate sliding movement there between during expansion and collapse of occluder 106 . In another embodiment, tubular member 102 may be a hollow tube enabling distal protection device 100 to also function as a medical guidewire.
[0024] Tubular member 102 may include a thin-walled, tubular structure of a metallic material, such as stainless steel, nitinol, or a cobalt-chromium superalloy. Such metallic tubing is commonly referred to as hypodermic tubing or a hypotube. Metallic tubing formed from other alloys, as disclosed in U.S. Pat. No. 6,168,571, which is incorporated by reference herein in its entirety, may also be used in the tubing of the present invention. In the alternative, outer shaft 102 may include tubing made from a thermoplastic material, such as polyethylene block amide copolymer, polyvinyl chloride, polyethylene, polyethylene terephthalate, polyamide, or a thermoset polymer, such as polyimide.
[0025] Fluid-column occluder 106 is comprised of an occluder casing 211 that contains occluder fluid 212 . Occluder casing 211 is comprised of a biocompatible elastic material that is impermeable to bodily fluids, as well as to the contained occluder fluid 212 . In an embodiment of the present invention, occluder casing 211 may be formed from an elastic material such as latex, silicone elastomer, or other viscous forms of natural and synthetic rubbers such as butadiene/acrylonitride copolymers, copolyesters, ethylene vinylacetate (EVA) polymers, ethylene/acrylic copolymers, ethylene/propylene copolymers, polyalkylacrylate polymers, polybutadiene, polybutylene, polyethylene, polyisobutylene, polyisoprene, polyurethane, styrenebutadiene copolymers, and styrene-ethylene/butylene-styrene. Occluder 106 may be made, completely or partially, self-expanding, meaning that occluder 106 may be made to have a mechanical memory to return from the radially contracted or columnar configuration to the radially expanded or deployed configuration, as shown in FIG. 4 . Such mechanical memory can be achieved in occluder 106 by making occluder casing 211 in the shape of the deployed configuration, as by casting or blow molding occluder casing 211 inside a hollow mold, or by forming occluder casing 211 over a removable mandrel, e.g. by dipping or thermoforming.
[0026] Occluder 106 is sized and shaped such that when it is deployed, as shown in FIG. 4 , its greatest diameter will be expanded into sealing contact with the inner surface of the blood vessel wall into which it is placed. The inner surface contact is maintained around the expanded circumference to prevent any emboli from escaping past occluder 106 . In the embodiment shown in FIG. 2 , occluder casing 211 is of a substantially cylindrical or columnar, radially contracted shape filled with occluder fluid 212 , as is occluder casing 511 shown in the embodiment of FIG. 5 that is described further below.
[0027] Alternatively, as shown in the embodiment of FIGS. 3, 3A and 3 B, occluder casing 311 of occluder 306 has an annular cross-section defined by the coaxial arrangement of an inner tubular wall and an outer tubular wall. The annular space between the inner and outer walls is closed at occluder proximal and distal ends 314 , 316 and the fixed internal volume thus defined is filled with a fixed amount of occluder fluid 212 , as measured by volume or mass. The inner tubular wall defines a central lumen 313 that surrounds core wire 108 and isolates core wire 108 from occluder fluid 212 . As in the embodiment of FIG. 2 , occluder distal end 316 is axially secured to core wire 108 and occluder proximal end 314 is attached about distal end 101 of tubular member 102 . However, because occluder fluid 212 is contained within annular occluder casing 311 and does not make contact with the portion of core wire 108 within lumen 313 , no seal or sealing member is needed to seal distal end 101 of tubular member 102 .
[0028] In a further embodiment as shown in FIG. 3B , occluder distal end 316 may be axially secured to and rotatable with respect to core wire 108 . Occluder distal end 316 may be affixed to a cylindrical collar or bearing 324 , such that core wire 108 may rotate relative to occluder 306 and tubular member 102 . The bearing may be held in its axial position relative to core wire 108 by proximal and distal stops 320 , 322 , which are fixedly attached to core wire 108 .
[0029] Distal protection device 100 is transformable between its radially contracted and deployed configurations by relative movement between proximal and distal ends 214 , 216 of fluid-column occluder 106 . Distal protection device 100 is tracked through a patient's vasculature with occluder 106 in its low profile, contracted form, as shown in FIG. 2 . Once occluder 106 is situated distal of the treatment site, occluder 106 is transformed into its deployed configuration by pulling core wire 108 proximally within tubular member 102 , or by pushing tubular member 102 distally over core wire 108 . This push-pull actuation draws ends 214 , 216 toward each other, thus shortening the length of occluder 106 and redistributing occluder fluid 212 radially outward within occluder casing 211 to thereby bring occluder 106 into contact with the walls of the vessel lumen, as shown in FIG. 4 .
[0030] If occluder fluid 212 is a gas, then the initial fixed amount, i.e. fixed mass, of fluid 212 may be compressed from its initial volume to a somewhat smaller volume and corresponding increased internal pressure resulting from shortening the length of occluder 106 during push-pull actuation. However, with proper selection of elastic material and thickness for occluder casing 211 , a gas-filled embodiment of occluder 106 will expand into its deployed configuration in response to push-pull actuation of distal protection device 100 . Occluder 106 is contracted for removal from the body lumen by reversing the push-pull deployment actuation, i.e. by distally advancing core wire 108 relative to tubular member 102 or by proximally drawing tubular member 102 over core wire 108 . As described above, fluid-filled occluder 106 is transformable between contracted and deployed configurations by mechanical actuation, not by adding fluid to, or removing fluid from, the interior of occluder 106 .
[0031] FIG. 5 illustrates a further embodiment of the present invention situated within a body lumen, with an embolic occluder 506 in its contracted configuration. Distal protection device 500 includes occluder 506 attached at a proximal end 514 to a distal end 501 of an outer tubular member or shaft 502 and attached at a distal end 516 to an inner tubular member or shaft 503 . Inner tubular member 503 includes a lumen 509 to slidably accommodate a therapy device (not shown) and/or a guidewire 508 therein, whereas outer tubular member 502 includes a lumen 507 to slidably accommodate inner tubular member 503 therein. Occluder ends 514 , 516 may be joined to outer and inner tubular members 502 , 503 , respectively by a bonding sleeve, and/or an adhesive, as would be apparent to one of ordinary skilled in the relevant art. Occluder casing 511 of occluder 506 may be formed from the same elastic materials described above with respect to occluder casing 211 , such that occluder proximal end 514 forms integral seal 505 for accommodating sliding movement of inner tubular member 503 there through without leakage of fluid 512 from occluder 506 . Alternatively, distal protection device 500 may include a seal positioned and secured between inner and outer tubular members 503 , 502 , as described above with reference to seal 205 in the embodiment of FIG. 2 .
[0032] Distal protection device 500 is transformable between its deployed and contracted configurations by relative movement between proximal and distal ends 514 , 516 of occluder 506 . Distal protection device 500 is tracked through a patient's vasculature over guidewire 508 with occluder 506 in its contracted or columnar configuration, as shown in FIG. 5 . Once occluder 506 is situated distal of the treatment site, occluder 506 is transformed into its deployed configuration by pulling inner tubular member 503 proximally relative to outer tubular member 502 . This push-pull actuation draws ends 514 , 516 toward each other, thus shortening the length of occluder 506 and redistributing occluder fluid 512 radially outward within occluder casing 511 to thereby bring occluder 506 into contact with the walls of the vessel lumen.
[0033] Similarly to the embodiment shown in FIG. 2 , occluder 506 is contracted for removal from the body lumen by distally advancing inner shaft 503 relative to outer shaft 502 . Inner tubular member 503 and outer tubular member 502 may be of any construction or material previously described with reference to tubular member 102 .
[0034] While various embodiments of the present invention have been described above, it should be understood that they have been presented by way of illustration and example only, and not limitation. It will be apparent to persons skilled in the relevant art that various changes in form and detail can be made therein without departing from the spirit and scope of the invention. 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 appended claims and their equivalents. It will also be understood that each feature of each embodiment discussed herein, and of each reference cited herein, can be used in combination with the features of any other embodiment. All patents and publications discussed herein are incorporated by reference herein in their entirety.
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A flexible elongate device having a distally mounted occluder for collecting particulate debris in a body lumen. The occluder containing a fixed amount of fluid is reversibly expandable by push-pull actuation from a contracted configuration to a deployed configuration wherein the occluder is expanded into sealing engagement with the wall of the body lumen. The occluder has a distal end axially secured to an elongate inner member and a proximal end attached to a distal end of an outer tubular member. The occluder has an impermeable occluder casing for containing the occluder fluid. The elongate inner member is slidable within the outer tubular member such that relative longitudinal movement between the elongate inner member and outer tubular member changes the length of the occluder and thus redistributes the occluder fluid within the occluder casing to transform the occluder between its contracted and deployed configurations.
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The present invention relates generally to document preparation systems and, particularly, to document preparation systems used to create sets of related documents.
BACKGROUND OF THE INVENTION
A document preparation project, such as writing the user manuals for the Unix operating system, can involve many authors collectively writing tens of manuals comprising thousands of pages. In such a project an author of one manual section often needs to reference or include in their section data or information from different sections and/or manuals.
In a conventional document preparation system an author needing to find such information must laboriously scan the other sections and/or manuals until they find the file that contains the desired information.
Once an author finds the desired information, they can employ one of many prior art mechanisms to incorporate the found information in the target document. For example, a hypertext link that references the desired information can be inserted into the target document that causes the linked information to be printed out whenever the target document is printed.
Today, this method is generally only possible when the link and the cross-referenced material are in the same manual. This method does not work in any commercially-available system when information needs to be accessed across multiple manuals. However, this too might also be possible given World Wide Web technology. As an alternative to automatic incorporation the author can simply copy the information into their own section.
The prior art document preparation methodology becomes unmanageably complex and inefficient when many authors from different groups and in different physical locations cooperate to write multiple manuals of a large product or project. Additional complexity is added when the documents are being written or updated concurrently, in which case the search for current or a correct version of the information to link could be never ending.
Generally, the cross-reference is limited to standard entities supported in the document preparation system, such as chapters, figures, sections, etc. An author might wish to import only a small part of another author's document that is not necessarily characterized as a standard textual unit (e.g., section, chapter, figure, table, list, etc.). For example, an author might want to import part of a phrase that specifies a value for a parameter that appears in more than one document. Using prior art mechanisms, such as tables of contents or indices, it would be difficult to provide meaningful information about such importable information that would enable the author to find it, let alone import it.
SUMMARY OF THE INVENTION
In summary, the present invention includes methods and protocols that enable efficient and seamless collaboration among multiple sets of authors of related documentation books in a documentation set wherein each book in a set written by multiple authors constitutes a single domain, and multiple of these domains consititute the documentation set such that each domain may be independently administered, be geographically dispersed, be on different computer and operating systems, and be connected by either a corporate intranet, or the public internet, networking infrastructure.
In particular, the present invention is a method for linking data in a document set including a plurality of books written by different groups of authors. The first step involves an author of a first book tagging an information unit (iunit) in that book with a tag that provides information about the iunit, including a semantic attribute and a unique identifier. The author then exports the tag to a tag repository that is accessible to all groups of authors. An author of a second book can then access the tag repository and select a tag whose corresponding information they would like to import into the second book.
The semantic information is preferably a meaningful description provided by the author of the first book that is viewable and searchable in the tag repository to enable an iunit of a desired semantic type to be selected for importation into the second book.
The tag repository can be distributed across a plurality of networked nodes. In this embodiment the exporting step comprises exporting tags for a particular book to a respective tag repository located on a predetermined node and the selecting step comprises selecting relevant tags from among all of the tag repositories.
The tag repository can also be distributed across a plurality of networked nodes running a filesystem. In this case the exporting step comprises creating a common, shared directory including the tags for all of the books and the selecting step then comprises selecting relevant tags from the common directory using utilities provided by the filesystem.
Alternatively, the tag repository can comprise a single, global tag repository stored on a single computer and accessed through network protocols such as HTTP (hypertext transfer protocol), in which case the access could be from an HTML-based browser.
In another embodiment the tag repository can be distributed across multiple computers that permit access to the tags through a variety of means, such as Web browsers, remote procedure calls (RPC) and client-server engines.
The present invention also includes systems that perform the methods and protocols described above.
BRIEF DESCRIPTION OF THE DRAWINGS
Additional objects and features of the invention will be more readily apparent from the following detailed description and appended claims when taken in conjunction with the drawings, in which:
FIG. 1 is a diagram of a document preparation system in which the present invention is implemented;
FIG. 2 is a data flow diagram illustrating the operation of a generic document unit 218 (DocUnit) of FIG. 1;
FIG. 3 is a block diagram of a preferred embodiment of the present invention that employs a distributed tag repository;
FIG. 4 is a block diagram of a preferred embodiment of the present invention that employs a global tag repository;
FIG. 5 is a block diagram of a preferred embodiment of the present invention that is implemented on a computer network wherein the nodes are linked and are running a filesystem;
FIG. 6 is a block diagram of a computer system in which the present invention is implemented; and
FIG. 7 is a block diagram of a preferred embodiment of the present invention that is implemented on a computer network in which addressing is URL-based and wherein the tags are maintained in HTML files and accessed through Web browsers.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The following glossary defines terms that are used throughout the description.
______________________________________Glossary of Terms______________________________________iunit a unit of information in a Docunit that is identified by a property-value pair in the Doctags;Docunit a unit of documentation mapped to a single file;Document a collection of one or more Docunits;Doc- a self-contained unit of document administration with one ordomain more authors generating one or more Documents (for the purposes of the present discussion, Docdomains are also referred to as Books;Docset a collection of one or more DocdomainsDoctags a collection of one or more tags in a Docdomain that export pointers to iunits from Documents in their Docdomain to other Docdomains;tagfinder a software function that parses the Doctags database and finds a pointer to the requested information based on some user specified search function;tagmaker a software function that parses the Docunit to generate a Doctags database for that document;URL Universal Resource Locator, a file/resource address used on the Internet and intranets of the form: communications protocol. domain name. file/resource identifier).______________________________________
Referring to FIG. 1, there is shown a depiction of a document preparation system 200 in which the present invention is implemented. The system 200 is used to prepare a document set 210 that includes one or more books 212. For example, the document set 210 could comprise the documentation for a particular computer system, in which case respective books 212 might describe the computer system's operating software, programming tools, system utilities, processor architecture and communications capabilities.
Each book 212-1, 212-2, 212-N is created and/or updated by a set of authors 214-1, 214-2, 214-N using word processors/editors 220-1, 220-2, 220-N. A book 212 comprises one or more documents 216, each of which is sub-divided into one or more physical files/document units 218 (hereinafter referred to as "docunits"). A book author 214 creates or updates a book 212 by editing a docunit 218 with one of the editors 220.
An editor 220 can be any document editor/word processor (past, present or future) that has been modified in accordance with the teachings of the present invention to facilitate the linking of information between the different books 212-1, 212-2, 212-N. When the editor 220 is conventional, the computers on which the document preparation system 200 is executed must include software functions that perform at least a subset of the various information linking operations prescribed by the present invention. In such a case the software functions operate on the documents generated by the various editors 220. In the following discussions of the preferred embodiments it is assumed that the editors 220 are configured to implement at least a subset of the prescribed software functions.
In a document preparation environment 200 such as that depicted in FIG. 1 there is likely to be at least some duplication of information among at least a subset of the books 212. For example, the aforementioned docset 210 for a computer system might include books 212-1, 212-2 that describe the operating system at different levels of detail (e.g., a programmer's reference and a high-level user summary) and include common information, such as lists of operating system commands.
The present invention enables authors 214 to find and create links to information in other books 212 so that the common information need only be generated and maintained by the original set of authors 214. As a first step in the linking process authors 214 of a book 212 designate, or tag, information units (hereinafter, "iunits") within a docunit 218. After tagging, the creating authors export the tagged iunits to a tag repository, from which other authors may then import the exported tags. Following exporting, the tag repository includes pointers to the just-exported iunits in the docunit 218. The tag repository can include pointers to iunits exported from any or all of the books 212.
Authors 214 select from the repository iunits they wish to import into docunits 218 for their own books 212. The present invention enables authors to define tagged iunits at any document level (e.g., an entire docunit, a section of a document, a single word, etc.). As described in reference to FIGS. 3-5, the present invention can make the tagged iunits 222 accessible to all of the authors 214 regardless of whether the respective books 212 are stored on a single computer or distributed across a network of computers. The processing flow of the present invention that makes this possible is now described in reference to FIG. 2.
Referring to FIG. 2, there is shown a data flow diagram that illustrates how the present invention transforms tagged iunits 222 within a docunit 218 into a local tag database 236 and a tag repository 256. For the purposes of this discussion it is assumed that the generic docunit 218 includes one or more iunits 222 that have been marked for export with a respective tag 224. Each tag 224 designates the iunit name 226 and, optionally, the iunit value 228. The docunit 218 also includes other standard document elements that are not shown in FIG. 2.
For example, consider the docunit, "foo.bar", shown in Table 1:
TABLE 1______________________________________<group> atm.sub.-- group<docunit> foo.bar<section> "Switch Weight"˜<figure> "Switch Schematic" ˜<p> The weight of the matrix switch is <iutag> 10 tonsiunit="matrix switch" value="weight" <eiutag><p><esection><edocunit><egroup>______________________________________
The docunit, "foo.bar", is a file within the "atm -- switch" group/book/docdomain ("atm" is an abbreviation for asynchronous transfer mode). Table 1 represents the contents of the file, "foo.bar", in a generic markup language that is similar to GML™. The present invention is equally applicable to other types of document preparation systems, including WYSIWYG word processors, and is independent of any specific file format (e.g., the file may be an HTML file or any other type file). In Table 1 document elements (e.g., sections, figures, paragraphs) are delineated using mnemonics that are set off by matched sharp brackets "<" ">" and sometimes followed by a series of descriptors (e.g., "<section>"). Some of the mnemonics have a corresponding end mnemonic (e.g., "<esection>"). Thus, Table 1 includes a document section entitled "Switch Weight" (<section> "Switch Weight") that includes standard elements such as a figure showing a switch schematic (<figure> "Switch Schematic") and paragraphs (set off by <p>).
The present invention enables an author to mark phrases or paragraphs for export by assigning them an export property and then giving the property an optional value. In the preferred embodiment, this is done using iunit tags. For example, the following markup from Table 1:
<p> The weight of the matrix switch is <iutag> 10 tons iunit="matrix switch" value="weight" <eiutag>
defines the export property "matrix switch", assigns it the value "weight" and binds that value to the text "10 tons". The author of the original foo.bar docunit can then choose to export information about the "matrix switch" iunit along with any other tagged iunits. Using the exported "matrix switch" iunit information, other authors of other books that need to refer to the specific switch weight defined in the foo.bar docunit can then locate that information easily via the exported "matrix switch" tag. Thus, the present invention enables a reference/tag to be created to a document element (e.g., "10 tons") that includes the necessary information to allow another author to find the element and to create a reference to it after the tag has been exported. It is described below how the iunit information from the docunit 218 is exported and selected by other authors.
Referring again to FIG. 2, in the preferred embodiment whenever a docunit 218 is updated using the editor 220, the editor 220 executes a TagMaker program that scans the docunit 218 and generates/updates the tag database 236 from all of the exportable information within the docunit 218. The exportable information includes at least a subset of the standard document elements and the iunits that were tagged for export. In the preferred embodiment, there is one tag database 236 per book 212 (FIG. 1).
The tag database 236 includes for each iunit 222 an iunit name (IUnitName) 238, iunit location information (Location) 240 and, optionally, semantic information (Semantic Info) 242. The location information 240 specifies the docunit name 244 and, optionally, the section 246 in which the corresponding iunit 222 is found. The optional semantic information 242 indicates the value 248 of the iunit 222 and the document element 250, if any, that is bound to the iunit 222. For example, Table 2 shows the tag database entry that might be generated by the TagMaker from the "matrix weight" iunit defined in Table 1.
TABLE 2______________________________________iunit = "matrix switch""weight" = "@byte offset into the file pointing to 10 tons, num.sub.--bytes=7""DocUnitName = "foo.bar""section" = "Switch Weight"______________________________________
The first row of Table 2 indicates that this tag database entry is for the iunit, "matrix switch". The second row equates the value ("weight") of "matrix switch" with a pointer to the position in the "foo.bar" docunit/file that includes the particular occurrence of "10 tons" to which "weight" was bound and the number of bytes (7) of the referenced text. In Table 2, the pointer is shown as an unspecified offset in bytes ("@byte offset") from the beginning of the "foo.bar" file. In practice, this value would be definite. Any other pointer implementation can be used as long as it can uniquely reference the bound text. Alternatively, the referenced text can be incorporated as a string; e.g., weight="10 tons".
Note that the information in the tag database 236 can be represented in any format and that the information shown in Table 2 represents only a partial (i.e., neither maximum or minimum) set of the information that can be included in the tag database 236. For example, the tag database 236 might also indicate the book (or docdomain) 212 that encompasses the foo.bar docunit. Alternatively, if a section is not defined in the docunit 218, the section information 246 would not be included in the tag database 236.
In the preferred embodiment, the TagMaker is also configured to generate automatically tag database entries for a selectable subset of the structural elements from the docunit 218. Typically, the exportable structural elements include figures, tables, sections, chapters, etc., although other elements can also be exported. These elements are typically defined using commands provided by the editors 222. Thus, less information is needed in the tag database 236 to provide an unambiguous link to these elements. For example, Table 3 shows how the "Switch Weight" section might be referenced in the tag database 236.
TABLE 3______________________________________ iunit = :section. "Switch Weight" DocUnitName = "foo.bar"______________________________________
The first line of this tag database entry identifies the iunit by its structural type (":section.") and name ("Switch Weight"). The second line indicates the name ("foo.bar") of the DocUnit that includes the iunit.
As the docunits 218 that compose a book 212 are updated and the TagMaker is executed, the tag database 236 grows to reflect all of the exportable iunits within the docunits that compose that book 212. The tag database 236 is available to all authors 214 of the book 212. However, until it has been exported to the global tag repository 256, the information in the tag database 236 cannot be referenced by the other authors 214.
In the preferred embodiment, the tag database 236 is exported by a TagExporter that is invoked from with the editors 220 or from some other program. The TagExporter exports the information in the tag database 236 to the tag repository 256.
Like the tag database 236, the tag repository 256 includes for each iunit 222 an iunit name (IUnitName) 258, location information (Location) 260 and, optionally, semantic information (Semantic Info) 262. The location information 260 specifies the book 264, docunit 266 and, optionally, the section 268 in which the corresponding iunit 222 is found. The semantic information 262 indicates the value 270 of the iunit 222 and the bound text 272, if any. For example, Table 4 shows the tag repository entry that might be exported by the editor 220 from the "matrix weight" iunit defined in Table 1.
TABLE 4______________________________________iunit = "matrix switch""weight" = "@byte offset into the file pointing to 10 tons, num.sub.--bytes=7""DocUnitName = "foo.bar""section" = "Switch Weight""DocDomain" = "atm.sub.-- group"______________________________________
The information in the tag repository 256 is viewable and searchable. An author 214 can find iunits to import using a TagFinder program that searches for a particular iunit (or sets of iunits) in the tag repository 256 and returns to that author the corresponding link data. Once in possession of the link data, the author 214 can import the selected iunit by reference (such as a citation), or by inclusion in a target docunit 218. It is immaterial to the present invention what particular technology is used to import an iunit into the target docunit 218.
In some situations, an author 214 may wish to import an entire docunit 218, not just an iunit 222. In this case the author can execute a DocFinder program that searches for a designated docunit(s) and returns link information for the docunit(s) in the same manner as the TagFinder.
The manner in which the tag repository 256 is implemented depends largely on the architecture of the document preparation system 200. Three different architectures and corresponding tag repository implementations are now described in reference to FIGS. 3-5.
Referring to FIG. 3, there is shown a document preparation system wherein the tag repository is distributed over several networked nodes 280. In this system sets of authors 214 employ respective editors 220 to create and edit a respective book 212. The books 212 compose the docset 210. As described in reference to FIG. 2, each time one of the authors 214 updates one of the docunits 218 in the book 212 the tag database 236 is updated by the TagMaker with link information for all of the exportable iunits 222. In this embodiment the information in the tag database 236 is exported to a corresponding tag repository 286 hosted on a respective network node 280. Authors 214 import iunits 222 from different books 212 by issuing TagFind requests. A TagFind request results in the execution of the TagFinder program, which, in this system architecture, is configured to (1) visit each of the distributed tag repositories 286 in search of the desired iunits and (2) return any relevant link information to the requester. In the preferred embodiment, each node 280 that hosts one of the pieces of the distributed tag repository 286 includes server programs 282 that provide access to that piece. These server programs respond to search requests issued by the TagFinder.
Referring to FIG. 4, there is shown a document preparation system wherein the tag repository is implemented as a single, global repository. In the system of FIG. 4 the authors 214 update and edit the docunits composing their respective books 212 as described in reference to FIG. 3. The respective tag databases 236 (not shown) are also updated as described in reference to FIG. 3. All information exported from the tag databases is exported to a central tag repository 306 hosted on a global node 308. The global node 308 is accessible to all authors 214. Preferably, the tag repository 306 is implemented as a database that is accessed using search/query functions 310 provided by the global node 308. The query functions 310 are invoked in response to the TagFind requests issued by the various authors and return links to the authors as described in reference to FIG. 3.
Referring to FIG. 5, there is shown a document preparation system wherein the tag repository is implemented on a computer network whose nodes 318 are linked and are running filesystem software 320. The filesystem 320 may be a global filesystem, such as afs™; an intra-networked filesystem, such as nfs™ or a clustered filesystem. The filesystems generally allow transparent access to any file within their purview and, hence, the iunits or docunits are accessible uniformly to any programs or users. The TagMaker, TagFinder, DocFinder programs, etc. can easily make use of this transparency and can be implemented to access the linked information via normal filesystem operations.
In this system, the books 212 and tag databases 236 are updated and managed as in the embodiments of FIGS. 3 and 4. Tag repository segments 326 are stored as files on the networked nodes 318, some of which also host a respective book 212. Due to the filesystem 320, the iunit information in the repository segments 326 is visible to all authors 214 as separate files in a common, shared directory. An author 214 selects an iunit by simply copying the corresponding file into the target docunit. The
TagFinder/DocFinder can search the common, shared directory using any of the file search utilities provided by the filesystem 320. As in the other embodiments, an author who imports an iunit can choose to import the iunit by reference or by inclusion.
Referring to FIG. 6, there is shown is a block diagram of a computer system in which the present invention is implemented. This system is modeled on the document preparation system of FIG. 4, which incorporates a global tag repository. The dashed line in FIG. 5 separates a computer 360 that hosts the global tag repository 362 from a computer 410 used by a set of authors 214 to create a book 212 and its associated docunits 222.
The computer 410 includes a fast memory (such as a random access memory RAM) 412, one or more processors 414, a user interface 416 and a larger, slower memory (such as a hard disk drive--HDD) 418. In the conventional manner, application programs 422 are executed by the processor 414 in the memory 412 under control of the operating system 420. The application programs 422 include one or more editors 424, each of which, in accordance with the preferred embodiments, incorporate at least a subset of the software support functions prescribed by the present invention. As described above, these software support functions include the TagMaker 426, the TagExporter 428, the TagFinder 430 and the DocFinder 432. The memory 412 also includes at least a portion of any docunit 440 that is being edited using the editor 422.
The HDD 418 permanently stores docunits 442 and, optionally, a local tag database 444. The authors 214 interact with the computer 410 through input/output devices 416.
Given this configuration, anytime a user updates a docunit the editor 424 executes the TagMaker 426, which updates the local tag database 444. When an author executes the TagExporter 428, that program exports information 415 from the tag database 444 to the computer 360. When an author 214 executes the TagFinder 430 or the DocFinder 432, corresponding requests 417, 419 are issued to the computer 360, which returns information regarding the existence of a pointer to the requested iunit or docunit.
The computer 360 includes a memory 366, one or more processors 368 and a database 362 that hosts the tag repository 364. The computer 360 operates conventionally. That is, the processor 368 executes application software 372 in the memory 366 under the control of the operating system 370. The application software 372 includes server routines 374, 376, 378 that enable the computer 360 to respond, respectively, to exported information 415 and TagFind and DocFind requests 417, 419, from the computer 410. The TagExportServer 374 writes the exported information 415 to the tag repository 364 using whatever language is supported by the database 362. The TagFindServer 376 issues database queries to the database 362 to find the iunits specified by the TagFind request 417 and returns link information 421 for those iunits to the computer 410. The DocFindServer 378 issues database queries to the database 362 to find the docunits specified by the DocFind request 419 and returns link information 423 to the computer 410 for those docunits.
The preferred embodiments of FIGS. 3 and 5 are implemented mostly as described above in reference to FIG. 6. Any differences in implementation follow from differences in the respective document preparation system architectures. For example, the implementation of the embodiment of FIG. 3 is like that of FIG. 4, except that there are a plurality of computers that perform the functions of the computer 360 (FIG. 6). For the embodiment of FIG. 5, in lieu of the TagMakeServer, TagFindServer and DocFindServer programs, the plurality of computers hosting the various tag repositories each run the various programs that constitute the filesystem.
Referring to FIG. 7, there is illustrated another preferred embodiment that employs URLs to export doctags and to import linked information into other documents. This embodiment can be structured similarly to either FIG. 4 or FIG. 5; i.e., it can utilize a distributed or a single tag repository. For the purposes of the present discussion the tag repository is assumed to be distributed. Each docdomain (or book) has a global URL (Docdomain -- URL) associated with it at the time the docdomain it is defined. The Docdomain -- URL for each docdomain is made well known to all of the docdomains within the docset. Each Docdomain -- URL points to a file that lists the URLs (Document -- URLs) for each of the documents that compose that docdomain. Each Document -- URL in turn points to a file that lists the URLs (Docunit -- URLs) for each docunit in that document and each Docunit -- URL points to a file that contains one Doctag -- URL for each doctag in that docunit.
For example, referring to FIG. 7, there is shown a collection of networked nodes 450-i (i being 1, 2 or 3), each hosting a respective docdomain (note that all of the docdomains could also be hosted on the same node). Each node 450-i includes a tag repository 456-i that includes, among other things, a directory 458 of Docdomain -- URLs for all of the docdomans in the docset. In this example the docset includes three docdomains, therefore each tag repository 456 has a directory 458 with three Docdomain -- URLs.
The tag repository 456-1 for an exemplary node 1 includes a Docdomain1 -- URL pointer that points to a top-level file 460 that includes Document -- URLs for each of the 3 documents that make up docdomain 1. For example, the Document3 -- URL points to a file 462 that includes Docunit -- URLs for each of the three docunits that make up document 3. Details are shown for the Docunit3 -- URL from the file 462, which points to a file 464 that includes URLs for each of the three doctags defined in the docunit 3, which are stored as individual files; e.g., the files Doctag3 466 and Doctag2 468. As described above, a doctag file (e.g., Doctag3 466) can include a pointer to its associated docunit (e.g., the Docunit3 470) or can simply include a copy of its linked iunit information (e.g., Doctag2 file 468).
Thus, when the tagmaker is executed, each new doctag is assigned a URL and this URL is added by the tagmaker to the file identified by the Document -- URL. Similarly, when a new document is created, the tagmaker adds that document's Document -- URL to the file 460 identified by the respective Docdomain -- URL.
The Docdomain -- URL file 460 contents are kept locally at the site that is the "owner" of that Docdomain. For example, the contents of the Docdomain 1 file 460 are all kept on the node 450-1. The tagmaker does not export any of the tags outside the Docdomain. Instead, other authors reference the contents of a respective Docdomain -- URL file by pointing the tagfinder to a corresponding Docdomain -- URL. Docdomains are easily located as each distributed site keeps a list of all of the Docdomain URLs corresponding to the docdomains of a particular docset. For example, referring to FIG. 7, all of the tag repositories 456 hold the URLs of the top-level docdomain files, such as the Docdomain URL file 460.
In a preferred embodiment of a document preparation system configured to work with URLs a menu item is provided that invokes the tagfinder. When invoked, the tagfinder shows the contents of the docset hierarchically by accessing each Docdomain -- URL and its constituents. This mode of operation can be achieved with conventional Web browsers, which display documents comprising many subdocuments by automatically retrieving each subdocument pointed to by a parent document.
Once a doctag of interest is located, its associated information unit (iunit) can be incorporated in one of two ways into the importing document. Either of these methods can be employed in any of the described embodiments.
In a first method the linked iunit is incorporated by reference. Then, at the time of printing, or when an index or cross reference listing is to be generated for the document, the doctag reference is resolved by the document preparation system software and the actual iunit value (as defined in the doctag) is pulled into the document to replace the reference for an appropriate duration. In other words, if the document preparation system is generating a cross reference listing, it merely uses the value without inserting it into the document. On the other hand, if the document preparation system is printing the document using a postscript process, it would incorporate the iunit value in the corresponding postscript file but not the source document.
In a second method the linked iunit is incorporated by copying the iunit value into the document itself. In this case the reference is resolved and the value in the iunit property-value pair replaces the reference in the document. In this embodiment if the iunit is updated the copy is unaffected. The only way such a copy can be updated is if the importing user runs an automatic tag update function, in which case some or all of the linked iunit values are updated as appropriate.
While the present invention has been described with reference to a few specific embodiments, the description is illustrative of the invention and is not to be construed as limiting the invention. Various modifications may occur to those skilled in the art without departing from the true spirit and scope of the invention as defined by the appended claims.
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Particularly, a system and method are disclosed that enable an author of a subsection of a document quickly to locate referenced information in other parts of the document or different documents prepared by other authors and then incorporate that information in their own document. An author tags information in their document that other authors might wish to import. Each time the document is updated, or as requested by the author, the author's tags and other tags that reference information that is importable by default (e.g., section headings, figures, tables) are exported to a tag repository that is accessible to all other authors. The tag repository also holds the tags generated by other authors from different documents. Using information finding/linking programs any of the authors can search the tag repository and select tags corresponding to information they would like to import into their own documents. The information can be imported by reference, by hypertext link, or by simple copying, among other techniques.
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TECHNICAL FIELD
[0001] The present invention relates to storage of data in holographic media. In particular, the present invention relates to storage of covert holographic data in an article having a holographic recording medium.
BACKGROUND
[0002] Holography is a familiar technology for displaying three dimensional images. Basically, two coherent light beams are caused to intersect in a holographic medium. An interference pattern or grating pattern results that is unique to the two beams and which is written into the medium. This grating pattern is referred to as the hologram and has the property that if it is illuminated by either of the beams used for recording, the illuminating beam diffracts in the direction of the second writing beam. To an observer, it appears as if the source of the second beam is still present at an observation plane.
[0003] There are two significant types of holograms to consider: surface relief holograms and volume holograms. Surface relief holograms act on an incident optical wavefront by imparting a local phase shift which is proportional to the holographic material height at a specific location. In a surface relief hologram, local optical path length is proportional to the physical path length at a specific location. Volume holograms act on an incident optical wavefront by imparting a local phase shift which is proportional to the index of refraction of the holographic material at a specific location. In a volume hologram, local optical path length is proportional to the index of refraction at a specific location, while the physical path length does not vary in the holographic material.
[0004] Holograms are becoming more common for use in other types of applications such as security and data storage. In data storage applications, as is well understood by those skilled in the art, a page of data is used as a source image and a detector array is placed at the observation plane. Additionally, due to Bragg effects, many holograms may be multiplexed within the same volume of holographic material by slightly changing the angle of the reference beam with each different data page. Large numbers of holograms can be multiplexed this way in a small volume of recording material, providing high data storage potential. A complete discussion of storage holograms can be found, for example, in John R. Vacca, Holograms & Holography Design, Techniques, & Commercial Applications, Charles River Media, Inc., 2001 (“Vacca”). Generally, data stored in holographic media is only machine readable.
[0005] With respect to security applications, it is well known to include holograms on credit cards to prevent duplication of these items. A hologram is useful in this context because of the relative difficulty involved in counterfeiting a hologram as compared to printed designs, embossed features and even photographs. However, security holograms used on credit cards are generally embossed only on the surface of the card. As such, while holograms in general are relatively difficult to duplicate, a hologram on the surface of a card can be somewhat easier to duplicate or alter.
[0006] One potential solution to the problems associated with relative ease of duplication of surface holograms is offered in U.S. Pat. No. 6,005,691 for “High-Security Machine-Readable Holographic Card” to Grot et al. Grot et al. discloses a hologram card which includes a first plastic material formed to include localized topological features constituting a diffractive optical element. The diffractive optical element is structured to generate a hologram image. The hologram card also includes a protective layer which is chemically bonded to and directly contacts the topological features constituting the diffractive optical element. While the hologram card of Grot et al. includes a protective layer to make any hologram included in the diffractive element more difficult to duplicate, the card includes only a surface hologram, which holds a relatively small amount of information. That is, the hologram card disclosed in Grot et al. is relatively inefficient.
[0007] Additionally, while credit cards, and drivers licenses and identification cards, can typically store some information in a magnetic stripe often included with such cards, the amount of information such magnetic stripes can store can be relatively low.
[0008] Holographic labels, seals, and markers of all appearances and types are increasingly being used for security applications in diverse arenas of activity such as credit card identification, document authentication, currency security, branding of commodities, unique marking of software and pharmaceuticals, and numerous other applications. Within the class of holographic appliqués, the machine-embossed foils most frequently used are called diffractive optically variable image devices (DOVIDs, OVIDs, OVDs). These devices are affixed permanently or semi-permanently to the devices or commodities that they mark, and their bright, three-dimensional appearances attract attention and identify the commodity as genuine. As might be expected, unscrupulous dealers of counterfeit products attempt to replicate these holographic markers to make their products appear genuine. In response, the manufacturers of these holograms have implemented approaches such as hidden or latent images embedded in the visible hologram that can be viewed only with a specialized optical reader. Another feature becoming widely employed within these holograms is machine-readable product identification markings, such as embedded UPC bar codes. Both optical and electron-beam mastering techniques are used to produce these modern holographic foils which multiplex visible images with machine-readable data within a single embossed foil patch.
SUMMARY OF THE INVENTION
[0009] An embodiment of this invention is an article comprising a holographic recording medium comprising digital data that cannot be seen by human eye, wherein the holographic recording medium is a holographic material that records volume holograms that permit authentication of the article, further wherein the holographic material is attached to or part of the article.
[0010] Preferably, the digital data is formatted in a two-dimensional page format. Preferably, the holographic recording medium is a holographic material that records volume holograms. Preferably, the holographic material that records volume holograms is a volume hologram layer. Preferably, the thickness of the volume hologram layer is such that human eye cannot substantially discern the digital data in visible light. Preferably, the fringe period of the data holograms stored in the holographic media is such that only light that is invisible to the human eye diffracts from the data holograms. In another variation, the diffraction efficiency is low enough that the human eye cannot substantially discern the digital data in visible light.
[0011] A further embodiment of the article comprises a visible image in the holographic recording medium. Preferably, the visible image is a hologram that diffracts light that is both visible and invisible to human eye. Preferably, the article comprises a patch capable of being attached to a document, a card, a banknote or merchandise. Preferably, the article further comprises a transparent protective layer overlaying the holographic recording medium. Preferably, the digital data is machine readable holographic data. Preferably, the holographic recording medium has multiple data sections for storing the digital data and other information. Preferably, the other information is visible to human eye.
[0012] Yet a further embodiment of the article further comprises a substrate layer and a laminating layer overlaying a protective layer. Preferably, the digital data includes multiplexed holographic data. Preferably, the volume hologram layer comprises a photo sensitive polymer.
[0013] Preferably, the digital data is multiplexed in substantially a same location as that of an image hologram visible to human eye. Preferably, the digital data is patterned as a two-dimensional array of data bits. Preferably, the digital data is patterned as a series of digital data that is read by a scanner. In another variation, the digital data is a full page of digital data. More preferably, the digital data are recorded with a reference beam that is spatially encoded using phase, or amplitude, or both thereby requiring an encoded readout beam to be read the digital data. Preferably, the digital data are recorded and read by UV light.
[0014] A further embodiment of the article comprises modulation marks for timing and/or positional servo. Preferably, a layer of a photosensitive material is positioned above an optically reflective surface, an optically transmissive surface or an optically absorptive surface. Preferably, the digital data is written into the holographic recording medium before assembling components of the article into the article. More preferably, the digital data is written into the holographic recording medium after assembling components of the article into the article. Preferably, the article is a document, a card, merchandise or a banknote.
[0015] Another embodiment is a method of authentication of the article comprising obtaining the article, reading the digital data and determining the authenticity of the article. The method could further comprise optically storing the digital data as an image at an image plane by interfering a coherent reference beam with a beam of a two-dimensional image. Preferably, the digital data is arranged in a parallel barcode fashion. In another variation, the digital data is arranged in a pagewise fashion. Preferably, the beam of a two-dimensional image is passed through an intervening optical system that is a spherical afocal telescopic system comprising a multiplicity of optical elements. Preferably, the intervening optical system is an afocal telescopic system comprising two spherical optical lens groups, positioned physically to bring the focal positions of the two spherical optical lens groups into coincidence. Preferably, a single cylindrical focusing optical element is also employed for light efficiency. In one variation, a combination of cylindrical and spherical imaging optical elements are employed.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. 1 —Reader system with spherical optics and a 2D parallel output.
[0017] FIG. 2 —Reader system with spherical optics and a 1D linear output.
[0018] FIG. 3 —Reader system with spherical and cylindrical optics and a 1D linear output. This system is more light-efficient than the system illustrated in FIG. 2 .
DETAILED DESCRIPTION
[0019] Holographic storage media can take advantage of the photorefractive effect described by David M. Pepper et al., in “The Photorefractive Effect,” Scientific American , October 1990 pages 62-74. Photorefractive materials have the property of developing light-induced changes in their index of refraction. This property can be used to store information in the form of holograms by establishing optical interference between two coherent light beams within the material. The interference generates spatial index of refraction variations through an electro-optic effect as a result of an internal electric field generated from migration and trapping of photoexcited electrons. While many materials have this characteristic to some extent, the term “photorefractive” is applied to those that have a substantially faster and more pronounced response to light wave energy.
[0020] Of more interest are photopolymer recording materials. With these materials the variations in light intensity generate refractive index variations by light induced polymeration and mass transport. See Larson, Colvin, Harris, Schilling “Quantitative model of volume hologram formation in photopolymers,” J Appl. Phy. 84, 5913-5923 1996. Also photochromatic materials can be used. These materials convert light variation into index variation through structural changes or isomerazations.
[0021] A holographic recording medium includes the material within which a hologram is recorded and from which an image is reconstructed. A holographic recording medium may take a variety of forms. For example, it may comprise a film containing dispersed silver halide particles, photosensitive polymer films (“photopolymers”) or a freestanding crystal such as iron-doped LiNbO 3 crystal. U.S. Pat. No. 6,103,454, entitled RECORDING MEDIUM AND PROCESS FOR FORMING MEDIUM, generally describes several types of photopolymers suitable for use in holographic storage media. The patent describes an example of creation of a hologram in which a photopolymer is exposed to information carrying light. A monomer polymerizes in regions exposed to the light. Due to the lowering of the monomer concentration caused by the polymerization, monomer from darker unexposed regions of the material diffuses to the exposed regions. The polymerization and resulting concentration gradient creates a refractive index change forming a hologram representing the information carried by the light.
[0022] In volume holographic storage, a large number of holograms are stored in the same volume region of a holographic recording medium. Multiple holograms can be recorded in a recording medium using an exposure schedule that equalizes the amplitudes. There are several methods of holographic storage such as, angle multiplexing, fractal multiplexing, wave length multiplexing and phasecode multiplexing.
[0023] Angle multiplexing is a method of for storing a plurality of images within a single recording medium. Such angle multiplexing is described by P. J. van Heerden in, “Theory of Optical Information Storage In Solids,” Applied Optics, Vol. 2, No. 4, page 393 (1963). Angle multiplexing generally involves maintaining a constant angle spectrum for an information carrying object beam, while varying the angle of a reference beam for each exposure. A different interference pattern thereby can be created for each of a plurality of different reference beam angles. Each different interference pattern corresponds to a different hologram. Angle multiplexing thus allows a larger number of holograms to be stored within a common volume of recording medium, thereby greatly enhancing the storage density of the medium.
[0024] U.S. Pat. No. 5,793,504 entitled “Hybrid Angular/Spatial Holographic Multiplexer,” describes a method of angularly and spatially multiplexing a plurality of holograms within a recording medium. According to that patent, since diffraction efficiency of stored holograms varies, at least approximately, inversely with the square of the number of holograms stored, there is a limit to the number of holograms that can be stored within a given volume of a particular recording medium. Therefore, spatial multiplexing is employed to store different sets of holograms in different volume locations within a recording medium. The patent states that storing sets of holograms in spatially separated locations mitigates the problem of undesirable simultaneous excitation of holograms from different sets by a common reference beam. Spatial multiplexing typically does not increase the media's density, just its capacity.
[0025] A method of phase correlation multiplexing is disclosed, for example, in U.S. Pat. No. 5,719,691 to Curtis et al. entitled “Phase Correlation Multiplex Holography” which is hereby incorporated herein in its entirety by reference. In one embodiment of phase correlation multiplex holography, a reference light beam is passed through a phase mask, and intersected in the recording medium with a signal beam that has passed through an array representing data, thereby forming a hologram in the medium. The spatial relation of the phase mask and the reference beam is adjusted for each successive page of data, thereby modulation the phase of the reference beam and allowing the data to be stored at overlapping areas in the medium. The data is later reconstructed by passing a reference beam through the original storage location with the same phase modulation used during data storage.
[0026] Data recorded in the article of this invention is preferably, though not necessarily, recorded in a holographic material layer after forming the article. Examples of reader/recorders which can be used by user in such a circumstance is disclosed, for example, in H. J. Coulfal et. al, Holographic Data Storage C. Springer-Verlag 2000, pp. 343-357 and 399-407, which is hereby incorporated by reference herein in its entirety. As discussed in Coulfal, such reader/recorders can also be used to read holographic data already stored in an article in the form of a card. It is also considered to record the data before holographic material layer has been laminated with the article of this invention.
[0027] A preferred article in accordance with the present invention includes a multi-layer holographic structure such as a card, a patch, or appliqué for use on merchandise having sections for containing holographic machine readable data as well as for containing security and/or presentation information which may be either machine or human readable and may also be holographic. The article of this invention is preferably constructed of multiple layers and preferably includes at least a data layer and a protective layer overlaying the data layer. By including the protective layer, information placed in the data layer can not be altered without removing the protective layer, thereby destroying the article of this invention. In this way, information placed in the data layer is advantageously more secure than if the protective layer was not provided. Additionally, information placed in the data layer can include volume holograms, allowing many holograms to be multiplexed at the same location. Multiplexed digital image patterns can be used to store information that is relatively difficult to replicate. This can advantageously make such a article of this invention relatively difficult to counterfeit.
[0028] The article of this invention could be small (e.g. stamp sized) or large (e.g. book size). Additionally, while article of this invention is in the form of a rectangle, a holographic article of this invention in accordance with the present invention can be any shape including, without limitation, a square, circle, triangle or toroid. Deterring counterfeiting would be important for applications such as driver's licenses, credit cards, ID cards, monetary currency, or content distribution.
[0029] Digital data is preferably contained in the volume of a holographic material layer. Additional holographic data can include, without limitation, images of the user; fingerprint, voice or other user biometric data; and/or holographic patterns to make the article difficult to copy. In addition, the article could have presentation data in a presentation/security section of the article. The presentation data can include, without limitation, a company name, company logo, user name, and user contact information. Some or all of this information can also be included in a holographic material layer in non-holographic form. For example, without limitation, a company logo or user contact information could be included in non-holographic form while other presentation/security information could be included in holographic form.
[0030] As used herein, a volume hologram indicates that an index of refraction change exists in the volume of the holographic material layer as opposed to existing merely at the surface of the holographic layer, as disclosed in Grot et al. discussed in the background section. Volume holographic data stored in holographic material layer can have a higher refractive efficiency than holograms placed on the surface of a foil (such as surface relief or embossed holograms). A surface relief hologram typically can refract only up to about 10% of the light incident on the hologram. However, a hologram in a translucent holographic material in the article of this invention can diffract up to 100% of the light incident thereon. As such, a hologram of the article of this invention can be relatively more visible and brighter to the eye that a surface hologram when the thickness of the volume holographic material is chosen correctly. Additionally, the images may be two dimensional or three dimensional holograms and more images can be recorded in a holographic material layer than in a surface hologram. For example, it is possible to multiplex 20-50 holograms with 100% efficiency each in a volume material while multiplexing that many in a surface relief fashion would typically result in efficiencies of approximately 10 −4 (that is, 0.01% of the light incident on the multiplexed surface relief holograms would be refracted). This would result in a hologram which would be relatively difficult to view. Recording of holograms in a holographic material such as a holographic material layer is well known to those skilled in the art and discussed, for example, in Vacca. Additionally, presentation/security data could be single or multiplexed holograms. If holograms are multiplexed digital image patterns, the data would be relatively difficult to reproduce. Specifically, as discussed in Curtis et al., using phase encoding to store an image requires highly precise matching of recording conditions to detect the image signal. As such, recording using phase encoding patterns can facilitate verification of article authenticity.
[0031] A method of making a holographic multi-layer structure having multiple layers in accordance with the present invention is disclosed in U.S. Pat. No. 5,932,045 entitled “Method for Fabricating a Multilayer Optical Article” issued to Campbell et al. on Aug. 3, 1999 (“Campbell”) which is hereby incorporated by reference herein in its entirety. The multi-layer structure could have protective layer and substrate layer affixed to a holder by vacuum, electrostatic force, magnetic attraction or otherwise. A holographic material layer could be placed between the protective layer and the substrate layer and then cured.
[0032] It is possible for the adherent to be photocurable or otherwise curable, e.g., radiation or chemical curable. Heat may be used to accelerate a radiation cure. When using the above method, it is preferable for the adherent to be a material that undergoes a phase transformation, e.g., liquid to solid, to attain a required adherence. As used herein, the terms cure and curable are intended to encompass materials that gel or solidify by any such methods. Photocurable adherents include materials that cure upon exposure to any of a variety of wavelengths, including visible light, UV light, and x-rays. It is also possible to use adherents that are curable by electron or particle beams. Useful adherents include photocurable adherents that are photosensitive, the term photosensitive meaning a material that changes its physical and/or chemical characteristics in response to exposure to a light source (e.g., selective, localized exposure). Such photosensitive adherents include but are not limited to certain photosensitized acrylates and vinyl monomers. Photosensitive adherents are useful because they act as both an adherent and a recording media.
[0033] It is possible for the adherent to comprise additives such as adherence-promoters, photoinitiators, absorptive materials, or polarizers. The thickness of the post-cure adherent will vary depending on several factors, including the adherent used, the method of application, the amount of adherent applied, and force exerted on the adherent by the substrates. Different thickness will be desired for different applications. Preferably, however, a holographic material layer is a volume layer with a thickness of 5 microns to 6 mm. The level of cure needed is determined by the particular adherent used and by the force required to maintain a substrate or multilayer article with the encased optical article in the position imparted by the holder or holders. For materials that are photocurable, heat curable, or chemically curable, it is possible for suitable cures to range from a few percent to 100%.
[0034] Additionally, in the method described above, a holographic material layer could be formed by mixing a matrix precursor and a photoactive monomer. Such a holographic medium is disclosed in U.S. Pat. No. 6,103,454 which is hereby incorporated in its entirety by reference. One advantage of using this type of media is that the article of this invention can be made to have relatively good transmitted wavefront quality (that is, the article of this invention looks optically flat). Specifically, using the method and media discussed above, a holographic article in accordance with the present invention, which is an article of this invention, can easily be made to have a reflected or transmitted optical flatness which exceeds λ/2 per centimeter squared at a wavelength of 780 nm measured interfermetrically. Transmitted optical flatness is a measure of the deviation, from a predetermined profile, of an optical path length through an optical article. Such a measure is well known to those skilled in the art and discussed, for example, in Campbell et al., which has been incorporated by reference. Such optical flatness can advantageously make the article of this invention relatively high performance and relatively simple. In particular, holograms can be recorded in a holographic material layer at a relatively high density and at a relatively high signal to noise ratio. Additionally, data can be transferred both to and from a holographic article of this invention having the cited flatness at relatively high transfer rates. The above described method of fabricating a holographic article in accordance with the present invention can also reduce wedge (increasing or decreasing thickness in a direction parallel to the surface of the article of this invention). By these methods the wedge of the entire article of this invention can be made to be less than a 20 wavelengths as measured interferometrically at 780 nm. That is, the thickness over the entire surface of the article of this invention will not vary more that 20 wavelengths when measured using a 780 nm light beam. Such a measure is well known to those skilled in the art and discussed, for example, in Campbell et al., which has been incorporated by reference.
[0035] Another medium from which a holographic material layer may be fabricated can be a member of a class described and claimed in U.S. Pat. No. 5,719,691 to Colvin et al. for a “Photo Recording Medium” which is hereby incorporated by reference herein in its entirety. Briefly, it is an all-acrylate composition constituted of an oligomeric matrix and dispersed monomer, which together, under the influence of a photoinitiator, respond to illumination by local polymerization to increase refractive index. The specific composition is:
Component Percent by Weight isobornyl acrylate 37.23 oligomeric urethane acrylate 55.84 photoinitiator 5.96 tertiary butyl hydroperoxide 0.97
[0036] However, the medium of a holographic material layer could also be any acrylate-based photopolymer, or other suitable holographic medium such as, without limitation, a film containing dispersed silver halide particles or a free-standing LiNbO3 crystal. As discussed above, exposing holographic storage or presentation/security data into a holographic material layer is well understood by those skilled in the art.
[0037] Protective layer and substrate layer of the article of this invention can be fabricated from either the same or different materials. The materials from which protective layer and substrate layer can be formed include, without limitation, ceramics (including glasses), silicon, metals, polycarbonate, polymethylmethacrylate, or acrylic, or plastics. In addition to self supporting substrates such as glass plates, it is possible for the substrate to be a polymeric material that is sprayed onto a holder, a thin polymer film such as Mylar®, or a polymer sheet such as polycarbonate. It is also considered that a polymeric material or film be combined with a self supporting material such as a glass plate to form a single substrate. Either or both protective layer and substrate layer may be an optical article such as, with limitation, a polarizer, half or quarter wave plate, neutral density filter, birefrengement plate, or diffractive optic.
[0038] The article could also have a laminating layer that is preferably transparent and can be made from the same material as the protective layer discussed above. The article could have a non-holographic layer that can be fabricated from any suitable material depending upon the nature of the non-holographic data contained therein. For example, without limitation, if the non-holographic layer could be a photograph, the fabrication material would be a photographic or printed paper or emulsion. If the non-holographic layer is text data or a printed symbol, the fabrication material could be printed paper or plastic.
[0039] The card, patch, merchandise or banknote shaped article of the preferred embodiment can be manufactured in substantially the same way as the article of this invention discussed above. In particular, the substrate layer, holographic media layer and protective layer can be laminated. Then, the non-holographic layer can be placed on or in the protective layer as is well understood by those skilled in the art and the laminating layer can be placed thereover, as is also well understood by those skilled in the art. Additional details are available in U.S. Pat. No. 6,695,213, which is incorporated herein by reference.
[0040] The security and presentation holograms could be recorded or mastered at time of fabrication of the article of this invention or the user could use the corresponding writer to recorded user specific holograms into these areas of the article of this invention. These user recorded holograms could be either machine readable or visible to the eye.
[0041] In order to produce a holographic security foil, a visible image and/or a concealed (latent) image and/or a data pattern are designed. If optical methods are used to construct initial holographic master, then masks or models of each constituent portion of the final hologram are constructed, and an optical hologram is exposed which combines all of the desired imagery in a single holographic master. This master is composed of volume index of refraction structures called fringe patterns that reconstruct the desired images upon illumination with light of the appropriate properties
[0042] One embodiment of this invention relates to a particular design approach for volume (non surface relief) security holograms that enables data and/or images to be stored which are entirely invisible when viewed by the human eye. In addition, these covert data pages and/or covert images are more difficult to detect and to reproduce than those produced through non-volumetric holographic data storage. These highly covert data and images can be multiplexed with a visible holographic image, and can also be multiplexed with any other security hologram data storage or imaging approach employed currently. A particular class of holograms with a reflective backing allows for customized data to be stored in situ. This customization can improve the security of the product (CD, DVD, clothing, etc) or document by combining the data stored with other security features or information such as serial number, manufacturer, etc. Examples of systems that can read and write holograms into polymer films are given.
[0043] Preferably, the construction of any material arrangement of the article of this invention comprises of one or more layers of photosensitive media to accomplish volume holographic data storage for any security or authenticity verification applications. In one embodiment, a photosensitive medium is applied in a single (or multiplicity of optically thick or thin (>5 micron) layer(s) upon a substrate or within a material stack. A single (or multiplicity of volume holographic fringe pattern(s) can be recorded in this (these) layer(s) using any one of several well-known multiplexing techniques (angle multiplexing, shift multiplexing, correlation multiplexing, etc.). The material arrangement that contains the photosensitive material can be constructed such that the photosensitive medium is located above an optically reflecting material, or above an optically transparent material or above an optically absorptive material.
[0044] The material arrangement could comprise of one or more layers of photosensitive media greater than 5 microns in thickness to accomplish volume holographic data or image storage for any security or authenticity verification applications. The one or more of the layers of the photosensitive material(s) could comprise a formulation such as those described in U.S. patent application Ser. Nos. 10/146,115, 10/166,172 and 10/207,158 which are incorporated herein by reference. The one or more of the layers of the photosensitive material(s) could be positioned above an optically reflective surface, above an optically transmissive surface or above an optically absorptive surface.
[0045] For a photosensitive medium above a reflective surface, the angle between the writing beams can have any value between zero and 180, and the orientation between the plane of data modulation and the plane of the recording medium can be any value between −90 and 90 degrees. For a photosensitive medium above a transmissive surface, the angle between the writing beams can have any value between zero and 360, and the orientation between the plane of data modulation and the plane of the recording medium can be any value between −90 and 90 degrees. The optical system required to reconstruct the original data pattern from volume holograms will be more complicated for cases of non-zero values of the orientation between the data-modulated plane and the recording medium plane than it will be for cases in which the data-modulation plane is parallel to the hologram recording plane.
[0046] To combine the covert data with a visible image can be desirable to hide the data more effectively. This can be done by placing normal artwork under the transmissive polymer, placed a prerecorded holographic film on top of a foil hologram, and or recording another strong visible hologram into the same polymer film as the data hologram. By recording the data at angles or with wavelengths that are not used for the visible hologram and making the diffraction efficiency weak the data can be made more covert. Also by using data pixels or bars that are fairly small (10-100 microns) the data will be harder to detect by eye. Recording the data hologram in the polymer film outside of the image plane also makes the data more covert. This covertness is limited by the surface quality of the polymer film.
[0047] The use of the optical writing and reading systems described in this disclosure for writing security holograms are similar to those contemplated for holographic data storage. The combination of data storage and allowing for in situ recording onto holographic patches, stripes, foils, windows for use in security of products and documents is novel. These holographic recording materials can be attached to documents or products or integrated into the actual structure, for example as in some plastic currency in use today, layered into/onto CD or DVD, or plastic credit cards. The systems shown below use transmissive optical elements to image but reflective imaging systems are equally suitable.
[0048] The data to be stored can be arranged for readout in a line, bit by bit, bit by bit but parallel independent streams, barcode, or pagewise. Examples include: storing the data in a fashion similar to CD or DVD bit patterns holographically, reading out a line of bar codes in parallel with a line detector, or a 2D data pattern readout out in parallel by imaging or line by line by using a line detector and moving the hologram in with respect to the optical system. The data would have error correction, channel modulation and timing/servo marks recording into the hologram with the data. A single layer of data can be stored or multiple virtual layers can be stored by using volume multiplexing techniques.
[0049] One embodiment of a reader system is shown in FIG. 1 , which depicts a reader system with spherical optics and a 2D parallel output. This approach requires stopping (or slowing) the hologram briefly to capture a 2D image on the output camera. As in all of these designs, the afocal imaging telescope could be replaced with a single lens element, if image quality and positioning tolerances are found to be acceptable. If magnification is required for pixel-matching between the input and output planes, the telescope approach is likely to be required. The 2D output approach will probably have tighter rotational requirements on the detector array (camera) than would be the case using a linear array.
[0050] A second embodiment of a reader system is shown in FIG. 2 , which shows a reader system with spherical optics and a 1D linear output. This approach requires continuous or stepped motion of the input hologram past the center of the illuminating beam. As in all of these designs, the afocal imaging telescope could be replaced with a single lens element, if image quality and positioning tolerances are found to be acceptable. If magnification is required for pixel-matching between the input and output planes, the telescope approach is likely to be required. This approach is not as light efficient as using a line focus to illuminate the hologram, but with the correct sizing of the collimated beam, it could be acceptable. The hologram might be pressed against roller to make flat as moved across reader.
[0051] A third embodiment of a reader system is shown in FIG. 3 , which shows a reader system with spherical and cylindrical optics and a 1D linear output. This approach requires continuous or stepped motion of the input hologram past the center of the illuminating beam. As in all of these designs, the afocal imaging telescope could be replaced with a single lens element, if image quality and positioning tolerances are found to be acceptable. If magnification is required for pixel-matching between the input and output planes, the telescope approach is likely to be required. This approach is very light efficient.
[0052] The reader system could also be a barcode reader or a page-code reader. The patents publications that are incorporated herein by reference include U.S. Pat. No. 6,482,551, U.S. Pat. No. 5,932,045, U.S. Pat. No. 5,306,899, and Japanese J. Appl. Phys. Vol. 42 (2003) pp 976-980.
[0053] The foregoing descriptions of specific embodiments of the present invention have been presented for purposes of illustration and description. They are not intended to be exhaustive or to limit the invention to the precise forms disclosed, and it should be understood that many modifications and variations are possible in light of the above teaching. 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 and various embodiments with various modifications as are suited to the particular use contemplated. Many other variations are also to be considered within the scope of the present invention.
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Disclosed is an article having a holographic recording medium having digital data that cannot be seen by human eye, wherein the holographic recording medium is a holographic material that records volume holograms that permit authentication of the article and the holographic material is attached to or part of the article. Also disclosed is a method of authentication of the article.
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FIELD AND BACKGROUND OF THE INVENTION
This invention relates to a thermo-luminescent material. More particularly, this invention is concerned with a highly sensitive composition based on crystalline lithium fluoride, which composition exhibits an excellent thermo-luminescence property and is suitable for use in radiation dosimetry.
DESCRIPTION OF THE PRIOR ART
As dosimetric elements based on thermo-luminescent materials have been hitherto employed in practice calcium fluoride(CaF 2 ), calcium sulfate(CaSO 4 ), lithium fluoride (LiF), lithium borate (Li 2 B 4 O 7 ) and the like. Among these, lithium fluoride has been regarded as most suitable for medical use as in man because of its following advantageous characteristics:
1. It is almost equivalent to the tissue of human body.
2. It shows less dependence on energy.
3. It shows little retrogression of the accumulated dose at temperatures around body temperature.
4. It is not influenced by the temperature at the time of irradiation, even when it is close to body temperature.
The lithium fluoride, however, produces less amount of light emission from thermo-luminescence. As a consequence its sensitivity in dosimetry with radioactive isotopes is considerably low in comparison with that of calcium derivatives, with the result that the presicion of measurement becomes low at low doses and that the detection sensitivity(lower detection limit) drops to several milliroentgen, it thus being impossible to measure doses lower than the lower limit.
SUMMARY OF THE INVENTION
Extensive studies have therefore been made with a view to eliminating such drawbacks involved in the use of lithium fluoride as mentioned above and it has now been found that addition thereto of certain metals or non-metals leads to a significant difference in its intensifying activity. The present invention has been accomplished on the basis of this finding. Thus in accordance with the present invention, the amount of light emission by thermo-luminescence can be markedly increased without adversely influencing the advantageous characteristics inherent to lithium fluoride, and the low measurement sensitivity in dosimetry at low doses, which has been hitherto regarded as the greatest drawback involved in the use of lithium fluoride, can be improved to a remarkable extent.
More specifically, the present invention provides a thermo-luminescent material capable of emitting an intense light as of such intensity as is higher than that of previous materials (in which magnesium alone is used as luminescent center) by factors of several tens to one hundred. The thermo-luminescent material in accordance with the present invention comprises crystals or powdery crystallites of lithium fluoride having present therein (A) luminescent center consisting of magnesium in combination with at least one element or more selected from the elemental group consisting of calcium strontium, copper, silver, and gold, aluminum and gallium and (B) sensitizer therefor consisting of at least one element or more selected from the non-metallic elemental group consisting of boron, carbon, silicon, phosphorus, sulfur, arsenic, selenium and tellurium.
The various features of novelty which characterize the invention are pointed out with particularity in the claims annexed to and forming a part of this disclosure. For a better understanding of the invention, its advantages and specific objects attained by its uses, reference should be had to the accompanying drawings and descriptive matter in which there are illustrated preferred embodiments of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
In the drawings:
FIG. 1 shows the difference in the amount of light emission by thermo-luminescence between the prior art product, lithium fluoride-magnesium, and the product of the invention, lithium fluoride-magnesium-copper-phophorus;
FIG. 3 shows the relationship between the dose of irradiation and the amount of light emission; and
FIG. 3 shows an emission spectrum of the product of the invention, lithium fluoride-magnesium-copper-phosphorus.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The thermo-luminescent material of the invention may be produced by subjecting powdered lithium fluoride containing activators and the like to heat treatment in an inert gas stream with the use of any conventional tubular electric furnace. The resulting baked product then may be comminuted until the desired particle size is reached, and washed with acid and then water and dried into the finished product. The amounts of the activators to lithium fluoride are preferably in the range of from 0.05 to 1.0 mol%, based on the lithium fluoride, for the main activator magnesium and also for the activator selected from the elemental group consisting of calcium strontium, copper, silver, gold, aluminum and gallium, For the sensitizing additive selected from the non-metallic group consisting of boron, carbon, silicon, phosphorus, sulfur, arsenic, selenium and tellurium, the preferred proportion based on the lithium fluoride is, although depending on the kind of the specific element, preferably in the range of from about 0.1 to 5.0 mol%.
Conditions for the heat treatment depend to some extent on the size of the furnace, that of the crucible, and other factors. In general, however, it is preferred to carry out the heat treatment at temperatures in the range of from 700° to 1,100° C. for periods of time in the range of from 30 minutes to 3 hours. The acid washing and the water washing are incorporated for the purpose of removing from lithium fluoride residual excesses and decomposition products of the activators which are not taken up into the crystal lattice of the lithium fluoride.
In the following are shown the radiation characteristics of the thermo-luminescent material of the invention on the basis of some test results. The glow curve, as shown in FIG. 1, shows the glow peak at about 200° C., thus having a convenient pattern for use in dosimetry. As regards the amount of thermo-luminescence, the product of the invention, for example, lithium fluoride-magnesium-copper with boron (a non-metal of Group 3A in the Periodic Table) added is found to produce 20-30 times larger amount of light emission in comparison with the prior art product, lithium fluoride-magnesium. Similarly, the addition of carbon or silicon(non-metals of Group 4A) give rise to an increase in the amount of light emission over the prior art product by factors of from about 30 to about 40. Furthermore, the addition of phosphorus or arsenic(non-metals of Group 5A) brings about an increase in the amount of light emission up to 80-100 times and that of sulfur, selenium or tellurium(non-metals of Group 6A) up to 60-70 times. Moreover, the use of such non-metallic elements in combination causes an increase in the amount of light emission by factors of 20-40.
As another embodiment of the invention there may be mentioned lithium fluoride-magnesium-phosphorus to which has been added calcium belonging to Group 2A in the same way as magnesium. In this case can be attained an increase in the amount of light emission over the prior art product by a factor of 20-30. Also in the case of addition of copper, silver or gold (metals of Group 1B) an increase in the amount of light emission by factors of about 80-100 is found to be reached. In the case of addition of aluminum or gallium (metals of Group 3A) brings about an increase in the amount of light emission by factors of about 10.
As shown in FIG. 2, the dose of irradiation shows a good linear relationship with the amount of thermo-luminescence over a wide dose range of from 0.1 milliroentgen up to 10,000 roentgens, which indicates that as a result of the increase in sensitivity in accordance with the present invention low doses in the order of 0.1 milliroentgen can be measured well.
The thermo-luminescent material of the present invention shows an emission spectrum as shown in FIG. 3.
The thermo-luminescent material of the invention has an effective atomic number of about 8.13, which is close to that of the living tissue(7.16), showing at the same time little dependence on energy. In addition it exhibits little the phenomenon of retrogression. Thus there is little difference from the prior art lithium fluoride product in these respects.
As is apparent from the above-mentioned characteristics, the thermo-luminescent material in accordance with the present invention eliminates the drawbacks involved in the use of lithium fluoride and is comparable to the prior art high sensitivity thermo-luminescent materials based on calcium or the like. Thus, it finds wide use not only in medicine, but also in general radiation dosimetry.
The present invention is explained in more detail by the following specific examples:
EXAMPLE 1
______________________________________Lithium fluoride (LiF)Magnesium fluoride (MgF.sub.2) 0.2 mol %Cupric chloride (CuCl.sub.2) 0.05 mol %Ammonium primary phosphate (NH.sub.4 H.sub.2 PO.sub.4) 0.46 mol %______________________________________
The above-mentioned powdered raw materials of lithium fluoride, magnesium, copper and phophorus are mixed in the proportions also mentioned above, placed in a platinum crucible. The cruicible is placed in a tubular electric furnace, heated at a temperature of 1,050° C. for 30 minutes under a nitrogen stream and cooled down to normal temperature. The contents are removed from the crucible, milled into a particle size of 90-200 mesh, washed with about 1N hydrochloric acid and then distilled water and dried.
EXAMPLE 2
______________________________________Lithium fluoride (LiF)Magnesium chloride (MgCl.sub.2) 0.2 mol %Cupric sulfate (CuSO.sub.4) 0.05 mol %Silicon dioxide (SiO.sub.2) 0.86 mol %______________________________________
The above-mentioned magnesium chloride is dissolved in distilled water and mixed with thorough stirring with a powder mixture of silicon dioxide and lithium fluoride in the amounts mentioned above. The resulting mixture is dried to obtain a powder mixture again. The powder mixture is placed in a platinum crucible and subjected, in the same way as in Example 1, to the 30-minute heat treatment at a temperature of 1,050° C. in an electric furnace.
The contents are discharged from the crucible and screened so that particles of particle size 90-200 mesh are obtained. The particles are charged with 1N hydrochloric acid and the mixture is boiled for several minutes then washed with distilled water until no chloride ions are detected, and finally dried.
EXAMPLE 3
______________________________________Lithium fluoride (LiF)Magnesium fluoride (MgF.sub.2) 0.2 mol %Silver chloride (AgCl) 0.05 mol %Boric acid (H.sub.3 BO.sub.4) 0.84 mol %______________________________________ fluoride, magnesium, raw materials of lithium boron and silver are mixed together in the proportions indicated above in the form of powder as in Example 1. The powder mixture is subjected, in the same manner as in Example 1, to heat treatment, removed from the crucible and subjected, again in the same manner as in Example 1, to washing with acid and water, and dried.
EXAMPLE 4
______________________________________Lithium fluoride (LiF)Magnesium fluoride (MgF.sub.2) 0.2 mol %Aluminum oxide (Al.sub.2 O.sub.3) 0.05 mol %Tellurium oxide (TeO.sub.2) 0.80 mol %______________________________________
The powdered raw materials are mixed together and subjected, in the same manner as in Example 1, to heat treatment, milling, acid washing and water washing, and dried.
EXAMPLE 5
______________________________________Lithium fluoride (LiF)Magnesium fluoride (MgF.sub.2) 0.2 mol %Calcium oxide (CaO) 0.4 mol %Silicon dioxide (SiO.sub.2) 0.86 mol %Ammonium primary phosphate (NH.sub.4 H.sub.2 PO.sub.4) 0.46 mol %______________________________________
The powdered raw materials are mixed together and subjected in the same manner as in Example 1, to heat treatment, milling, acid washing and water washing, and dried.
EXAMPLE 6
______________________________________Lithium fluoride (LiF)Magnesium fluroide (MgF.sub.2) 0.2 mol %Cupric chloride (CuCl.sub.2 ) 0.05 mol %Tellurium oxide (TeO.sub.2) 0.80 mol %______________________________________
The above-mentioned raw materials are processed in the same way as in Example 1.
It is to be understood that many other combinations of raw materials other than those employed in the above-mentioned Examples may be treated in the same manner as in Examples to obtain thermo-luminescent materials.
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A lithium fluoride thermo-luminescent material with increased sensitivity, which comprises crystals or powdery crystallites of lithium fluoride having present therein (A) luminescent center consisting of magnesium and at least one element or more selected from the elemental group consisting of copper, silver, and gold, and (B) sensitizer therefor consisting of at least one element or more selected from the elemental group consisting of carbon, phosphorus, sulfur, arsenic, selenium and tellurium.
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FIELD OF THE INVENTION
[0001] The present invention relates to a modular construction system of molding with multi-perforated arch centering for concrete or reinforced concrete of direct application to the construction industry, for the construction of all types of real estate properties. More specifically the modular construction system of permanent formwork molding refers to a set of elements including: first polymeric flat structural components, second, corner components; third flat connecting components, fourth: panel-shaped components; each component of the modular system includes longitudinally at the remaining end of one rail edge, at the remaining end of the edge at least one rail, the flat components across the width of its longitudinal surface have at least one longitudinal rail for coupling flat connectors, for assembly of the rail system and against rails of the structural components, which are coupled and locked together slidable to each other, successively until forming a mold structure with permanent arch centering with hollow interconnected interior cavities and multiperforated exposed faces in the hollow cavities where concrete is spread, on the exposed multiperforated faces concrete springs and is impregnated, thus covering the permanent arch centering and generating a new texture to the surface. This new surface can receive any type of finish.
BACKGROUND OF THE INVENTION
[0002] Currently in the construction industry there are a variety of materials and processes for construction of buildings. The most developed areas are prefabricated modular systems and materials, as these are useful anywhere where you need to build, whether it is a small or a large building. These materials and systems offer numerous solutions for businesses and individuals, because the works can be completed in very short periods of time, with greater control of work, cleaner works, safe and durable works, besides these materials are easy to assemble and the labor used is not specialized or regional.
[0003] Currently have been developed various components and modular systems for these purposes, for example there are some panel systems of rigid PVC and foamed PVC panel systems, systems with flat components, systems with angular components, extruded PVC systems, with elements to be continuously assembled together. These systems are complemented by structural reinforcement elements such as metal columns and rods for the construction of all types of outer walls, inner wall partitions, contemplating the formation of walls in corners with all these elements for different types of buildings.
[0004] For example, the description of the U.S. Pat. No. 5,608,999 (MX 202025), describes the use of a series of flat thermoplastic structural components and thermoplastic corner structural components, where some components are locked slidably and releasably together to form continuous wall structure with hollow cells, where these cells receive poured concrete internal and the surface finish is always smooth and plastic. The structural system components of the system of Bernard Mc Namara as has been disclosed include flat connectors, flat caps and corner angles, prefabricated and extruded in rigid PVC, so they can be assembled on-site, with unskilled labor and short periods of time.
[0005] A disadvantage of thermoplastic structural system components of the Bernard McNamara system, to assemble a wall structure it is required a lot of individual elements for assembly of the system, consequently before such manipulation of elements significantly it is increased the time of assembly and construction, in addition the final surface finish will always be smooth and plastic.
[0006] The patent description No. U.S. Pat. No. 5,729,944 discloses a building constructed of extruded thermoplastic structural components, these components include hollow panels, hollow connectors, hollow beams and adapters. For the assembly of the system the extruded components are locked over the edge together continuously to form vertical walls and the roof of the building. Each wall structural component is hollow, is made from PVC plastic material, and formed of spaced inner and outer walls connected by transverse entanglements that form internal cells, this essentially appears as a mold into which concrete is poured to form outer and inner wall faces with smooth finish and plastic.
[0007] A disadvantage of the system of Vittorio De Zen is that the thermoplastic hollow panel is formed at both ends of the edge for engaging and interlocking with a male member, for assembly between panels to build a continuous flat wall, it is always required a connector between panels, without these connectors is not possible to assemble the panels, in addition the resulting final surface will be smooth and plastic.
[0008] The Mexican Patent Application PCT/MX2005/000012 with International Publication Number WO 2005/098158 A1 discloses and describes a panel structure with coupling means, for prefabricated buildings, the panel structure of rectangular longitudinal shape with internal individual cavities not interconnected, with ease of assembly and engagement with each other, besides the complementary structural elements such as steel columns are inserted and engage only in the cavities formed between the panel structure assemblies against the panel structure, such that concrete or some other material is poured into the internal cavities, forming a wall structure with plastic surface finish for the construction of buildings.
[0009] A major disadvantage of this panel structure system with coupling means, for prefabricated buildings, is that there is no internal communication between the elements and their internal cavities in the structure of vertical wall, thus reducing the structural capabilities of the system and when the concrete is poured it is not obtained a final continuous monolithic structure, to achieve structural stability the system uses steel columns of noncommercial structural shapes, so this greatly increases manufacturing costs and project costs, and besides the surface finish will always be smooth and plastic.
[0010] U.S. Pat. No. 7,628,570 B2 US discloses a modular retaining wall where the wall is at least partially below the surface, where the surface may be land-based or water-based; the walls are compounds polygonal modules with open and closed channels disposed therein, in addition to components as hollow profiles, flat profiles, module connectors, hollow profiles and corner connectors and hollow adapters. The wall modules are fastened together by respective coupling and fastening closures so that connectivity is provided between the modules, however it retains the ability for the liquid to pass through, being always smooth surface finish and plastic.
[0011] A disadvantage of the modular system of John Davidsaver and Acott Yeany is that in forming intermediate configurations walls and dividers, nuts and bolts are required, and this increases the time of building and the apparently low costs for these items, but they are at large scale reflected in longer periods of construction and project costs; however, the final surface finish is always smooth and plastic.
[0012] Due to the above, there is in the market a need for a modular construction system being more versatile, handy and of a smaller scale, easy assembly and rapid construction for use in the construction industry, for the building of any kind of construction, which solves the disadvantages mentioned and that is functional over existing systems. The present invention aims to provide a solution to this gap detected, it would be of great relevance in the area of materials prefabricated construction industry.
OBJECTIVES
[0013] The present invention is generally intended to provide a modular construction system multi-perforated with permanent formwork for reinforced concrete, which is assembled and coupled structurally with panels and components easily and quickly constructed.
[0014] Another objective of the present invention is to provide a permanent construction system with permanent arch centering, multi-perforated for reinforced concrete, with hollow cavities interconnected to function as mold of permanent arch centering formwork to the concrete poured into the cavities by the multiperforated surfaces with anterior and posterior concrete “outbreak” hiding permanently the formwork and generating a new texture on the surface, which can receive any additional finish.
[0015] Another object of the invention is to provide a modular building system of permanent formwork for reinforced multi-perforated concrete, where the final specific surface is exposed and can receive any type of finish.
[0016] Another object of the invention to provide a modular construction system multi-perforated permanent formwork for reinforced concrete, where one of the exposed end surfaces of the concrete wall is able to receive any type of finish and the remaining wall surface has smooth and plastic finish.
[0017] Another objective of the invention is to provide a modular molding system of permanent multiperforated formwork for reinforced concrete where panels and hollow components are molds for pouring concrete, which support the weight and the expansion of the concrete.
[0018] Another important objective is to make available a panel and modular structural multi-perforated components with coupling means easily and stably assembled together, eliminating the use of nuts, bolts, welding, bolts, wedges, and stay bolts.
[0019] Another object of the invention is to provide a modular panel system with prefabricated structural multi-perforated components for an assisted self construction model where labor manual labor can be regional and unskilled.
[0020] Another object of the invention is to make available a modular construction system of permanent formwork multiperforated for reinforced concrete being resistant of low molecular weight, thermo acoustic, minimizing energy consumption and building timing.
[0021] Another object of the invention is to make available a modular construction system of permanent formwork for reinforced concrete multi-perforated where doors, windows, electrical, hydraulic, sanitary facilities are compatible with the system.
[0022] A further object of the present invention to provide a prefabricated modular multi-perforated polymeric components, that can be implemented in all kinds of constructions maintaining the character of being lightweight, easy to maneuver, easy to transport and easy to assemble.
[0023] A further object of the present invention to provide a modular construction system of permanent formwork for reinforced concrete where modules can be trimmed and sectioned according to the requirements and needs of the construction project.
[0024] Another object of the invention is to provide a modular construction system of permanent multiperforated formwork for reinforced concrete that when assembled to act as an integrated structure but can be reinforced as needed.
[0025] Finally another object of the invention is to make available a modular construction system multi-perforated permanent formwork for reinforced concrete where prefabricated components are extruded and high strength polymeric materials involving large-scale production.
DESCRIPTION OF THE INVENTION
[0026] The elements of the modular construction system of permanent formwork multi-perforated for reinforced concrete in all its forms and its plurality of arrays are formed first by modular flat profiles multi-perforated characterized by comprising a multi-perforated longitudinal surface at the ends of perpendicular edge to the longitudinal multi-perforated surface with a longitudinal extension all along rail geometrically defined as a female element, the remaining end on the longitudinal rail as male member, as coupling means, and interlocking along the width of the longitudinal surface comprises a plurality multi-perforated longitudinal rails of T-shaped connectors for flat couplings.
[0027] Second: a modular plug multi-perforated hollow with corners characterized by comprising two perpendicular longitudinal elongated faces bonded together with cut cores distributed longitudinally, these attached to a semicircular longitudinal surface multi-perforated, said modular connector multi-perforated in one of the perpendicular longitudinal faces has integrated two rails of defined geometric shape as the female member and on the remaining face has two rails integrated geometrically defined as male element, such as engagement and interlocking means.
[0028] Third: a flat modular connector characterized by comprising a longitudinal surface with sections cut cores strategically distributed longitudinally, in addition to comprising at both ends of the longitudinal edge a U-shaped rail with extended inward edges as coupling means. Also a modular flat connector rectangular multi-perforated characterized by comprising a multi-perforated front wall, a rear multi-perforated wall and longitudinal furring strips with sections of cut cores longitudinally and strategically distributed perpendicular to the multiperforated walls, said modular connectors in a rib has two rails integrated defined geometrically as the female member on the remaining there are two rails integrated, geometrically defined as male element, such as engagement means, and interlocking crimp.
[0029] Fourth: One Multi-perforated modular panel characterized by comprising a rectangular configuration, a longitudinal multi-perforated front wall, a longitudinal multi-perforated rear wall, a plurality of longitudinal ribs with core cut sections strategically distributed longitudinally, forming between these, interconnected rectangular cavities, at one end of multi-perforated modular panel on the rib has an integrated two longitudinal rails defined geometrically as the female member on the remaining end rib has an integrated two longitudinal rails defined geometrically as the male element, such as engagement, interlocking and crimping means.
[0030] The assembly of modular construction system of permanent formwork multi-perforated for reinforced concrete consists of the continuous and subsequent coupling of the components of the modular construction system, where each component includes in at least one of its ends a male element and at the remaining end a female element; for the coupling between the elements, the rail with the male element is housed, is fitted and slides against the rail with the female element performing continuous and subsequent assembly of the components of the building system to form a structural configuration with permanent formwork molds multi-perforated with all interior hollow cavities communicated with each other and whose front and back walls of the mold are multiperforated permanent formwork.
[0031] In the cavities of the mold structure of permanent formwork can be poured concrete or other aggregate, through multiperforated surface the poured concrete will have the effect of “spring and impregnating the multiperforated surfaces” thus generating a new texture to the surface covering and hiding to the structure of permanent formwork mold. The permanent formwork covered by the concrete cover on its front and back faces are able to have any additional finishing either smooth, textured, etched or adding another material.
[0032] Walls obtained by the modular construction system of permanent formwork forming the building can be blind, comprise windows, doors, openings for air conditioning; since the plurality of arrangements between panels and thermoplastic elements interconnected internal cavities are formed, these allow you to place covertly to sight, electrical, voice, data wiring, water, sanitary facilities. Besides, you can structurally reinforce the system installing rods in the cavities or a commercial structural shape vertically or horizontally according to the needs of the construction project system.
[0033] The modular construction system of permanent formwork multiperforated for reinforced concrete is designed for construction and buildings of all kinds, where all components of the modular construction system can be manufactured, cut and sectioned according to the needs of the construction project.
[0034] The modular construction system of multiperforated permanent formwork for reinforced concrete configured and described provides structural properties because of being formed as a structural element in itself and comprise a solid and reinforced structure, increasing its capacities, mechanical strength, and is also easy to manufacture, easy to transport and maneuver, easy to install and can be used on any type of construction.
DESCRIPTION OF THE DRAWINGS
[0035] FIG. 1 schematically shows a perspective view of the modular flat multi-perforated profile with partially increased details illustrating the different types and arrangements of multi-perforated and partially enlarged details showing the female and male coupling means.
[0036] FIG. 2 shows a top plan view multi-perforated modular profile of FIG. 1 , with partially enlarged of the coupling means of female and male type.
[0037] FIG. 3 shows the perspective view of the modular corner connector profile with partially enlarged details illustrating the different types and arrangements of multi-perforated, and partially enlarged details showing the male and female coupling types.
[0038] FIG. 4 shows a top view of the modular profile multi-perforated corner connector of FIG. 3 with partially enlarged details showing the female and male coupling means.
[0039] FIG. 5 schematically shows a perspective view of a flat profile modular connector of the construction system.
[0040] FIG. 6 schematically shows the top view of the modular flat profile of FIG. 5 .
[0041] FIG. 7 shows the perspective view of the modular connector multi-perforated profile with partially enlarged details showing different types and arrangements of multi-perforated and partially enlarged details of the coupling means of female and male type.
[0042] FIG. 8 shows a top view of the modular connector multi-perforated flat profile of FIG. 7 with details partially enlarged of the female and male coupling means.
[0043] FIG. 9 shows the perspective view of the modular panel multi-perforated with partially enlarged details and arrangement of multi-perforated at their anterior and posterior surface, and partially enlarged details showing the female and male coupling means.
[0044] FIG. 10 shows schematically the top view of the modular multi-perforated panel of FIG. 9 with partially enlarged details of female and male couplings.
[0045] FIG. 11 shows the perspective view of a portion of assembly section of the mold structure multi-perforated permanent formwork, comprises components of flat profile and flat connecting components with partially enlarged drawings of the female and male coupling means. Also it shows the assembly of tongue and groove coupling means, wherein the male type is snapped, slid and locked against the female type element.
[0046] FIG. 12 shows the perspective view of a section of the assembly of permanent formwork mold comprises flat components, flat connectors and components panel-shaped components, with the partially enlarged details of FIG. 10 shows schematically the top view of the modular multi-perforated panel of FIG. 9 with partially enlarged female coupling means and male type details.
[0047] FIG. 13 is a perspective view of an assembly section of the mold structure of permanent formwork mold and comprises flat components pads connectors, panel components and corner shaped components, with partially enlarged details of dovetail type assembly coupling means, wherein the male type is snapped, slid and locked against the female type element.
[0048] FIG. 14 shows the perspective view of a section of the modular construction system assembly of permanent mold structure formwork for reinforced concrete, comprising flat structural components, flat connector components, corners components, panel-shaped components, elements of vertical and horizontal structural reinforcements, besides concrete poured into the hollow cavities, showing the behavior of the permanent concrete hiding the permanent multiperforated formwork in the front and back surfaces of the permanent formwork.
[0049] FIG. 15 schematically shows the perspective view of a portion of assembly section of the modular structure of a permanent multiperforated mold for reinforced concrete formwork modular construction system, comprising: flat structural components, flat connector components corner connector components, panel shaped components, commercial standards structural elements and reinforcements placed vertically and horizontally, poured concrete in the hollow cavities, showing in particular the behavior of the concrete in the rear face was multiperforated which hides the permanent formwork and displaying multiperforated front face of the permanent formwork which is smooth with plastic finish.
[0050] FIG. 16 shows the perspective view of a section of assembly of a mold structure permanent formwork of the modular construction system of permanent formwork multiperforated for reinforced concrete, comprising flat structural components, flat connector components, corner shaped connecting components, panel-shaped components, vertical and horizontal elements of structural reinforcements, thermoacoustic insulation cores, poured concrete in the hollow cavities, showing in particular the behavior of concrete in the faces with multiperforation.
[0051] FIG. 17 shows the perspective view of a portion of assembly mold structure permanent formwork of the modular construction system permanent formwork multiperforated for reinforced concrete comprising flat structural components, flat connector components, corner connectors components, panel shaped components, vertical and horizontal and structural elements and reinforcements, thermoacoustic insulation cores, poured concrete in the hollow cavities, the new texture generated on the surface and some of the different types of additional finishing that can receive the new texture.
DETAILED DESCRIPTION OF A PREFERRED EMBODIMENT
[0052] The characteristic details of the modular construction system of permanent formwork perforated for reinforced concrete are shown in the following illustrative description and accompanying drawings, serving the same reference signs to indicate the same parts.
[0053] As shown in FIGS. 1 and 2 , a flat support rail multiperforated 10 comprising an elongated longitudinal surface 11 multiperforated 15 this can be of different types 15 a, 15 b, 15 c, 15 d strategically distributed on the surface 11 , the ends perpendicular to the multi-edge surface 11 with a longitudinal extension all along rail geometrically defined as female element 13 may be of the 13 th or 13 b, the remaining end in the longitudinal rail such that plug 12 may be 12 a or 12 b of the type, such as coupling means, and interlocking crimp, the width of the multi-longitudinal surface 11 comprises a plurality of longitudinal T-shaped rails 14 to engage the flat plugs.
[0054] With reference to FIGS. 3 and 4 show a modular connector multiperforated corners profile 40 with hollow cavity 22 characterized by comprising two longitudinal elongated faces 23 interconnected with perpendicular cut longitudinally distributed plus 17 comprise two parallel longitudinal cores 31 eyebrows crossing to the surface 23 , an elongated longitudinal side semicircular 32 multiperforated 15 this can be of different types of multiperforated 15 a, 15 b, 15 c, 15 d, said multiperforated modular connector 40 in one of the perpendicular longitudinal sides 23 has an integrated two rails geometrically defined as female element 13 which may be of the type 13 a or 13 b, in the rest face 23 has two rails integrated geometrically defined as male element 12 which may be of the type 12 a or 12 b, such as means of coupling and interlocking crimp.
[0055] As shown in FIGS. 5 and 6 , a flat modular connector profile 20 characterized by comprising an elongated longitudinal surface 16 with sections of cores cut 17 longitudinally distributed strategically, eyebrows 31 parallel longitudinal crossing the surface 16 , plus comprise edge at both ends of coupling means, shaped longitudinal U-shaped rail with extended edges 18 inwards.
[0056] Referring to FIGS. 7 and 8 , a modular plug plane rectangular multiperforated 50 characterized by comprising a front wall 11 , a rear wall 11 , 15 which can both be multiperforated 15 a, 15 b, 15 c, 15 d on the surface distributed type 11 longitudinal ribs 21 sections cut 17 cores distributed longitudinally, the walls 11 and ribs 21 form a hollow cavity 22 , said flat modular connector multiperforated 50 in a rib 21 I have built two rails geometrically defined as female member 13 which may be of the type 13 a or 13 b , the remaining rib has two rails integrated geometrically defined as male element 12 which may be of the type 12 a or 12 b, such as means of coupling and interlocking crimp.
[0057] Referring to FIGS. 9 and 10 , a modular panel 30 multiperforated characterized by comprising a rectangular configuration, a front wall 19 with longitudinal multiperforated 15 , a rear wall 19 with longitudinal multiperforated 15 , which may be of the type 15 a, 15 b, 15 c , 15 d distributed strategically, a plurality of longitudinal ribs 21 sections cut longitudinally 17 cores distributed strategically, you also have 31 parallel longitudinal eyebrows crossing to the surface 21 , in the configuration of walls 19 and ribs 21 rectangular form hollow cavities 22 connected to one another, said modular panel 30 in a rib 21 has two rails integrated geometrically defined as female element 13 which may be of the type 13 a or 13 b, the remaining two rails integrated rib has geometrically defined as male element 12 which may be of the type 12 a or 12 b, such as coupling means, and interlocking crimp.
[0058] Referring to FIG. 11 , a section of assembly consists of six modular profiles multiperforated plates 10 , eighteen connector pads 20 and a modular connector plane multiperforated 50 , which when assembled is shown subsequently will form a mold structure of permanent formwork with cavities RHS 22 interconnected with multiperforated surfaces 15 , 17 cut type cores and assembly of the male elements 12 and female 13 .
[0059] Referring to FIG. 12 , a section formed by modular assembly profiles shown multiperforated plates 10 , 20 flat connectors, modular connectors multiperforated flat profiles 50 , panel-shaped components 30 which are subsequently to be assembled to form a mold structure permanent formwork with hollow rectangular cavities 22 interconnected with multiperforated surfaces 15 , 17 cut type cores and assembly of the male elements 13 and female 12 .
[0060] Referring to FIG. 13 , a section formed by modular assembly multiperforated profiles 10 is shown flat, modular connectors multiperforated corner profiles 40 , 20 flat connectors, modular connectors multiperforated flat profiles 50 , panel-shaped components 30 which when assembled will subsequently forming a mold structure with permanent formwork hollow rectangular cavities 22 interconnected with multiperforated surfaces 15 , 17 cut type cores and assembly of the male elements 13 and female 12 .
[0061] Referring to FIGS. 14 , 15 , 16 and 17 a section of the assembly mold structure multiperforated permanent formwork for reinforced concrete formed by the multi-perforated plates 10 , 20 flat profiles connectors, modular panels 30 multiperforated shown modular profiles, modular connectors multiperforated corner profiles 40 and 50 modular connectors multiperforated planes, which when assembled subsequently one after another, these system components give form to a mold structure permanent formwork for reinforced concrete hollow cavities 22 interconnected to each other, where front and back faces of this structure may be with multiperforated 15 , this mold structure permanent formwork generated in the assembly is reinforced with structural elements 24 can be vertically and horizontally, in addition to the alternative of adding cores thermo acoustic insulation 25 in the hollow cavities 22 , 34 then spreads concrete mold cavities in these permanent formwork, where for the concrete surfaces 15 multiperforated spread 34 “and will generate” a new texture to the surface 26 , covering and hiding the permanent mold structure formwork, this structure in its front and rear surfaces as the construction project can be on one side of the form 26 and the remaining side of the finish surface can be smooth plastic surfaces 27 . Specifically generated 26 were able to make any type of finish either smooth flattened type 26 , 29 generate a textured surface, attach other material 45 as additional finishing.
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The present invention relates to a modular construction system with molding formwork or permanent formwork for concrete or reinforced concrete industry aimed at building construction. It Incorporates a number of key elements: structural-elements for forming flat walls, corner-elements, -elements connectors between the flat elements, auxiliary-elements of rectangular cross section which are located adjacent to the panels. Each cell has at least one of their edges a longitudinal rail and at the opposite end has at least one counter-rail so that they can connect adjacent elements. Along the inner surface of the flat structural elements exists at least one longitudinal rail in order to couple connectors between each pair of elements and stabilize the position. Once the final structure concrete is poured into the hollow interior of this cavity and flows through the perforations in the structure generating a textured finish that can also receive other materials for creating different types of coating.
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CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application relies for priority upon Korean Patent Application No. 2003-58463 filed on Aug. 23, 2003, the contents of which are herein incorporated by reference in its entirety.
BACKGROUND OF THE INVENTION
[0002] 1. Field of the Invention
[0003] The present invention relates to a CMOS (Complementary Metal Oxide Silicon) image sensor and a method for sensing an image using the same.
[0004] 2. Description of the Related Art
[0005] A photo detector detects light, converts the detected light into an electrical signal, and outputs an image signal. For example, the photo detector may be included in a CCD (Charge Coupled Device) or a CMOS image sensor.
[0006] The CCD includes a light-sensitive element such as a photo diode, a charge transmission element and a signal output element. The photo diode detects light and generates a charge signal (or a photo charge) that is indicative of the amount of light received by the photo diode. The charge transmission element transmits the charge signal generated from the photo diode without signal loss to the signal output element. The signal output element accumulates the charge signal, and outputs an analog voltage signal in proportion to the quantity of the charge signal.
[0007] The CCD sequentially transmits the charge signal to neighboring pixels, but does not randomly access the pixels.
[0008] A CMOS image sensor has a few advantages over the CCD. In particular, the fabrication process of the CMOS image sensor is simpler than that of the CCD. In addition the CMOS image sensor employs a correlated double sampling circuit to greatly reduce a reset noise caused by resetting the charges accumulated from the photo diodes.
[0009] The correlated double sampling circuit samples a reset voltage of a pixel, and then samples a signal voltage. An output of the correlated double sampling circuit equals the difference between the reset voltage and the signal voltage. Thus, the correlated double sampling circuit may reduce fixed pattern noises due to threshold voltage differences of the transistors in pixels, and the correlated double sampling circuit reduces the reset noise due to the reset voltage differences.
[0010] One example of a pixel in the CMOS image sensor has a photo diode and four transistors. The four transistors function to transfer charge from the photo diode to the correlated double sampling circuit and to reset the accumulated charge. FIG. 1 illustrates an example of a CMOS image sensor having a photo diode and four transistor structure. As shown, a plurality of row lines 115 cross a plurality of column lines 113 . At respective crossing, pixels 101 having a photo diode and four transistor structure are formed. As further shown, reset lines 117 provide reset signals Rs for causing the pixels 101 to reset their charges, and selection lines 119 provide selection signals RSEL for causing pixels to transfer charges to an associated column line 113 .
[0011] The CMOS image sensor having pixels of the four-transistor structure has an advantage that noise is reduced, but has a disadvantage that the fill factor of the pixel is low. In other words, the area occupied by the photo diode in one pixel is relatively reduced since the pixel includes four transistors. An increased number of pixels and a decreased area occupied by a unit pixel may lead to a CMOS image sensor of high resolution. A low fill factor leads to a decrease in the area occupied by the photo diode. This decreased area occupied by the photo diode reduces the quantity of the electron-hole pairs generated by light incident on the photo diode, and thus the quantum efficiency (Q.E.) of the CMOS image sensor decreases. Therefore, the decreased quantum efficiency of the CMOS image sensor deteriorates the sensitivity of the CMOS image sensor.
SUMMARY OF THE INVENTION
[0012] The present invention provides an image sensor and method of image sensing.
[0013] In an exemplary embodiment, the pixels of the image sensor have a reduced number of transistors. This has the advantage of providing for an increased fill factor.
[0014] In another exemplary embodiment, column lines of the image sensor receive the charges generated by the pixels, and a reset circuit is associated with each column line. Each reset circuit is configured to reset the charges generated by the pixels associated with the same column line. Accordingly, a reset operation may be performed while maintaining a reduced number of transistors in an individual pixel. This promotes an increased fill factor and/or greater pixel density.
[0015] In one exemplary embodiment, the image senor includes a plurality of row lines and a plurality of column lines crossing the plurality of row lines. A pixel is formed at respective crossings of the row and column lines. Each pixel generates a charge based on light incident thereon and selectively transfers the charge to an associated column line based on a signal received from an associated row line. Each column line has a column driver circuit associated therewith. The column driver circuit is configured to generate an output voltage based on the charge on the associated column line.
[0016] For example, the pixel may include a transfer transistor for transferring the charge produced by a photo diode to an associated column line.
[0017] In another exemplary embodiment, the image sensor includes a plurality of row lines and a plurality of column lines crossing the plurality of row lines. A pixel is formed at respective crossings of the row and column lines. Each pixel generates a charge based on light incident thereon and selectively transfers the charge to an associated column line based on a signal received from an associated row line. Each column line has a reset circuit associated therewith. Each reset circuit is configured to reset the charge of each pixel associated with the associated column line.
[0018] For example, a reset circuit may include a transistor for applying a supply voltage to the associated column line.
[0019] In an exemplary embodiment of the image sensing method of the present invention, voltages are applied to the column lines based on the charges generated by in the pixels. Then, for each column line, a data voltage is generated as an output voltage based on the applied voltage.
[0020] In one exemplary embodiment, prior to the applying step, the charge of each pixel is reset.
BRIEF DESCRIPTION OF THE DRAWINGS
[0021] The above and other features and advantages of the present invention will become more apparent by describing in detail exemplary embodiments thereof with reference to the accompanying drawings, in which:
[0022] FIG. 1 illustrates an example of a prior art CMOS image sensor having a photo diode and four transistor structure;
[0023] FIG. 2 is a circuit diagram showing pixels and column driver circuit of a CMOS image sensor according to a first exemplary embodiment of the present invention;
[0024] FIG. 3 is a flow chart showing a CMOS image sensing method using the CMOS image sensor of FIG. 2 ;
[0025] FIG. 4 is a timing diagram showing the operation of the CMOS image sensor of FIG. 2 ;
[0026] FIG. 5 is a circuit diagram showing a column driver circuit of a CMOS image sensor according to a second exemplary embodiment of the present invention; and
[0027] FIG. 6 is a timing diagram showing the operation of the CMOS image sensor of FIG. 5 .
DESCRIPTION OF EMBODIMENTS
[0028] Detailed illustrative embodiments of the present invention are disclosed herein. However, specific structural and functional details disclosed herein are merely representative for purposes of describing exemplary embodiments of the present invention. This invention may, however, be embodied in many alternate forms and should not be construed as limited to the embodiments set forth herein.
[0029] Accordingly, while the invention is susceptible to various modifications and alternative forms, specific embodiments thereof are shown by way of example in the drawings and will herein be described in detail. It should be understood, however, that there is no intent to limit the invention to the particular forms disclosed, but on the contrary, the invention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention. Like numbers refer to like elements throughout the description of the figures.
[0030] <Embodiment 1>
[0031] FIG. 2 is a circuit diagram showing pixels and a column driver circuit of a CMOS image sensor according to a first exemplary embodiment of the present invention.
[0032] Referring to FIG. 2 , a plurality of row lines 215 and a plurality of column lines 213 define a matrix and a pixel 200 is located at respective crossings of the row and column lines 215 and 213 . Each of the pixels 200 comprises a photoelectric transformation element 203 and a switching element 205 . For example, the photoelectric transformation element 203 has a photo diode or a photo gate light sensitive region. In the photo gate light sensitive regions, a photo gate electrode is disposed over the photo diode so that the charge signal (or photo charge) accumulated at the photo diode may be transmitted to a sensing node 201 , which in this embodiment is on the associated column line 213 . Namely, the sensing node 201 stores the charge signal generated by the photo diode while a data voltage is detected, and generates a voltage signal corresponding to the stored charges. As described in detail below, the charges accumulated at the sensing node 210 are discharged during a reset operation.
[0033] The switching element 205 may be an NMOS transistor or a PMOS transistor. The switching element 205 may be a depletion mode MOSFET (Metal Oxide Silicon Field Effect Transistor) or an enhancement mode MOSFET. A conductive channel is formed under a gate electrode (or a control electrode) of the depletion mode MOSFET. The depletion mode MOSFET already has the conductive channel through which current may flow between a source electrode and a drain electrode of the depletion mode MOSFET, and thus the charge signal is easily transferred to the sensing node 201 .
[0034] The depletion mode MOSFET 205 is referred to as a transfer transistor since the charge signal generated from the photo diode is transferred to the sensing node 201 by the depletion mode MOSFET 205 .
[0035] A gate electrode of the transfer transistor 205 is connected to a row line 215 , a source electrode of the transfer transistor 205 is connected to an anode of the photo diode, and a drain electrode of the transfer transistor 205 is connected to the sensing node 201 .
[0036] As further shown in FIG. 2 , each of the column lines 213 includes a column driver circuit 210 . Each column driver circuit 210 includes a reset control circuit 207 , a driver circuit 209 and an output load 211 . The reset control circuit 207 performs a reset operation by discharging charges of the sensing nodes 201 . The driver circuit 209 is controlled by the voltage level at the sensing nodes 201 , and outputs one of a reference voltage and a data voltage based on the voltage level of the sensing nodes 201 . Hereinafter, the reference voltage is referred to as an output voltage of the pixel when the reset control circuit 207 is turned on, and the data voltage is referred to as an output voltage of the pixel when the reset control circuit 207 is turned off and the transfer transistor 205 is turned on. The output load 211 is coupled to an output terminal of the driver circuit 209 , and maintains the output of the driver circuit 209 above a given voltage level.
[0037] The reset control circuit 207 may include a reset transistor. For example, as shown in FIG. 2 , the reset transistor 207 comprises a depletion mode NMOS transistor. A drain electrode of the reset transistor 207 is coupled to a power or supply voltage Vdd, and a source electrode of the reset transistor 207 is coupled to a column line 213 . The reset transistor 207 is turned on or turned off in response to a reset control signal Rs received at a gate electrode of the reset transistor 207 .
[0038] The driver circuit 209 may include a driver transistor. For example, the driver transistor 209 is an enhancement mode NMOS transistor. A drain electrode of the driver transistor 209 is coupled to the power voltage Vdd, and a source electrode of the driver transistor 209 is connected to the output load 211 . A gate electrode of the driver transistor 209 is connected to the column line 213 , and is controlled by the voltage level of the column line 213 . The driver transistor 209 operates in a saturation region as a source follower amplifier during a reset operation or when the transfer transistor 205 is turned on.
[0039] The output load 211 may include a bias transistor. For example, as shown in FIG. 2 , the bias transistor 211 is an enhancement mode NMOS transistor. A source electrode of the bias transistor 211 is connected to a ground, and a drain electrode of the bias transistor 211 is connected to the source electrode of the drive transistor 209 . The gate of the bias transistor 211 receives a bias Vbias. The bias transistor 211 acts as a constant current source and as an output transistor of a current mirror (not shown) when the bias transistor 211 operates in the saturation region. Thus, the bias transistor 211 acts as an active load.
[0040] The voltage of the source electrode of the driver transistor 209 is an output of the column driver circuit 210 . The output of the column driver circuit 210 is sampled by a correlated double sampling circuit CDS (not shown).
[0041] FIG. 3 is a flow chart showing a CMOS image sensing method using the CMOS image sensor of FIG. 2 , and FIG. 4 is a timing diagram showing the operation of the CMOS image sensor of FIG. 2 .
[0042] Referring to FIGS. 3 and 4 , when a reset control signal Rs has a high level, the reset transistor 207 in each column driver circuit 210 is turned on and a reset operation begins. Since the drain electrode of the reset transistor 207 has the voltage level of the power voltage Vdd, a voltage difference is formed between the source and drain electrodes of the reset transistor 207 when electrons remain at the sensing node 201 . Thus, the electrons remaining at the sensing node 201 are attracted toward the drain electrode of the reset transistor 207 via the conductive channel. The electrons remaining at the sensing node 201 are discharged toward the power voltage (Vdd) source, and the voltage level of the sensing node 201 has substantially the same level as that of the power voltage Vdd.
[0043] The above reset operation is simultaneously performed on each of the pixels of the CMOS image sensor (step S 10 ).
[0044] The driver transistor 209 operates in a saturation region because the voltage level of the sensing node 201 is about Vdd. In order that the driver transistor 209 may operate in the saturation region, Vgs of the driver transistor 209 needs to be higher than a threshold voltage (Vth) of the driver transistor 209 and Vgd of the driver transistor 209 needs to be lower than the threshold voltage (Vth) of the driver transistor 209 when the driver transistor 209 is an enhancement mode MOSFET.
[0045] As a result of the reset operation, the driver transistor 209 outputs the reference voltage (step S 20 ).
[0046] The bias transistor 211 acts as a constant current source. In order that the driver transistor 209 may supply a constant current, Vgs' of the bias transistor 211 is determined based on the condition in which Ids=K(Vgs′−Vth) 2 , wherein Ids is the drain-source current of the driver transistor 209 . The bias transistor 211 operates in the saturation region, and the output voltage of the pixel is set at a given DC level. Thus, the reference voltage is Vdd−Vgs, and the reference voltage is input to a correlated double sampling circuit CDS.
[0047] Each of the column lines 213 is coupled to a correlated double sampling circuit CDS. The correlated double sampling circuit CDS samples the reference voltage and the data voltage, and outputs the difference between the reference voltage and the data voltage. In other words, an output of the correlated double sampling circuit equals the difference between the reference voltage and the data voltage.
[0048] When the reset transistor 207 is turned off and light is applied to a photo diode 203 , electron-hole pairs (EHPs) are generated. The photo diode 203 has a PN junction, and a depletion area is formed at the PN junction. The electrons recombine with the holes in the depletion area and disappear. An N type semiconductor has a plurality of positive ions, and a P type semiconductor has a plurality of negative ions, thus the potential of the N type semiconductor is higher than the potential of the P type semiconductor in the depletion area. As a result, an electric field is formed from the N type semiconductor to the P type semiconductor in the depletion area. The electrons of the EHPs generated from the P type semiconductor are attracted toward the N type semiconductor to be accumulated at the N type semiconductor by the electric field formed in the depletion area of the PN junction.
[0049] When a row line selection signal Tg has a high level, the transfer transistors 205 connected thereto are turned on. The charges generated by the photo diodes 203 associated with these transfer transistors 205 are transferred to the respective sensing nodes 201 via the transfer transistors 205 (step S 30 ). Since the sensing nodes 201 have the voltage level of the power voltage Vdd because of the reset operation, there is formed a voltage difference between the source and drain electrodes of each transfer transistor 205 that is turned on. Thus, the electrons accumulated at the source electrodes of the transfer transistors 205 are attracted toward the drain electrodes of the transfer transistors 205 . The potential of the drain electrodes (or the sensing nodes 201 ) of the transfer transistors 205 decreases due to the movement of the electrons.
[0050] The potential of the gate electrode of a driver transistor 209 decreases according to above described process, and the potential decrease of the gate electrode of the driver transistor 209 is reflected at the output of the driver transistor 209 since the driver transistor 209 acts as the source follower amplifier in the saturation region.
[0051] Since the small signal voltage gain of the source follower amplifier is about 1, the voltage variation of the gate electrode of the driver transistor 209 is substantially the same as the voltage variation of the source electrode of the driver transistor 209 . Thus, the potential decrease of the gate electrode of the driver transistor 209 leads to a potential decrease of the source electrode of the driver transistor 209 , and the potential decrease of the source electrode of the driver transistor 209 is input as the data voltage to a correlated double sampling circuit. Namely, the data voltage is sampled by the correlated double sampling circuit (step S 40 ). Since the correlated double sampling circuit outputs the voltage difference between the reference voltage and the data voltage, the resulting image data corresponds to the difference between the reference voltage and the data voltage.
[0052] An image signal sensed by the photo diode 203 may be represented by the variations in the difference between the reference voltage and the data voltage. In order to enhance the sensitivity of the image sensor, the variations in the difference between the reference voltage and the data voltage are increased and the driver transistor 209 is operated in the saturation region. That is, the voltage level of the sensing node 201 (or the gate electrode of the driver transistor 209 ) is higher than the threshold voltage Vth of the driver transistor 209 before application of the selection signal T g+1 for the next row line.
[0053] When a small amount of light is incident on the photo diode 203 , the amount of the generated EHPs is small. Thus, the voltage variation at the gate electrode of the driver transistor 209 is small, and the difference between the reference voltage and the data voltage is small. When a large amount of light is incident on the photo diode 203 , the amount of the generated EHPs is large, and the difference between the reference voltage and the data voltage is large.
[0054] After the image sensing operation is performed on a row line, the image sensing operation is performed on a next row line. Thus, the signal Rs has a high level and the reset operation is performed before application of the selection signal T g+1 for the next row line. In an example embodiment, the reset signal Rs is a periodic signal, and therefore the reset operation is performed periodically on each pixel of the image sensor.
[0055] <Embodiment 2>
[0056] FIG. 5 is a circuit diagram showing a column driver circuit 210 ′ of a CMOS image sensor according to a second exemplary embodiment of the present invention.
[0057] Referring to FIG. 5 , the configuration of the CMOS image sensor is the same as that of the CMOS image sensor of FIG. 2 , however, the column driver circuit 210 ′ of this embodiment further includes a selection control circuit 217 that controls the output of the driver circuit 209 by turning on/off the driver circuit 209 . The selection control circuit 217 includes a starting transistor. For example, the starting transistor 217 is an enhancement mode NMOS transistor. A drain electrode of the starting transistor 217 is connected to a source electrode of the driver transistor 209 , and a source electrode of the starting transistor 217 is connected to the output load (or the bias transistor 211 ). In addition, an output terminal of the column driver circuit 210 ′ is the source electrode of the starting transistor 217 . The gate of the starting transistor 217 receives a start signal Vstart.
[0058] The start signal Vstart is applied such that the starting transistor 217 remains in a turned-on state during the reset operation, and such that the starting transistor 217 remains in the turned-on state when the data voltage is being output after the reset operation. The start signal Vstart is applied such that the starting transistor 217 is turned off when the output of the data voltage and sampling of the data voltage by the correlated double sampling circuit are complete, and to initialize the output voltage of the column driver circuit 210 ′.
[0059] FIG. 6 is a timing diagram showing the operation of the CMOS image sensor of FIG. 5 .
[0060] Referring to FIG. 6 , when the reset signal Rs becomes a high level after the starting transistor 217 is turned on, the reset transistor 207 is turned on. As described in detail in Embodiment 1, the sensing node 201 of each pixel 200 is reset, and the voltages of the sensing nodes 201 become the power voltage Vdd.
[0061] The voltage of sensing node 201 is output as the reference voltage via the associated driver transistor 209 and the starting transistor 217 of the column driver circuit 201 ′. The starting transistor 217 operates in a triode region in order that the reference voltage may be output. Namely, the channel area approximate to a drain region of the starting transistor 217 is not in pinch-off.
[0062] In addition, since the driver transistor 209 and the bias transistor 211 operate in the saturation region, the size of the starting transistor 217 is relatively large in order that the current flowing through the driver transistor 209 and the bias transistor 211 in the saturation region may be substantially the same as the current flowing through the starting transistor 217 in the triode region. In other words, the area of the source/drain region of the starting transistor 217 is larger than that of the driver transistor 209 and the bias transistor 211 .
[0063] The transfer transistors 205 of the pixels 200 connected to the (i)th row line are turned on in order to select the pixels connected to the (i)th row line.
[0064] The data voltages are output according to the transfer transistors 205 being turned on as described in Embodiment 1.
[0065] The starting transistors 217 remain in the turned-on state while the data voltages are output.
[0066] The respective correlated double sampling circuits (not shown) sample the data voltages while the data voltages are output. The image sensing for the pixels connected to the (i)th row line ends when the starting transistors 217 are turned off. The starting transistors 217 are turned off when gate electrodes of the starting transistors 217 have a low voltage level, and the signal path between the output terminal of the column driver circuits CDSs and the column lines 213 of the image sensor are disconnected. The operation region of the bias transistors 211 varies from the saturation region to the triode region because of the disconnection of the signal path, and the charges accumulated at the capacitors of the correlated double sampling circuits are discharged to the ground via the channel of bias transistors 211 .
[0067] Thus, the output voltage of a column driver circuit is about 0 volt when the associated starting transistor 217 is turned off, so that the output signal of the column driver circuit CDS is initialized.
[0068] Then, the starting transistors 217 are turned on again so as to perform the image sensing operation for the pixels connected to (i+1)th row line, and the image sensing operation is performed on the pixels connected to (i+1)th row line according to above mentioned procedure.
[0069] While the exemplary embodiments of the present invention and their advantages have been described in detail, it should be understood that various changes, substitutions and alterations may be made herein without departing from the scope of the invention.
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The image senor includes a plurality of row lines and a plurality of column lines crossing the plurality of row lines. A pixel is formed at respective crossings of the row and column lines. Each pixel generates a charge based on light incident thereon and selectively transfers the charge to an associated column line based on a signal received from an associated row line. Each column line has a column driver circuit associated therewith. The column driver circuit is configured to generate an output voltage based on the charge on the associated column line.
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