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Gasket for a filtration element and module integrating a filtration element fitted with such a gasket

The invention provides a sealing gasket for mounting in a passage (5) of a support plate (4) to surround the end of a tubular-shaped filter element (3) provided with at least one fluid flow channel (31), the channel lying within a flow section Sc, the gasket being constituted in the form of a sleeve: possessing a height h not less than the height hps of the passage (5) in the support plate (4); and presenting an overlap bore (15) for the filter element (3) defined between one end (16) of the sleeve and a shoulder (17) which co-operates with the other end of the sleeve to define a channel bore (19) for the fluid, the shoulder (17) possessing a surface for acting as an abutment for the terminal portion of the filter element and presenting dimensions that are adapted to extend outside the flow section Sc so as to avoid impeding fluid circulation, the overlap bore (15) being provided with a groove (28) adjacent to the shoulder (17) in order to allow the gasket to creep.

1. A sealing gasket for mounting in a passage (5) of a support plate (4) to surround the end of a tubular-shaped filter element (3) provided with at least one fluid flow channel (31), the channel lying within a flow section Sc, the gasket being characterized in that it is made in the form of a sleeve: Possessing a height h not less than the height hps of the passage (5) in the support plate (4); and Presenting an overlap bore (15) for the filter element (3) defined between one end (16) of the sleeve and a shoulder (17) which co-operates with the other end of the sleeve to define a channel bore (19) for the fluid, the shoulder (17) possessing a surface for acting as an abutment for the terminal portion of the filter element and presenting dimensions that are adapted to extend outside the flow section Sc so as to avoid impeding fluid circulation, the overlap bore (15) being provided with a groove (28) adjacent to the shoulder (17) in order to allow the gasket to creep. 2. A sealing gasket according to claim 1, characterized in that the groove (28) presents a diameter dg and a height hg such that the ratio dg/dm lies in the range 1 to 1.5 and the ratio hg/hci lies in the range 0.2 to 1, with dm being the diameter of the filter element (3), and with hci being the height of the channel bore (19). 3. A sealing gasket according to claim 1, characterized in that the overlap bore (15) possesses a height hp and a diameter dp such that the ratio dp/dm lies in the range 0.6 to 1, and the ratio hp/dm lies in the range 0.2 to 1.5, where dm is the diameter of the filter element (3). 4. A sealing gasket according to claim 1, characterized in that the channel bore (19) possesses an inside diameter dci and an inside height hci lying in the range dci/2 to dci/24 and such that the ratio dci/dm lies in the range 0.77 to 0.9. 5. A sealing gasket according to claim 1, characterized in that the sleeve possesses on the outside, starting from the end (18) into which the channel bore (19) opens out, a diameter dcc extending over a height hce, so as to form an outside collar (21), the ratio dce/dm lying in the range 1.1 to 2 and the ratio hce/hl lying in the range 1.5 to 10, where hl is the height of a gasket-receiving countersink (23) formed in the backplate (11) for fixing on the support plate (4). 6. A sealing gasket according to claim 5, characterized in that the outside of the sleeve, starting from the collar (21), possesses a first tapering portion (25) and a second tapering portion (26) extending to its end (16) into which the overlap bore (15) opens out. 7. A sealing gasket according to claim 6, characterized in that: The first tapering portion (25) possesses a maximum outside diameter dpc1ma, a minimum outside diameter dpc1mi and an outside height hpc1 lying in the range dm/5 to dm/20, and such that the ratio dpc1ma/dce lies in the range 0.77 to 1, and the ratio dpc1mi/dpc1ma lies in the range 0.83 to 1; and The second tapering portion (26) possesses a maximum outside diameter dpc2ma equal to the minimum outside diameter dpc1mi of the first tapering portion (25) and a minimum outside diameter dpc2mi and an outside height hpc2 such that the ratio dp/dpc2mi lies in the range 0.8 to 1, and the ratio hpc2/dm lies in the range 0.2 to 1.5. 8. A multiple sealing gasket characterized in that it comprises a series of gaskets (6) in accordance with claim 1 interconnected by connection zones (30). 9. A multiple sealing gasket according to claim 8, characterized in that the connection zones (30) are of a height hmp such that the ratio hmp/hce lies in the range 1 to 0.2. 10. A filter module of the type comprising at least one filter element (3) supported at each of its terminal portions by a support plate (4) provided with a passage (5) and having a backplate (11) fixed thereon, which backplate is provided with a countersink (23) for each filter element (3), the module being characterized in that for each passage (5) of the support plates (4), it includes a gasket (6) in accordance with claim 1. 11. A filter module of the type comprising at least one filter element (3) supported at each of its terminal portions by a support plate (4) provided with a passage (5) and having a backplate (11) fixed thereon, which backplate is provided with a countersink (23) for each filter element (3), the module being characterized in that it includes a gasket (6) in accordance with claim 1, fitted to each support plate (4). 12. A filter module of the type comprising at least one filter element (3) supported at each of its terminal portions by a support plate (4) provided with a passage (5) and having a backplate (11) fixed thereon, which backplate is provided with a countersink (23) for each filter element (3), the module being characterized in that it includes a multiple gasket in accordance with claim 8 fitted to each support plate (4).

PACKAGED INTEGRATED CIRCUITS AND METHODS OF PRODUCING THEREOF

A packaged integrated circuit and method for producing thereof, including an integrated circuit substrate lying in a substrate plane and having electrical circuitry formed thereon, a package enclosing the integrated circuit substrate and defining first and second planar surfaces generally parallel to the substrate plane and a plurality of electrical contacts, each connected to the electrical circuitry at the substrate plane, at least some of the plurality of electrical contacts extending onto the first planar surface and at least some of the plurality of electrical contacts extending onto the second planar surface.

1. A packaged integrated circuit comprising: an integrated circuit substrate lying in a substrate plane and having electrical circuitry formed thereon; a package enclosing said integrated circuit substrate and defining first and second planar surfaces generally parallel to said substrate plane; and a plurality of electrical contacts, each connected to said electrical circuitry at said substrate plane, at least some of said plurality of electrical contacts extending onto said first planar surface and at least some of said plurality of electrical contacts extending onto said second planar surface. 2. A packaged integrated circuit according to claim 1 and wherein said package is a chip-scale package. 3. A packaged integrated circuit according to claim 1 and wherein said package includes at least one portion which is at least partially transparent to visible radiation. 4. A packaged integrated circuit according to claim 1 and wherein said package includes at least one portion which is at least partially transparent to infra-red radiation. 5. A packaged integrated circuit according to claim 2 and wherein said package includes at least one portion which is at least partially transparent to visible radiation. 6. A packaged integrated circuit according to claim 2 and wherein said package includes at least one portion which is at least partially transparent to infra-red radiation. 7. A packaged integrated circuit assembly comprising: a packaged integrated circuit including an integrated circuit substrate lying in a substrate plane and having electrical circuitry formed thereon, a package enclosing said integrated circuit substrate and defining first and second planar surfaces generally parallel to said substrate plane and a plurality of electrical contacts, each connected to said electrical circuitry at least some of said plurality of electrical contacts extending onto said first planar surface and at least some of said plurality of electrical contacts extending onto said second planar surface; and at least one additional electrical circuit element mounted onto and supported by said second planar surface and electrically coupled to at least one of said plurality of electrical contacts extending therealong. 8. A packaged integrated circuit assembly according to claim 7 and wherein said at least one additional electrical circuit element comprises an electrical component selected from the group consisting of: passive electrical elements, light generating elements, heat generating elements, light detecting elements, integrated circuits, hybrid circuits, environmental sensors, radiation sensors, micromechanical sensors, mechanical actuators and force sensors. 9. A packaged integrated circuit according to claim 7 and wherein said package is a chip-scale package. 10. A packaged integrated circuit according to claim 7 and wherein said package includes at least one portion which is at least partially transparent to visible radiation. 11. A packaged integrated circuit according to claim 7 and wherein said package includes at least one portion which is at least partially transparent to infra-red radiation. 12. A packaged integrated circuit according to claim 9 and wherein said package includes at least one portion which is at least partially transparent to visible radiation. 13. A packaged integrated circuit according to claim 9 and wherein said package includes at least one portion which is at least partially transparent to infra-red radiation. 14. A method for producing packaged integrated circuits comprising: producing, on a wafer scale, an integrated circuit substrate lying in a substrate plane and having electrical circuitry formed thereon; providing wafer scale packaging enclosing said integrated circuit substrate and defining first and second planar surfaces generally parallel to said substrate plane; forming on said wafer scale packaging a plurality of electrical contacts, each connected to said electrical circuitry at said substrate plane, at least some of said plurality of electrical contacts extending onto said first planar surface and at least some of said plurality of electrical contacts extending onto said second planar surface; and separating said integrated circuit substrate in said wafer scale packaging into a plurality of individual chip packages. 15. A method for producing packaged integrated circuits according to claim 14 and wherein said plurality of individual chip packages are chip scale packages. 16. A method according to claim 14 and wherein said package includes at least one portion which is at least partially transparent to visible radiation. 17. A method according to claim 14 and wherein said package includes at least one portion which is at least partially transparent to infra-red radiation. 18. A method according to claim 15 and wherein said package includes at least one portion which is at least partially transparent to visible radiation. 19. A method according to claim 15 and wherein said package includes at least one portion which is at least partially transparent to infra-red radiation. 20. A method for producing packaged integrated circuit assemblies, the method comprising: producing, on a wafer scale, an integrated circuit substrate lying in a substrate plane and having electrical circuitry formed thereon; providing wafer scale packaging enclosing said integrated circuit substrate and defining first and second planar surfaces generally parallel to said substrate plane; forming on said wafer scale packaging a plurality of electrical contacts, each connected to said electrical circuitry, at least some of said plurality of electrical contacts extending onto said first planar surface and at least some of said plurality of electrical contacts extending onto said second planar surface; separating said integrated circuit substrate in said wafer scale packaging into a plurality of individual chip packages; and mounting onto said at second planar surface of at least one of said plurality of individual chip packages, at least one additional electrical circuit element, said at least one additional electrical circuit element being supported by said second planar surface and electrically coupled to at least one of said plurality of electrical contacts extending therealong. 21. A method of forming a packaged integrated circuit assembly according to claim 20 and wherein said at least one additional electrical circuit element comprises an electrical component selected from the group consisting of: passive electrical elements, light generating elements, heat generating elements, light detecting elements, integrated circuits, hybrid circuits, environmental sensors, radiation sensors, micromechanical sensors, mechanical actuators and force sensors. 22. A method for producing packaged integrated circuits according to claim 20 and wherein said plurality of individual chip packages are chip scale packages. 23. A packaged integrated circuit according to claim 20 and wherein said package includes at least one portion which is at least partially transparent to visible radiation. 24. A packaged integrated circuit according to claim 20 and wherein said package includes at least one portion which is at least partially transparent to infra-red radiation. 25. A packaged integrated circuit according to claim 22 and wherein said package includes at least one portion which is at least partially transparent to visible radiation. 26. A packaged integrated circuit according to claim 22 and wherein said package includes at least one portion which is at least partially transparent to infra-red radiation. 27. A method for producing packaged integrated circuit assemblies, the method comprising: producing, on a wafer scale, an integrated circuit substrate lying in a substrate plane and having electrical circuitry formed thereon; providing wafer scale packaging enclosing said integrated circuit substrate and defining first and second planar surfaces generally parallel to said substrate plane; forming on said wafer scale packaging a plurality of electrical contacts, each connected to said electrical circuitry, at least some of said plurality of electrical contacts extending onto said first planar surface and at least some of said plurality of electrical contacts extending onto said second planar surface; mounting onto said at second planar surface of said wafer scale packaging, at least one additional electrical circuit element, said at least one additional electrical circuit element being supported by said second planar surface and electrically coupled to at least one of said plurality of electrical contacts extending therealong; and separating said integrated circuit substrate in said wafer scale packaging into a plurality of individual chip packages. 28. A method of forming a packaged integrated circuit assembly according to claim 27 and wherein said at least one additional electrical circuit element comprises an electrical component selected from the group consisting of: passive electrical elements, light generating elements, heat generating elements, light detecting elements, integrated circuits, hybrid circuits, environmental sensors, radiation sensors, micromechanical sensors, mechanical actuators and force sensors. 29. A method for producing packaged integrated circuits according to claim 27 and wherein said plurality of individual chip packages are chip scale packages. 30. A packaged integrated circuit according to claim 27 and wherein said package includes at least one portion which is at least partially transparent to visible radiation. 31. A packaged integrated circuit according to claim 27 and wherein said package includes at least one portion which is at least partially transparent to infra-red radiation. 32. A packaged integrated circuit according to claim 29 and wherein said package includes at least one portion which is at least partially transparent to visible radiation. 33. A packaged integrated circuit according to claim 29 and wherein said package includes at least one portion which is at least partially transparent to infra-red radiation.

<SOH> BACKGROUND OF THE INVENTION <EOH>Various types of packaged integrated circuits are known in the prior art. The following patents and published patent applications of the present inventor and the references cited therein are believed to represent the state of the art: U.S. Pat. Nos. 4,551,629; 4,764,846; 4,794,092; 4,862,249; 4,984,358; 5,104,820; 5,126,286; 5,266,833; 5,546,654; 5,567,657; 5,612,570; 5,657,206; 5,661,087; 5,675,180; 5,703,400; 5,837,566; 5,849,623; 5,857,858; 5,859,475; 5,869,353; 5,888,884; 5,891,761; 5,900,674; 5,938,45; 5,985,695; 6,002,163; 6,046,410; 6,080,596; 6,092,280; 6,098,278; 6,124,637; 6,134,118. EP 490739 A1; JP 63-166710 WO 85/02283; WO 89/04113; WO 95/19645 The disclosures in the following publications: “Three Dimensional Hybrid Wafer Scale Integration Using the GE High Density Interconnect Technology” by R. J. Wojnarowski, R. A. Filliion, B. Gorowitz and R. Sala of General Electric Company, Corporate Research & Development, P.O. Box 8, Schenectady, N.Y. 12301, USA, International Conference on Wafer Scale Integration, 1993. “M-DENSUS”, Dense-Pac Microsystems, Inc., Semiconductor International, December 1997, p. 50; “Introduction to Cubic Memory, Inc.” Cubic Memory Incorporated, 27 Janis Way, Scotts Valley, Calif. 95066, USA; “A Highly Integrated Memory Subsystem for the Smaller Wireless Devices” Intel(r) Stacked-CSP, Intel Corporation, January 2000; “Product Construction Analysis (Stack CSP)”, Sung-Fei Wang, ASE, R & D Group, Taiwan, 1999; “Four Semiconductor Manufacturers Agree to Unified Specifications for Stacked Chip Scale Packages”, Mitsubishi Semiconductors, Mitsubishi Electronics America, Inc., 1050 East Arques Avenue, Sunnyvale, Calif. 94086, USA; “Assembly & Packaging, John Baliga, Technology News, Semiconductor International, December 1999; “<6 mils Wafer Thickness Solution (DBG Technology)”, Sung-Fei Wang, ASE, R & D Group, Taiwan, 1999; “Memory Modules Increase Density”, DensePac Micro Systems, Garden Grove, Calif., USA, Electronics Packaging and Production, p. 24, Nov. 1994; “First Three-Chip Staked CSP Developed”, Semiconductor International, January 2000, p. 22; “High-Density Packaging: The Next Interconnect Challenge”, Semiconductor International, February 2000, pp. 91-100; “3-D IC Packaging”, Semiconductor International, p. 20, May 1998; “High Density Pixel Detector Module Using Flip Chip and Thin Film Technology” J. Wolf, P. Gerlach, E. Beyne, M. Topper, L. Dietrich, K. H. Becks, N. Wermes, O. Ehrmann and H. Reichl, International System Packaging Symposium, January 1999, San Diego; “Copper Wafer Bonding”, A. Fan, A. Rahman and R. Rief, Electrochemical and Solid State Letters, 2(10), pp. 534-536, 1999; “Front-End 3-D Packaging”, J. Baliga, Semiconductor International, December 1999, p 52, are also believed to represent the state of the art.

<SOH> SUMMARY OF THE INVENTION <EOH>The present invention seeks to provide improved packaged integrated circuits and methods for producing same. There is thus provided in accordance with a preferred embodiment of the present invention a packaged integrated circuit including an integrated circuit substrate lying in a substrate plane and having electrical circuitry formed thereon, a package enclosing the integrated circuit substrate and defining first and second planar surfaces generally parallel to the substrate plane and a plurality of electrical contacts, each connected to the electrical circuitry at the substrate plane, at least some of the plurality of electrical contacts extending onto the first planar surface and at least some of the plurality of electrical contacts extending onto the second planar surface. Further in accordance with a preferred embodiment of the present invention the package is a chip-scale package. Additionally in accordance with a preferred embodiment of the present invention the package includes at least one portion which is at least partially transparent to visible radiation. Alternatively the package includes at least one portion which is partially transparent to infra-red radiation. There is also provided in accordance with another preferred embodiment of the present invention a packaged integrated circuit assembly including a packaged integrated circuit including an integrated circuit substrate lying in a substrate plane and having electrical circuitry formed thereon, a package enclosing the integrated circuit substrate and defining first and second planar surfaces generally parallel to the substrate plane and a plurality of electrical contacts, each connected to the electrical circuitry at least some of the plurality of electrical contacts extending onto the first planar surface and at least some of the plurality of electrical contacts extending onto the second planar surface and at least one additional electrical circuit element mounted onto and supported by the second planar surface and electrically coupled to at least one of the plurality of electrical contacts extending therealong. Further in accordance with a preferred embodiment of the present invention the additional electrical circuit element includes an electrical component selected from the group consisting of: passive electrical elements, light generating elements, heat generating elements, light detecting elements, integrated circuits, hybrid circuits, environmental sensors, radiation sensors, micromechanical sensors, mechanical actuators and force sensors. Additionally in accordance with a preferred embodiment of the present invention the package includes at least one portion which is at least partially transparent to visible radiation. Alternatively the package includes at least one portion which is at least partially transparent to infra-red radiation. Still further in accordance with a preferred embodiment of the present invention the package is a chip-scale package. There is further provided in accordance with a preferred embodiment of the present invention a method for producing packaged integrated circuits. The method includes producing, on a wafer scale, an integrated circuit substrate lying in a substrate plane and having electrical circuitry formed thereon, providing wafer scale packaging enclosing the integrated circuit substrate and defining first and second planar surfaces generally parallel to the substrate plane, forming on the wafer scale packaging a plurality of electrical contacts, each connected to the electrical circuitry at the substrate plane, at least some of the plurality of electrical contacts extending onto the first planar surface and at least some of the plurality of electrical contacts extending onto the second planar surface and separating the integrated circuit substrate in the wafer scale packaging into a plurality of individual chip packages. Further in accordance with a preferred embodiment of the present invention the plurality of individual chip packages are chip scale packages. Additionally in accordance with a preferred embodiment of the present invention the package includes at least one portion which is at least partially transparent to visible radiation. Alternatively the package includes at least one portion which is at least partially transparent to infra-red radiation. There is also provided in accordance with yet another preferred embodiment of the present invention a method for producing packaged integrated circuit assemblies. The method includes producing, on a wafer scale, an integrated circuit substrate lying in a substrate plane and having electrical circuitry formed thereon, providing wafer scale packaging enclosing the integrated circuit substrate and defining first and second planar surfaces generally parallel to the substrate plane, forming on the wafer scale packaging a plurality of electrical contacts, each connected to the electrical circuitry, at least some of the plurality of electrical contacts extending onto the first planar surface and at least some of the plurality of electrical contacts extending onto the second planar surface, separating the integrated circuit substrate in the wafer scale packaging into a plurality of individual chip packages and mounting onto the at second planar surface of at least one of the plurality of individual chip packages, at least one additional electrical circuit element, the at least one additional electrical circuit element being supported by the second planar surface and electrically coupled to at least one of the plurality of electrical contacts extending therealong. Further in accordance with a preferred embodiment of the present invention the additional electrical circuit element includes an electrical component selected from the group consisting of: passive electrical elements, light generating elements, heat generating elements, light detecting elements, integrated circuits, hybrid circuits, environmental sensors, radiation sensors, micromechanical sensors, mechanical actuators and force sensors. Additionally in accordance with a preferred embodiment of the present invention the package includes at least one portion which is at least partially transparent to visible radiation. Alternatively the package includes at least one portion which is at least partially transparent to infra-red radiation. There is further provided in accordance with yet another preferred embodiment of the present invention a method for producing packaged integrated circuit assemblies. The method includes producing, on a wafer scale, an integrated circuit substrate lying in a substrate plane and having electrical circuitry formed thereon, providing wafer scale packaging enclosing the integrated circuit substrate and defining first and second planar surfaces generally parallel to the substrate plane, forming on the wafer scale packaging a plurality of electrical contacts, each connected to the electrical circuitry, at least some of the plurality of electrical contacts extending onto the first planar surface and at least some of the plurality of electrical contacts extending onto the second planar surface, mounting onto the at second planar surface of the wafer scale packaging, at least one additional electrical circuit element, the at least one additional electrical circuit element being supported by the second planar surface and electrically coupled to at least one of the plurality of electrical contacts extending therealong and separating the integrated circuit substrate in the wafer scale packaging into a plurality of individual chip packages. Further in accordance with a preferred embodiment of the present invention the additional electrical circuit element includes an electrical component selected from the group consisting of: passive electrical elements, light generating elements, heat generating elements, light detecting elements, integrated circuits, hybrid circuits, environmental sensors, radiation sensors, micromechanical sensors, mechanical actuators and force sensors. Additionally in accordance with a preferred embodiment of the present invention the package includes at least one portion which is at least partially transparent to visible radiation. Alternatively the package includes at least one portion which is at least partially transparent to infra-red radiation.

Solder foil semiconductor device and electronic device

A solder foil formed from a material comprising particles of Cu, etc. as metal particles and Sn particles as solder particles by rolling is suitable for solder bonding at a high temperature side in temperature-hierarchical bonding, and semiconductor devices and electronic devices produced by use of such solder bonding have distinguished reliability of mechanical characteristics, etc.

1. A solder foil, characterized by being formed from a material comprising metal particles and solder particles by rolling. 2. A solder foil, characterized by being formed from a material comprising Cu particles and Sn particles by rolling. 3. A solder foil characterized by being formed from a solder comprising Cu and Sn by pressing, where Cu is in a particulate state and Sn is in a state of filling in spaces between the Cu particles. 4. A solder foil according to claim 2, characterized in that when the solder foil is subjected to reflowing, at least one portion of the Cu particle surface is covered by Cu6Sn5. 5. A solder foil according to claim 2, characterized in that when the solder foil is subjected to reflowing, the Cu particles and Sn after plastic deformation are bonded to each other by a compound comprising Cu6Sn5. 6. A solder foil according to claim 2, characterized in that the Cu particles have particle sizes of 10-40 μm. 7. A solder foil according to claim 2, characterized in that the Cu particles have particle sizes of 3-10 μm. 8. A solder particles according to claim 2, characterized in that the Cu particles have a Ni plating or Ni/Au plating layer on the surfaces. 9. A solder foil according to claim 2, characterized in that at least Cu-exposed portion of the foil are Sn-plated. 10. A solder foil according to claim 1, characterized in that the solder foil has a thickness of 80 μm-150 μm. 11. A solder foil according to claim 1, characterized in that the solder foil has a thickness of 150 μm-250 μm. 12. A solder foil according to claim 1, characterized in that plastic particles are further contained. 13. A solder foil according to claim 2, characterized in that other particles having a lower coefficient of thermal expansion than that of Cu is further contained. 14. A solder foil according to claim 2, characterized in that other particles having a lower coefficient of thermal expansion than that of Cu are particles of Invar alloy series, silica, alumina, AlN or SiC. 15. A solder foil according to claim 2, characterized in that In particles are further contained. 16. A solder foil according to claim 2, characterized in that the Cu particles and the Sn particles are mixed together in vacuum, in a reductive atmosphere or in an inert gas atmosphere, and then formed into a foil by pressing. 17. A solder foil according to claim 2, characterized in that a draft percentage is 15%-20%. 18. A solder foil, characterized by being formed from a material comprising metal fibers and solder particles by rolling. 19. A solder foil, characterized by being formed from a solder comprising Cu metal fibers and Sn particles by rolling. 20. A solder foil according to claim 19, characterized in that the Cu metal fibers of the solder material are in an oblong shape. 21. A solder foil, characterized by being formed from a solder material comprising particles of Al, An or Ag, and Sn particles by rolling. 22. A solder foil, characterized by being formed from a solder material comprising particles of Zn—Al system alloy or Au—Sn system alloy, and Sn particles by rolling. 23. An electronic device, which comprises a first electronic device, a second electronic device, and a third electronic device, characterized in that the first electronic device and the second electronic device are bonded to each other by a first solder foil according to claim 1, and the second electronic device and the third electronic device are bonded to each other by a second solder having a lower melting point than that of the first solder foil. 24. An electronic device, characterized in that a first electronic device and a second electronic device are bonded to each other by a solder foil formed from a material comprising Cu particles and Sn particles by rolling, and the second electronic device and a third electronic device are bonded to each other by a solder having a lower melting point than that of the solder foil. 25. A semiconductor device, which comprises a semiconductor chip, a tab on which the semiconductor chip is to be disposed, and a lead serving as a connector terminal to the outside, an electrode on the semiconductor chip being bonded to the lead by wire bonding, characterized in that the semiconductor chip and the tab are bonded to each other by a solder foil formed from a material comprising a mixture of metal particles and solder particles. 26. A semiconductor device according to claim 25, characterized in that the solder foil is a solder foil formed from a material comprising a mixture of metal particles and solder particles by rolling. 27. A semiconductor device according to claim 25, characterized in that the solder foil is a solder foil formed from a material comprising Cu particles and Sn particles by rolling. 28. An electronic device, which comprises a circuit board and a semiconductor chip, an electrode on the circuit board and an electrode on the semiconductor chip being bonded to each other by wire bonding, characterized in that the circuit board and the semiconductor chip are bonded to each other by a solder foil comprising a mixture of metal particles and solder particles. 29. An electronic device, which comprises a circuit board, and a semiconductor chip, an electrode on the circuit board and an electrode on the semiconductor chip being bonded to each other by wire bonding, characterized in that the circuit board and the semiconductor chip are bonded to each other by a solder foil formed from a solder material comprising Cu particles and Sn particles by rolling.

<SOH> BACKGROUND ART <EOH>In the case of solders of Sn—Pb system, it has been possible to carry out temperature-hierarchical bonding, which comprises soldering lead (Pb)-rich Pb-5Sn (melting point: 314-310° C.), Pb-10Sn (melting point: 302-275° C.), etc. as high temperature series solders at temperatures of approximately 330° C., and then bonding a Sn-37Pb eutectic mixture (melting point: 183° C.) as low temperature series solders without melting the first soldered portions. These solders have been capable of bonding Si chips, etc., which are flexible and high in deformability and thus is easy to break, to a substrate having a different coefficient of thermal expansion. Such a temperature-hierarchical bonding has been applied to semiconductor devices of chip die-bonding type, semiconductor devices of chip flip-chip-bonding type such as BGA, CSP, etc. That is, this means that a solder for use within the semiconductor device and a solder for bonding a semiconductor device itself to a substrate undergo temperature-hierarchical bonding. In every field, there is now a growing tendency to make the solder lead-free. Sn—Ag eutectic series (melting point: 221° C.), Sn—Ag—Cu eutectic series (melting point: 221°-217° C.) and Sn—Cu eutectic series (melting point: 227° C.) are now the mainstreams of Pb-free solders. A lower soldering temperature is desirable for the surface mounting in view of the heat resistance of parts, but actually it is approximately 235°-245° C. in the case of Sn—Ag—Cu eutectic series having a possibly lowest bonding temperature in view of the necessity for assuring a wettability to attain the reliability and also in view of considerable temperature fluctuations throughout a substrate in spite of using a furnace with distinguished temperature uniformity control. Thus, solders for the hierarchical bonding, which can withstand such a soldering temperature, must have a melting point of at least 250° C., but actually any Pb-free solders for use on the high temperature side of temperature-hierarchical bonding, which can be used in combination thereof, is not yet available. Sn-5Sb (melting point: 240°-232° C.) is a most possible Pb-free solder composition, but is not available for the temperature-hierarchical bonding because of melting thereof. Au-20Sn (melting point: 280° C.) is known as a solder of higher temperature series, but it is so hard and expensive that its use is restricted to a narrow range. Particularly in bonding Si chips to a material having a different coefficient of thermal expansion and also in bonding of large chips, the Au-20Sn solder is not available, because it is so hard as to break Si chips with high possibility.

<SOH> BRIEF DESCRIPTION OF DRAWINGS <EOH>FIG. 1 is views showing manufacturing steps of a composite metal from composite balls. FIG. 2 is cross-sectional views of a model before and after rolling of elastomer plastic balls in a dispersion state, respectively. FIG. 3 is a cross-sectional view of a model according to one embodiment of die bonding process. FIG. 4 is a cross-sectional view of model showing a die bonded joint by using a solder foil comprising Cu and Sn in combination. FIG. 5 is cross-sectional views of a model of bonding LSI and cap to a substrate. FIG. 6 is a cross-sectional view of power module. FIG. 7 is cross-sectional views of a model of mounting modules onto a printed circuit board. FIG. 8 is cross-sectional views of a model of mounting RF module. FIG. 9 is process flow charts each showing a process for mounting an RF module. FIG. 10 is a plan view of a high power output resin package and cross-sectional views of models thereof. FIG. 11 is a flow chart showing a process for making a high power output resin package. FIG. 12 is a cross-sectional view of a model of plastic package. FIG. 13 is a perspective view and a cross-sectional view of a model of a combination with metal fibers. FIG. 14 is a perspective view of a model with crossed metal fibers. FIG. 15 is cross-sectional views of a model with network fibers. FIG. 16 is a plan view and a cross-sectional view showing long and slender fibers disposed at random, followed by flattening. FIG. 17 is a cross-sectional view of a model with oblong metal fibers and non-metal fibers. detailed-description description="Detailed Description" end="lead"? In the drawings, reference numerals denote the following members: 1 . . . carbon jig, 2 . . . Cu ball, 3 . . . Sn ball, 4 . . . Sn, 5 . . . roll, 6 . . . plastic ball, 7 . . . resistance heater tool, 8 . . . Si chip, 9 . . . vacuum suction hole, 10 . . . nitrogen, 11 . . . solder foil, 12 . . . silicone gel, 13 . . . Al 2 O 3 substrate, 14 . . . W (sintered)-Cu plated electrode, 15 . . . heater for preheating, 16 . . . thermocouple for temperature measurement, 17 . . . Cu—Sn combination foil, 18 . . . bump, 19 . . . soft resin, 20 . . . lead, 21 . . . solder ball bump, 22 . . . printed circuit board, 23 . . . Al fin, 24 . . . bonded portion with fin, 25 . . . bonded portion with lead, 26 . . . lead, 27 . . . solder foil, 28 . . . terminal of substrate, 29 . . . module substrate, 30 . . . terminal, 31 . . . Cu, 32 . . . organic substrate, 33 . . . Cu throughhole conductor, 34 . . . Ag—Pd conductor, 35 . . . wire bond, 36 . . . AlN interposer substrate, 37 . . . connection terminal, 38 . . . Cr—Cu—Au, 39 . . . die bonding, 40 . . . solder foil, 41 . . . press, 42 . . . Ni—Au-plated metallization layer, 43 . . . interposer substrate, 44 . . . Cr—Ni—Au metallization layer, 45 . . . electroless Ni plating, 46 . . . electrical Ni plating, 47 . . . solder, 48 . . . Cu disc, 49 . . . Cu base, 50 . . . Al 2 O 3 insulation substrate, 51 . . . Cu lead, 52 . . . chip part, 53 . . . Cu pad, 54 . . . TQFP-LSI, 55 . . . Sn—Ag—Cu system solder, 56 . . . lead, 57 . . . dam cut portion, 58 . . . resin, 59 . . . throughhole, 60 . . . W—Ni—Au thick film electrode, 61 . . . W—Ni (or Ag—Pd, Ag) thick film conductor, 62 . . . Au-plated electrode, 63 . . . caulked portion, 64 . . . heat diffusion plate (header), 65 . . . lead frame, 66 . . . tab, 67 . . . electroconductive paste, 68 . . . solder, 69 . . . fiber, 70 . . . Cu netting (lateral cross-section), 71 . . . Cu netting (longitudinal cross-section), 72 . . . solder (sea), 73 . . . long and slender fiber, and 74 . . . oblong fiber

Surface-functionalised carrier material, method for the production thereof and solid phase synthesis method

The invention concerns a novel surface-functionalized carrier material with a polymeric surface and at least one linker compound according to the general formula (I), which is covalently bound to the surface. In the formula, P indicates the polymeric surface; R2 has the meaning OR4 or NR4R5 and R1, R4 and R5, independently of one another, indicate H, an alkyl group or an aryl group; R3 indicates H, an alkyl, an aryl, an acyl, an alkoxycarbonyl or an aryloxycarbonyl group; and the alkyl, aryl, acyl, alkoxycarbonyl and/or aryloxycarbonyl group of the radicals R1, R3, R4 and R5, independently of one another, are substituted or unsubstituted. The material according to the invention can be very easily produced by photochemical coupling and serves for the solid-phase synthesis of amino acids, peptides, proteins or molecules with at least one peptidic structural unit.

1. A surface-functionalized carrier material with a polymeric surface and at least one linker compound according to general formula (I), which is covalently bound to the latter: in which P indicates the polymeric surface; R2 has the meaning OR4 or NR4R5 and R1, R4 and R5, independently of one another, indicate H, an alkyl group or an aryl group; R3 indicates H, an alkyl, an aryl, an acyl, an alkoxycarbonyl or an aryloxycarbonyl group; and the alkyl, aryl, acyl, alkoxycarbonyl and/or aryloxycarbonyl group of the residues R1, R3, R4 and R5, independently of one another, are substituted or unsubstituted. 2. The surface-functionalized carrier material according to claim 1, further characterized in that the polymeric surface (P) and/or the carrier material is an organic polymer. 3. The surface-functionalized carrier material according to claim 2, further characterized in that the organic polymer is polypropylene, polyethylene, polysulfone, polyether sulfone, polystyrene, polyvinyl chloride, polyacrylonitrile, cellulose, amylose, agarose, polyamide, polyimide, polytetrafluoroethylene, polyvinylidene difluoride, polyester, polycarbonate, polyacrylate, polyacrylamide or a derivative of these or a copolymer or a blend thereof. 4. The surface-functionalized carrier material according to claim 1, further characterized in that the carrier material is an inorganic and/or mineral material. 5. The surface-functionalized carrier material according to claim 4, further characterized in that the carrier material is a glass, a silicate, a ceramic material or a metal. 6. The surface-functionalized carrier material according to one of claims 2 to 5, further characterized in that the carrier material is a composite of at least one inorganic and/or mineral material and at least one organic polymer. 7. The surface-functionalized carrier material according to one of the preceding claims, further characterized in that the carrier material is present in the form of a membrane, a film, a plate, a microtiter plate, a test tube, a glass slide, a fiber, a hollow fiber, a nonwoven material, a woven fabric, a powder, a granulate, or of particles, and may be porous or nonporous. 8. The surface-functionalized carrier material according to claim 7, further characterized in that the carrier material is present in the form of a membrane with a symmetric or asymmetric pore structure. 9. The surface-functionalized carrier material according to claim 7 or 8, further characterized in that a pore size amounts to 1 nm to 10 μm. 10. The surface-functionalized carrier material according to one of the preceding claims, further characterized in that the alkyl groups of the radicals R1, R3, R4 and R5 and the acyl and the alkoxycarbonyl groups of the radical R3 are C1 to C20 alkyl units. 11. The surface-functionalized carrier material according to one of the preceding claims, further characterized in that the aryl groups of the radicals R1, R3, R4 and R5 and the aryloxycarbonyl group of the radical R3 is a phenyl group. 12. A method for the production of a surface-functionalized carrier material according to formula (I): wherein P indicates the polymeric surface of the carrier material; R2 has the meaning OR4 or NR4R5 and R1, R4 and R5, independently of one another, indicate H, an alkyl group or an aryl group; R3 indicates H, an alkyl, an aryl, an acyl, an alkoxycarbonyl or an aryloxycarbonyl group; and the alkyl, aryl, acyl, alkoxycarbonyl and/or aryloxycarbonyl group of the radicals R1, R3, R4 and R5, independently of one another, are substituted or unsubstituted, with the steps: a) Introducing a linker compound according to general formula (II): in which R1, R2 and R3 have the above meaning, onto a polymeric surface (P) of a carrier material, b) Irradiating the surface with light of the UV-vis spectral region, whereby a covalent bond forms between the linker compound according to formula (II) and the polymeric surface (P) with the formation of the surface-functionalized carrier material according to formula (I). 13. The method according to claim 12, further characterized in that the irradiation is conducted with light of a wavelength region of 250 to 500 nm. 14. The method according to claim 13, further characterized in that lasers, UV tubes or mercury vapor lamps, optionally with the use of suitable filters, are utilized as light sources. 15. The method according to one of claims 12 to 14, further characterized in that the irradiation of the surface is conducted in the presence or in the absence of a sensitizer. 16. The method according to one of claims 12 to 15, further characterized in that after the irradiation, unreacted substances are removed by washing with a washing fluid. 17. The method according to claim 16, further characterized in that water, an organic solvent or a solvent mixture is used as the washing fluid. 18. The method according to one of claims 12 to 17, further characterized in that a material according to one of claims 2 to 9 is used as the polymeric surface (P) and/or carrier material. 19. Use of a surface-functionalized carrier material according to general formula (I) for the covalent immobilization of biomolecules, particularly of amino acids, peptides or proteins or molecules with amino and/or carboxyl groups. 20. A method for the synthesis of amino acids, peptides, proteins or molecules with at least one peptide structural unit at solid phases, wherein the first amino acid to be utilized for the synthesis is covalently bound to a surface-functionalized carrier material and the chain extension is conducted by successive coupling of additional amino acids and/or chemical modification is produced, is hereby characterized in that a surface-functionalized carrier material according to general formula (I) is used according to one of claims 1 to 11 as the solid phase. 21. The method according to claim 20, further characterized in that the first amino acid utilized for the synthesis is bound to the carrier material by a peptide bond, selectively, either between the amino group of the amino acid and the C1 position of the linker compound or between the carboxyl group of the amino acid and the amino group of the linker compound. 22. The method according to claim 21, further characterized in that the N or C-terminal binding of the amino acid to the linker compound is controlled by blocking the amino group or the carboxyl group of the amino acid and/or the C1 position or the amino group of the linker compound with chemical protective groups.

Interconnecting module for the base of electronic equipment casing

This interconnection module for the base of an electronic device casing carries out the transfer, at the faces of the printed circuit boards (4, 5) supporting the components of the device housed in the casing, of a field of connection points with the external environment of the casing embodied by the rear ends of the pins of a semi-connector 3 fixed to the back of the casing while still retaining the compactness of the casing despite a very large number of connection points with the external environment of the casing (several hundreds of them). This module takes the form of a three-panel structure with a central panel 7 fixed to the rear ends of the pins of the semi-connector (3) mounted on the back of the casing and two side panels (8, 9) folded and placed flat against each other, joined to the longitudinal edges of the central panel (7) by flexible printed circuit elements (10, 11) and supporting the field of connection points transferred to the level of the faces of the boards (4,5) of the electronic device. Electronic connections link the two fields of connection points in going through the joining parts (10, 11).

1. Interconnecting module for the base of an electronic device casing including two groups of printed circuit boards bearing electronic device components, each group having one or more stacked printed circuit boards, and that has a back equipped with a field of contacts constituting electrical connection points accessible from the exterior of the casing, said interconnecting module providing for the transfer, at the level of the two groups of printed circuit boards of the connection points of the casing accessible from the exterior, comprising a field of electrical connection points transferred to the interior of the casing so as to be facing the two groups of printed circuit boards and tracks setting up the electrical links between this transferred field of connection points and the field of contacts with which the back of the casing is equipped, comprising: a central panel in printed circuit form, fixed to the back of the field of contacts of the connection points of the casing with the external environment, parallel to the back of the casing, and supporting the electrical connection tracks, on a portion of their paths starting from the contacts of this field of connection points with the external environment, said tracks being divided, on this portion of their paths, into at least two groups going towards opposite edges of the central panel, called longitudinal edges, and two side panels in printed circuit form, folded and placed flat against each other between the two groups of printed circuit boards, attached on either side of the central panel, each by an edge of one of the longitudinal edges of the central panel, by means of a linking part in the form of a flexible printed circuit having a size sufficient to enable them to be folded and placed flat against each other, sharing the transferred field of connection points and the linking tracks that lead thereto from the field of contacts of the connection points of the casing with the external environment, the transferred field of connection points being equipped with through-contacts, the connection points of the part of the transferred field borne by a side panel being shifted laterally with respect to the connection points of the matching part of the transferred field borne by the other side panel, the side panels supporting the connection tracks on the portion of their paths that leads to their part of the transferred field of connection points and being provided with at least one aperture leaving space for the through-contacts of the other side panel, the connecting tracks that lead to the part of the transferred field of connection points of a side panel passing, in order to meet contacts of the field of connection points accessible from the exterior of the casing, through the linking part attaching one of the edges of the side panel considered with one of the longitudinal edges of the central panel. 2. The module according to claim 1, wherein the central and side panels are rigid panels. 3. The module according to claim 1, adapted to a casing comprising a metal shielding partition wall between the two groups of printed circuit boards characterized in that said metal shielding partition wall interposed between the two side panels that are folded and placed flat against each other. 4. The module according to claim 1, wherein the two side panels are folded and placed flat against each other in parallel to a plane perpendicular to the central panel. 5. The module according to claim 1, wherein the two side panels are folded and placed flat against each other, in parallel and on either side of a plane perpendicular to the central panel, parallel to the longitudinal edges of this central panel and passing through its middle. 6. The module according to claim 1, wherein the ends of the through-contacts of the transferred field of connection points form pins for semi-connectors mounted back-to-back, on each side of the block constituted by the two side panels folded and placed flat against each other, designed to co-operate by fitting together with semi-connectors having matching shapes mounted on the printed circuit board of each of the two groups of printed circuit boards that directly face the two side panels. 7. The module according to claim 1, wherein the side panels are provided with an internal field of electrical connection points having no link with the contacts of the field of connection points with the environment outside the casing, borne by the central panel, said internal field of connection points comprising through-contacts forming pins of semi-connectors on the two opposite faces of the block constituted by the two side panels, folded and placed flat against each other, these pins of semi-connectors being designed to co-operate by fitting together with semi-connectors of matching shapes mounted on the printed circuit board of each of the two groups of printed circuit boards that directly face the two side panels. 8. The module according to claim 7, wherein the semi-connectors mounted on each side of the block constituted by the two side panels folded and placed flat against each other comprise, without distinction, pins constituted by through-contacts belonging to the transferred field of connection points and to the internal field of connection points. 9. The module according to claim 1, wherein the part of the transferred field of connection points borne by a side panel is shifted laterally with respect to the matching part of the transferred field of connection points borne by the other side panel, each side panel comprising an aperture allowing passage to the part of the transferred field of connection points that is borne by the other side panel. 10. The module according to claim 9, wherein the semi-connectors equipping the block formed by the side panels folded and placed flat against each other have different thicknesses as a function of the side panel that supports them so that all are flush with the same level on each face of the block although the levels at which they are affixed depend on the side panel that supports them. 11. The module according to claim 10, wherein the differences in thickness imposed on the semi-connectors equipping the block constituted by the side panels folded and placed flat against each other, so that they are flush at the same level, are obtained by means of thickness shims. 12. The module according to claim 9, wherein the side panels have identical dissymmetrical contours and are placed so as to be folded and positioned flat against each other so as to have non-coinciding contours. 13. The module according to claim 1, wherein the semi-connectors equipping the block constituted by the side panels folded and placed flat against each other co-operate with the semi-connectors of matching shapes mounted on the printed circuit boards of each of the two groups of printed circuit boards coming into a position that directly faces the two side panels whose pins are constituted by through-contacts forming, at their other end, other pins for the semi-connectors mounted on an opposite face reproducing the semi-connectors of the two side panels and making the fields of connection points of the side panels accessible to the next printed circuit board belonging to the same group. 14. The module according to claim 13, wherein the printed circuit boards of a group comprising through-contacts aligned with those of the semi-connectors borne by the side panels, forming, on one face of the board, pins of nestable semi-connectors with shapes matching the nestable semi-connectors of the side panels and, on the other face, nestable semi-connectors having the same shapes as the semi-connectors of the side panels so that, in fitting together, they make it possible, with the printed circuit boards of a group, to form a stack of printed circuit boards having access to all the connection points of the fields of connection points of the side panels.

Dispensing Apparatus

A dispensing apparatus (1) including a combination of a tube (2), cap (4) and plunger (3). The tube is arranged for carrying a collapsible sausage (6) and includes longitudinally extending ribs (8) projecting inwardly of the tube and defining longitudinal grooves (7) therebetween, the grooves having an annular dimension (A) greater than the distance (B) between adjacent ribs. The cap includes: a coupling portion (20) for mounting the cap to the tube; an outlet (21) through which contents of the collapsible sausage carried within the tube arc dispensed; and a chamber (22) into which the sausage is adapted to be collapsed under action of the plunger within the tube. The plunger itself has a main body (11) with radial fins (10) projecting therefrom for receipt in the grooves of the tube, between adjacent ribs, the fins being dimensioned to engage lateral edges of the ribs, in a point contact manner.

1. A tube for carrying a collapsible sausage and dispensing contents therefrom, the tube having longitudinally extending ribs projecting inwardly of the tube and defining longitudinal grooves therebetween, the grooves having an annular dimension greater than the distance between adjacent ribs. 2. A tube as claimed in claim 1, wherein the ribs and grooves extend substantially the entire length of the tube. 3. A tube as claimed in claim 1 or 2, wherein ends of the tube are provided with inwardly directed stop surfaces for capturing a plunger therebetween. 4. The ends of the tube are provided with an inwardly directed lip for engaging with and securing a cap relative thereto. 5. A cap for use with the above tube, the cap having: a coupling portion for mounting the cap to the tube; an outlet through which contents of the collapsible sausage carried within the tube are dispensed; and a chamber into which the sausage is adapted to be collapsed under action of a plunger within the tube. 6. A cap as claimed in claim 5, wherein the coupling portion includes a spline formed on an outer surface of the cap for receipt in an associated groove of the tube. 7. A cap as claimed in claim 5 or 6, wherein the cap includes a well, provided within the chamber for receipt of an end clip of the sausage. 8. A cap as claimed in any one of claims 5 to 7, wherein the cap includes piercing structure projecting from a base of the cap for puncturing the sausage. 9. A cap as claimed in claim 8, wherein the piercing structure is provided in the well, adjacent the outlet. 10. A cap as claimed in claims 8 or 9, wherein the piercing structure includes two teeth positioned toward either side of the outlet. 11. A cap as claimed in claim 10, wherein one of tho teeth projects a lesser distance from the base of the cap and includes a vane directed away from an other of the teeth, so as to tension the sausage away from a puncture zone and facilitate propagation of a tear in the sausage. 12. A cap as claimed in any one of claims 8 to 11, wherein the cap includes a shroud arranged adjacent the well, an a side of the outlet opposite the piercing structure, the shroud serving to impart a turning moment at an end of the sausage so as to deflect the end clip of the sausage into the well at a location offset from the outlet. 13. A cap as claimed in claim 12, wherein the shroud is formed by a series of arc-shaped ribs. 14. A cap as claimed in any one of claims 6 to 13, wherein the cap is provided with a rebate on an exterior surface thereof for engagement with a complimentary lip of the tube, for securing the cap relative to the tube. 15. A plunger for use in the above described tube, the plunger having a main body with radial fins projecting therefrom for receipt in the grooves of the tube, between adjacent ribs, the fins being dimensioned to engage lateral edges of the ribs, in a point contact manner. 16. A plunger as claimed in claim 15, wherein the body of the plunger includes a central bulb for driving the sausage into a cap coupled to the tube. 17. A plunger as claimed in claim 16, wherein the plunger includes a reduced dimension region between the bulb and the fins. 18. A plunger as claimed in claim 17, wherein the bulb includes a bore for receipt of an end clip of the sausage. 19. A plunger as claimed in any one of claims 16 to 18, wherein the plunger is symmetric and reversible. 20. A dispensing apparatus including: a tube, as claimed in any one of claims 1 to 4; a cap, as claimed in any one of claims 6 to 14, and a plunger, as claimed in any one of claims 15 to 19.

<SOH> BACKGROUND OF THE INVENTION <EOH>It is known to dispense contents of a collapsible sausage from a caulking gun arrangement or the like which carries a tube, with a plunger. The plunger is intended to be reversible within the tube for subsequent dispensing of contents from another sausage, in a reverse direction. The known arrangement is, however, considered to be inadequate insofar as the plunger tends to got jammed and replacement of the sausage can be somewhat messy.

<SOH> SUMMARY OF THE INVENTION <EOH>In accordance with the present invention, there is provided a tube for carrying a collapsible sausage and dispensing contents therefrom, the tube having longitudinally extending ribs projecting inwardly of the tube and defining longitudinal grooves therebetween, the grooves having an annular dimension greater than the distance between adjacent ribs. Preferably, the ribs and grooves extend substantially the entire length of the tube. Preferably, ends of the tube arc provided with inwardly directed stop surfaces for capturing a plunger therebetween. Preferably, ends of the tube are provided with an inwardly directed lip for engaging with and securing a cap relative thereto. In another aspect, there is provided a cap for use with the above tube, the cap having: a coupling portion for mounting the cap to the tube; an outlet through which contents of the collapsible sausage carried within the tube are dispensed; and a chamber into which the sausage is adapted to be collapsed under action of a plunger within the tube. Preferably, the coupling portion includes a spline formed on an outer surface of the cap for receipt in an associated groove of the tube. Preferably, the cap includes a well, provided within the chamber for receipt of an end clip of the sausage. Preferably, the cap includes piercing structure projecting from a base of the cap for puncturing the sausage. Preferably, the piercing structure is provided in the well, adjacent the outlet. Preferably, the piercing structure includes two teeth positioned toward either side of the outlet. More preferably, one of the teeth projects a lesser distance from the base of the cap and includes a vane directed away from an other of the teeth, so as to tension the sausage away from a puncture zone and facilitate propagation of a tear in the sausage. Preferably, the cap includes a shroud arranged adjacent the well, on a side of the outlet opposite the piercing structure, the shroud serving to impart a turning moment at an end of the sausage so as to deflect the end clip of the sausage into the well at a location offset from the outlet. Preferably, the shroud is formed by a series of arc-shaped ribs. Preferably, the cap is provided with a rebate on an exterior surface thereof for engagement with a complimentary lip of the tube, for securing the cap relative to the tube. In another aspect, there is provided a plunger for use in the above described tube, the plunger having a main body with radial fins projecting therefrom for receipt in the grooves of the tube, between adjacent ribs, the fins being dimensioned to engage lateral edges of the ribs, in a point contact manner. Preferably, the body of the plunger includes a central bulb for driving the sausage into a cap coupled so the tube. Preferably, the plunger includes a reduced dimension region between the bulb and the fins. Preferably, the bulb includes a bore for receipt of an end clip of the sausage. Preferably, the plunger is symmetric and reversible. In another aspect, there is provided a dispensing apparatus including a combination of the tube, cap and plunger, as described above.

Compositions for oral use

An oral composition comprising trifluoromethionine as an effective component is provided as a useful oral composition for preventing and/or treating intraoral diseases such as bad breath, periodontal disease, alveolar pyorrhea, etc., which is safe even if daily used.

1. An oral composition, which comprises trifluoromethionine as an effective component. 2. An oral composition according to claim 1, which is a preparation for preventing and/or treating bad breath. 3. An oral composition according to claim 1, which is a preparation for preventing and/or treating alveolar pyorrhea. 4. An oral composition according to claim 1, which is a preparation for preventing and/or treating periodontal disease.

<SOH> BACKGROUND ART <EOH>Recently, there has been a growing interest in prevention and treatment of intraoral diseases such as bad breath, alveolar pyorrhea, periodontal disease, etc. Most important causative substances of bad breath are so-called volatile sulfides such as hydrogen sulfide, methylmercaptan and dimethyl sulfide, among which methylmercaptan is known to be produced by many causative organisms of periodontisis and thus has been watched with interest as an indicator of periodontisis and also as one of pathogenic factors of periodontisis. The methylmercaptan is produced from methionine by L-methionine-α-deamino-γ-mercaptomethane-lyase(METase) as an enzyme contained in bacteria. Among causative organisms of periodontal disease, well known organisms capable of efficiently producing methylmercaptan include bacteria of genus Porphyromonas such as Porphyromonas gingivalis, etc., bacteria of genus Fusobacterium such as Fusobacterium nucleatum, etc. Thus, it can be presumed that prevention and treatment of the above-mentioned intraoral diseases can be effectively attained by inhibiting propagation of these bacteria, and the ordinary antibacterial active substances have a possibility to kill the bacteria, thereby effectively attaining prevention and treatment of bad breath, etc. However, the ordinary antibacterial active substances can kill even intraoral indigenous bacteria free from pathogenicity, and thus are not recommendable from the viewpoint of preventing fixation of harmful exogenetic bacteria. Thus, it has been presumed useful to find substances having a bactericidal effect or a growth inhibiting effect selectively on the methylmercaptan-producing organisms, which have been presumed to cause the above-mentioned intraoral diseases.

<SOH> BRIEF DESCRIPTION OF THE DRAWINGS <EOH>FIG. 1 is a diagram showing results of antibacterial effect tests of trifluoromethionine as an effective component of the present oral composition on the strain Porphyromonas gingivalis W83. FIG. 2 is a diagram showing results of antibacterial effect tests of trifluoromethionine as an effective component of the present oral composition on the strain Porphyromonas gingivalis ATCC33277. FIG. 3 is a diagram showing results of antibacterial effect tests of trifluoromethionine as an effective component of the present oral composition on the strain Porphyromonas gingivalis M1217. FIG. 4 is a diagram showing results of antibacterial effect tests of trifluoromethionine as an effective component of the present oral composition on the strain Fusobacterium nucleatum ATCC10953. FIG. 5 is a diagram showing results of antibacterial effect tests of trifluoromethionine as an effective component of the present oral composition on the strain Actinobacillus actinomycetemcomitans Y4. FIG. 6 is a diagram showing results of antibacterial effect tests of trifluoromethionine as an effective component of the present oral composition on the strain Escherichia coil BL21. detailed-description description="Detailed Description" end="lead"?

Sulphur-containing amphiphilic agents for the transfer of biologically active molecules into cells

The present invention relates to amphiphilic, cationic sulpho-substituted phosphatidyl ethanolamine analogs and their salts, which are capable of complexing biopolymers such as DNA, RNA, oligonucleotides, ribozymes, proteins and peptides and to infiltrate them into eukaryotic cells. Particularly suitable are compounds which are derived from 1,2-dioleoyl-3-sn-phosphatidyl ethanolamine (DOPE) and in which the phosphoric acid ester group of DOPE is replaced by an isosteric group CH2—SO—CH2 or CH2—S(O)2—CH2. Because of their property of forming aggregates with biologically active molecules, such as for example DNA or RNA, there compounds are particularly suitable for application in gene therapy, but also for diagnostic purposes.

1. Sulfur-containing amphiphiles of the general formula I: in which R1 denotes a straight or branched chain, saturated or unsaturated alkyl or acyl residue with 10-24 carbon atoms, a denotes a group O—R2 or CH2—O—R2, in which R2 has the meaning given for R1 and may be the same as R1 or different from R1, where with the presence of a steric center, the methine carbon atom connected to A can be present in R- or S-configuration or racemic, X denotes a group Y denotes a group N+R3R4R5Z− or a group NR3R4, where R3-R5, independently of each other, denote hydrogen, an alkyl group with 1-4 carbon atoms, a group —(CH2)i—OH, or a group —(CH2)i—NH2 with i=2-6 and Z− denotes a pharmaceutically acceptable anion, and where m and n, independently of each other, denote an integer 1-6. 2. Compounds according to claim 1, wherein the residue R1 is an acyl residue from the group of lauroyl, myristoyl, palmitoyl, steroyl, oleoyl, linoloyl, or linoleoyl, m=2 and n=3. 3. Compounds according to claim 1 or 2, wherein R1 is a lauroyl, myristoyl or oleoyl residue, the group A is a lauroyloxy, myristoyl or oleoyl, m=2 and n=3, X is a —SO— or —SO2— group, and Y is an —NH3+Z− group or an —NH2 group. 4. Compounds according to one of claims 1-3, wherein the pharmaceutically acceptable anion is an ion from the group of halide, acetate, trifluoroacetate, mesylate, besylate, phosphate, tartrate, or citrate. 5. Use of a reagent for the transfer of biologically active, anionic macromolecules into eukaryotic cells for pharmaceutical or diagnostic purposes, wherein aggregates are formed from the reagent, which contains at least one compound of claims 1-4, where in addition further lipoid compounds may be admixed in different proportions, with the biologically active, anionic macromolecules, and these aggregates are brought into contact with the cells in vivo or in vitro. 6. Use of a reagent according to claim 5, wherein as the biologically active, anionic macromolecules, DNA, RNA, antisense DNA, antisense RNA, oligonucleotides, ribozymes, peptides or proteins are concerned. 7. Use of a reagent according to claim 5 or 6, wherein the additionally admixed lipoid compounds belong to the phospholipids or steroid classes, 1,2-dioleoyl-sn-glycero-3-phosphoethanolamine being particularly suitable. 8. Use of a reagent according to one of claims 5-7, wherein the reagent is present as a dispersion in aqueous media or as a solution in a solvent miscible with water, and in the case of an aqueous dispersion cryoprotective media from the group of lactose, trehalose, sucrose, glucose, fructose, galactose, maltose, mannitol or polyethylene glycol can be dissolved at the same time. 9. Use of a reagent according to one of claims 5-8, wherein the biologically active anionic macromolecules may be present as complexes with polycationic molecules from the group of spermine, spermidine, protamine sulfate, histone H1, histone H2A, histone H2B, histone H3, histone H4, HMG1 or HMG17 protein. 10. Use of a reagent according to one of claims 5-9, wherein the aggregates formed from the lipids and the anionic macromolecules are stored in lyophilized form, and are rehydrated in a suitable aqueous medium before use.

Optical system having a holographic optical element

An optical laser system wherein a holographic optical element (HOE) replaces a bulky feedback system comprising a large number of optical element. The feedback system is adjusted so that the laser device and the feedback system cooperate to select a state having a high temporal and/or spatial coherence, and the optical properties of the optical elements are recorded into the HOE. When the feedback system is removed the HOE reproduces the properties of the optical elements of the feedback system. The laser system is compact in size, cheap to manufacture, has high mechanical stability, and is less fragile than ordinary feedback systems. The laser system may be used in environments, such as the printing industry, which normally do not permit an ordinary feedback system, e.g. due to mechanical vibrations or misalignment due to temperature variations. A number of centre frequencies may be multiplexed into the HOE. May be mass produced. Furthermore, a method of producing such an optical laser system.

1. An optical system for emission of an output light beam, wherein a holographic optical element reproduces the optical properties of a plurality of optical elements, the plurality of optical elements forming a feedback system being adapted to cooperate with a laser device to select a high temporal and/or spatial coherent state of the laser device. 2. An optical system according to claim 1, wherein at least one of the plurality of optical elements is selected from the group consisting of: spatial filters, gratings, mirrors, Fabry Perot etalons, frequency filters. 3. A method of producing an optical system for emission of an output beam, the method comprising the steps of: inserting a holographic recording material into an external cavity formed between a laser device and a feedback system, said feedback system comprising a plurality of optical elements, emitting, by means of the laser device, a first light beam, at least part of said first light beam illuminating at least part of the feedback system via said holographic recording material, adjusting the feedback system so that the laser device and the feedback system cooperate to select a state having a high temporal and/or spatial coherence, recording a holographic optical element in the holographic recording material, developing the holographic optical element so that the holographic optical element is adapted to reproduce the optical properties of the plurality of optical element when said feedback system is removed, and removing the feedback system. 4. A method according to claim 3, the method comprising the steps of, for each of the optical elements: adjusting the feedback system so that the laser device and the feedback system cooperate to select a state having a high temporal and/or spatial coherency, recording a holographic optical element in the holographic recording material, repeating the adjusting and recording steps until the properties of eachof the plurality of optical elements has been recorded, and performing the development after the optical properties of all the optical elements have been recorded and removing the feedback system when the holographic optical element has been developed. 5. A method according to claim 3 or 4, wherein at least one of the plurality of optical elements is selected from the group consisting of: spatial filters, gratings, mirrors, Fabry Perot etalons, frequency filters. 6. A method according to any of claims 3-5, further comprising the step of positioning the holographic optical element in connection with a laser device, so that the holographic optical element and the laser device may cooperate to select a state having a high temporal and/or spatial coherency. 7. A method according to any of claims 4-6, further comprising the step of multiplexing a plurality of centre frequencies into the holographic optical element. 8. A method according to claim 7, the method further comprising the steps of, for each of the plurality of centre frequencies: adjusting the feedback system to emit a centre frequency feedback light beam so that the laser device and the feedback system cooperate to select a state having a high temporal and/or spatial coherency, and so that a specific centre frequency is obtained, recording a holographic optical element in the holographic recording material, repeating the adjusting and recording steps until each of the plurality of centre frequencies has been recorded, and performing the development after all the centre frequencies have been recorded and removing the feedback system when the holographic optical element has been developed. 9. A method according to any of claims 3-8, wherein the developing step is performed using a chemical or thermal fixing procedure. 10. A method according to any of claims 3-9, wherein the laser system is a compact laser system. 11. A compact laser system for emission of an output light beam, the system comprising: alaser device for emission of a first light beam, and a holographic optical element being illuminated by at least a part of the first light beam, thereby causing a feedback light beam to be emitted from the holographic optical element and being reinjected into the active gain medium of the laser device, whereby the laser device and the holographic optical element cooperate to select a high spatial and/or high temporal coherent state of the laser device, whereby the laser system is controlled to emit an output light beam having an improved spatial and/or temporal coherence. 12. A laser system according to claim11, wherein the holographic optical element is adapted to reconstruct an original light beam from a feedback system. 13. A laser system according to claim 12, wherein the feedback system comprises one or more optical elements selected from the group consisting of: spatial filters, gratings, lenses, mirrors, Fabry Perot etalons, frequency filters. 14. A laser system according to any of claims 11-13, wherein the holographic optical element is adapted to, in coopreation with the laser device, select at least one centre frequency from the first light beam. 15. A laser system according to any of claims 11-14, wherein the holographic optical element is adapted to, in cooperation with the laser device, select a plurality of centre frequencies, each centre frequency being multiplexed into the holographic optical element. 16. A laser system according to any of claims 11-15, wherein the laser device comprises a laser array. 17. A laser system according to any of claims 11-16, wherein the laser device comprises at least one laser selected from the group consisting of: broad area lasers, laser diode arrays, laser diode bars, stacked laser arrays. 18. A method of generating an output light beam from a laser system comprising a laser device and a holographic optical element, the method comprising the steps of: emitting, by means of the laser device, a first light beam in such a way tha t at least part of the holographic optical element is illuminated by at least part of the first light beam, injecting, by means of the holographic optical element and in response to the first light beam, a feedback light beam into the laser device, and outputting, by means of the holographic optical element and in response to the first light beam, an output light beam from the laser system, said output light beam having an imptoved spatial and/or temporal coherence state. 19. A method according to claim 18, wherein the feedback system comprises one or more optical elements selected from the groupt consisting of: spatial filters, gratings, lenses, mirrors, Fabry Perot etalons, frequency filters. 21. A method according to any of claims 18-20, further comprising the steps of, by means of the holographic optical element in cooperation with the laser device, selecting at least one centre frequency from the first light beam. 22. A method according to any of claim 18-21, further comprising the steps of, by menas of the holographic optical element in cooperation with the laser device, selecting at least one centre frequency from the first light beam. 23. A method of producing a compact laser system for emission of an output light beam, the method comprising the steps of: inserting a holographic recording material into a laser cavity formed between a laser device and a feedback system, emitting, by means of te laser device, a first light beam, at least part of said first light beam illuminating at least part of the feedback system via said holographic recording material, adjusting the feedback system to emit a feedback light beam so that the laser device and the feedback system cooperate to select a state having a high temporal and/or spatial coherency, recording a holographic optical element in the holographic recording material, developing the holographic optical element so that the holographic optical element is capable of reconstructing the feedback light beam from the feedback system when said feedback system is removed, and removing the feedback system. 24. A method according to claim 23, further comprising the step of multiplexing a plurality of centre frequencies into the holographic optical element. 25. A method according to claim 24, the method further comprising the steps of, for each of the plurality of centre frequencies: adjusting the feedback system to emit a centre frequency feedback light beam so that the laser device and the feedback system cooperate to select a state having a high temporal and/or spatial coherency, and so that a specific centre frequency is obtained, recording a holographic optical element in the holographic recording material, repeating the adjusting and recording steps until each of the plurality of centre frequencies has been recorded, and performing the development after all the centre frequencies have been recorded and removing the feedback system when the holographic optical element has been developed. 26. A method according to any of claims 23-25, wherein the developing step is performed using a chemical or thermal fixing procedure.

<SOH> BACKGROUND OF THE INVENTION <EOH>From WO 98/56087, it is known to use phase conjugate feedback in a laser system in order to obtain a highly coherent, possibly single mode, output light beam. However, the laser system disclosed in WO 98/56087 requires a number of optical elements. Such optical elements are expensive, especially if one of the optical elements comprises an anisotropic ferroelectric crystal, such as a BaTiO 3 crystal. Furthermore, BaTiO 3 crystals have a phase transition near room temperature and consequently they are very fragile and therefore need to be handled with much care. In addition to this, using a large number of optical elements requires a precise alignment of the elements, and it also results in a bulky laser system which is sensitive to mechanical vibrations. The alignment may be difficult to obtain and especially to preserve outside of a laboratory, and, furthermore, the bulky laser system is not very convenient for the user. ‘In Holographic optical head for compact disk applications’, Optical Engineering, Vol. 28(6), pp 650-653, June 1989, is disclosed an optical head for a CD player based on the holographic optical element and laser/detector hybrid technology. The holographic optical elements disclosed in this document are adapted to replace a number of refractive elements, such as lenses, beamsplitters, and diffraction gratings, or optionally a simple mirror. The document further discloses a method of fabrication of computer-generated holographic optical elements. A number of references describe the use of a holographic optical element (HOE) for replacing one or more optical elements. However, none of these references disclose using a HOE for injecting the beam back into the laser in order to improve the spatial and/or temporal properties of the output beam. The HOE is rather used for compensating for ‘beam defects’, such as astigmatism, after the beam has been output from the optical system. WO 99/57579 discloses a method for designing and constructing miniature optical systems and devices employing light diffractive optical elements (DOEs) for modifying the size and shape of laser beams produced from commercial-grade laser diodes. The DOEs may be implemented as holographic optical elements (HOEs). The DOE compensates for ‘beam defects’, such as astigmatism, of a beam emitted from a laser system. The beam is not injected back into the laser. U.S. Pat. No. 6,018,402 discloses the use of a holographic optical element (HOE) to reconstruct optical elements typically used to phaseencode an object beam emanating from a spatial light modulator (SLM). The HOE replaces the complicated phase mask and conventional four-F lens system arrangement typically used to phase-encode an amplitude-encoded object beam emanating from the SLM. Thus, the HOE is in this case used for converting and transforming laser light from one state to another. ‘Recent studies of miniaturization of optical disk pickups in Japan’ by Hiroshi Nishihara, Proceedings of the SPIE—The International Society for Optical Engineering, 1990, USA, vol. 1248, pages 88-95, XP001029989, describes methods for improving pickups for compact disk players. A holographic optical element may be used for improving the output power of the diode laser. Thus, the temporal and/or spatial properties of the beam are not affected by the HOE. It is, furthermore, known to produce holographic optical elements, e.g. for producing bright, sharp, three-dimensional images. In contrast to the applications of HOE and DOE mentioned above the present invention deals with the improvement of the spatial and temporal coherence of high power laser diodes when the HOE or DOE is used to feedback light into the active region of the high power laser diode.

<SOH> SUMMARY OF THE INVENTION <EOH>It is an object of the present invention to provide a laser system which is compact and cheap to manufacture, which is less fragile than known laser systems, and which is less sensitive to misalignment of the optical elements which may be caused, e.g., by mechanical vibrations, temperature changes, etc. It is a further object to provide methods of manufacturing a laser system having the properties described above. It is an even further object to provide an optical system having a simple optical component which provides a passive feedback to the laser system. It is an even further object to provide an optical system in which the output beam has been subject to losses which are substantially smaller than losses caused by known feedback systems. It is an even further object to provide a feedback system with a high mechanical stability. It is an even further object to provide an optical system which is capable of producing an output beam having better spatial and/or temporal properties than the output beam from known systems. It is a very important object of the invention to provide a diode laser system with high output power, in the range of 1 W to 1000 W, which can be focused to a small diffraction limited spot. According to a first aspect of the present invention there is provided an optical system for emission of an output light beam, wherein a holographic optical element reproduces the optical properties of a plurality of optical elements, the plurality of optical elements forming a feedback system being adapted to cooperate with a laser device to select a high temporal and/or spatial coherent state of the laser device. The output light beam is emitted from the optical system, i.e. it is available for other purposes. That is, the output light beam may be used as a source of electromagnetic radiation. Thus, the output light beam is an electromagnetic output beam, such as a light beam, an ultraviolet beam, a microwave beam, an X-ray beam, or any other suitable kind of electromagnetic beam. The optical properties of the optical elements may be any suitable kind of optical properties, such as refractive index, reflectivity, selection of, e.g., frequencies or spatial modes, frequency doubling, etc., depending on which kinds of optical elements are used. The plurality of optical elements which may be reproduced by the holographic optical element form a feedback system being adapted to cooperate with a laser device to select a high temporal and/or spatial coherent state of the laser device. The laser device, thus, being adapted to supply a first light beam to the optical system, and the laser device and the holographic optical element reproducing the optical properties of the optical system may then cooperate to select a high temporal and/or spatial coherent state of the laser device. The feedback system used to improve the coherence properties of laser systems may be an optical system reflecting at least a part of the first light beam emitted from the laser device back into the laser device. In cooperation, the feedback system and the laser device then force the laser device to emit laser radiation with a high temporal and/or spatial coherence. When a high temporal coherent state is selected, the output light beam of the system, thus, comprises radiation within a very narrow frequency range, and, preferably, the output light beam substantially comprises only a single frequency. When a high spatial coherent state is selected the output light beam may be focused to a small spot size of the order of a wavelength. This is an important property for a large number of applications. Preferably, at least one of the plurality of optical elements is selected from the group consisting of: spatial filters, gratings, mirrors, Fabry Perot etalons, frequency filters. It is a great advantage of the present invention that a HOE is used as a feedback system. Thus, a HOE is substantially less expensive than a large number of optical elements. Furthermore, the size of the entire optical system is substantially reduced, and the system is much more stable, e.g. with respect to vibrations, misalignments, etc. Thus, the HOE may be attached to the laser facet itself, thereby substantially improving the mechanical stability properties of the optical system. Also, the HOE provides a passive feedback system as opposed to the active feedback system provided by a feedback system comprising non-linear optical components. This is a great advantage because in comparison with the active feedback the passive feedback only uses low cost elements. Finally, a feedback system being represented by a HOE may introduce fewer losses than a feedback system comprising the actual optical components which the HOE represents. This is because it is possible to let the HOE reproduce other optical properties of the individual optical component without reproducing the loss characteristics of that component. In case the HOE represent a large number of optical components, this is a very important advantage since the entire system may introduce very heavy losses. A spatial filter may, e.g., be an aperture, a slit, a pinhole or any other suitable kind of spatial filter. The optical properties of a spatial filter which may be reproduced by the holographic optical element in this case preferably comprise selection of specific modes or frequencies. In case one of the optical elements is a grating, the optical properties to be reproduced by the holographic optical element preferably comprise a frequency selectivity. In case one of the optical elements is a mirror, the optical properties to be reproduced by the holographic optical element preferably comprise the reflective properties of the mirror, such as a frequency dependent reflectivity, i.e. the reflectivity of the mirror at a certain frequency, the tilt angle of the mirror, and/or any focusing properties of the mirror. The mirror may be a plane mirror, a parabolic mirror, a spherical mirror, a mirror with a spatial selectivity, or a mirror having any other suitable shape. A frequency filter may e.g. comprise a grating, such as a diffractive optical element, preferably in combination with a spatial filter, such as an aperture or a slit, or it may be a filter which transmits electromagnetic radiation within a specific frequency range and reflects or absorbs any other frequencies. It may comprise an interference filter, an absorbance filter, such as a semiconductor doped glass, an etalon, such as a Fabry Perot element, a prism etc. The frequency filter may be adapted to select a range of frequencies, preferably a narrow range, most preferably a single frequency. In case one of the optical elements is a frequency filter, the optical properties to be reproduced by the holographic optical element preferably comprise frequency selection, transmission/reflection/absorption properties, selection of modes, reflective properties, refractive index, transmission properties, reflectivity, interference properties (destructive and/or constructive), or any other suitable properties of the frequency filter. According to a second aspect the present invention further provides a method of producing an optical system for emission of an output light beam, the method comprising the steps of: inserting a holographic recording material into an external cavity formed between a laser device and a feedback system, said feedback system comprising a plurality of optical elements, emitting, by means of the laser device, a first light beam, at least part of said first light beam illuminating at least part of the feedback system via said holographic recording material, adjusting the feedback system so that the laser device and the feedback system cooperate to select a state having a high temporal and/or spatial coherence, recording a holographic optical element in the holographic recording material, developing the holographic optical element so that the holographic optical element is adapted to reproduce the optical properties of the plurality of optical element when said feedback system is removed, and removing the feedback system. The holographic recording material may be any material with a photosensitive refractive index and/or absorption coefficient for example a dichromatic gelatine, a Silver Bromide (AgBr) solution, photo resist, and/or a photorefractive medium. The laser device may be a single laser, e.g. a gas laser, a semiconductor laser, a broad area laser, a superluminescent laser diode, a dye laser, a Nd-YAG laser, an argon ion laser, a titanium sapphire laser, an F-center laser, or any other suitable kind of laser. It may also be an array of lasers, said lasers being of any of the types mentioned above. The feedback system is defined above. Adjusting the feedback system may comprise adjusting one or more of the optical elements forming the feedback system in such a way that a state having a high temporal and/or spatial coherency is selected. The adjusting step may, furthermore, comprise alignment of the optical elements. Additionally or alternatively, the adjusting step may comprise adjusting one or more optical element(s) in such a way that, e.g., a certain frequency, a certain spatial mode, etc. is selected. This may, for example, be done in the following way. In a preferred embodiment of the invention, the feedback system comprises a reflector, the reflector being adapted to reflect at least a part of the first light beam emitted by the laser device back into the laser device. The free running laser emits a large number of spatial modes. By using spatial filtering for example in the Fourier plane, e.g. by means of one or more spatial filter(s), such as aperture(s), slit(s), pinhole(s), etc., the system is adjusted to emit laser light having a high temporal and/or spatial coherency. The feedback system may, furthermore, comprise a grating or an etalon so that the frequency of the first light beam may be tuned by tilting the grating or the etalon. It is, thus, possible to adjust the system to emit an output light beam having, e.g., a certain spatial mode, frequency, etc., depending on the optical elements being provided in the feedback system. When the feedback system has been adjusted so that the output light beam has the desired properties, a holographic optical element having these properties is recorded in the holographic recording material positioned between the laser device and the feedback system. When the holographic optical element is subsequently developed, it will thus be adapted to reproduce the optical properties of the elements in the feedback system. The feedback system may then be removed and the holographic optical element will act as the feedback system, i.e. the output beam will have the same desired properties which the feedback system was adjusted to provide. Of course, the recorded and developed holographic optical element itself may not afterwards be adjusted as the feedback system, thus, limiting the flexibility of the system. However, it is an advantage of the system according to the present invention that the system provided is substantially non-sensitive to misalignments due to vibrations, temperature variations, etc. It is a further advantage that a rather bulky, expensive, and fragile feedback system may be replaced by the compact, cheap, and reliable holographic optical element. These advantages makes the system very advantageous for commercial purposes. It is, thus, possible to use to system under conditions which are normally not suited for a feedback system comprising a large number of fragile optical components, e.g. in an environment introducing vibrations, temperature variations, a dirty environment, etc. It is possible to manufacture HOEs under ideal conditions and subsequently position the HOEs in optical systems under less ideal conditions. Thus, an ideal feedback system is provided even though the environment is not suited for such a feedback system. Furthermore, the price of the entire system will be sufficiently low to attract potential customers. The system may, thus, advantageously be used, e.g., in the printing industry, medical applications, or telecommunication. In a very preferred embodiment laser systems having a HOE replacing a feedback system may be mass produced by recording one HOE by the method described above, and subsequently reproduce this HOE. The reproduced HOEs may then be positioned in laser systems having similar properties. It should be noted that the HOE in each case should be positioned in the laser system in a position corresponding to the position in which the original HOE was recorded in order for the HOE to properly reproduce the feedback system. Such mass produced laser systems are very advantageous from a commercial point of view since they are very cheap to manufacture, and the price therefore will be acceptable for potential customers. The method may comprise the steps of, for each of the optical elements: adjusting the feedback system so that the laser device and the feedback system cooperate to select a state having a high temporal and/or spatial coherency, recording a holographic optical element in the holographic recording material, repeating the adjusting and recording steps until the properties of each of the plurality of optical elements has been recorded, and performing the development after the optical properties of all the optical elements have been recorded and removing the feedback system when the holographic optical element has been developed. In this case, the adjusting and recording steps are performed for each optical element of the feedback system. Thus, each optical element is in turn adjusted to achieve a desired optical property of the optical element in question. This optical property is then recorded. In order to record the optical properties of all the optical elements into the same holographic optical element, the holographic optical recording material is not developed until all the optical properties have been recorded. At least one of the plurality of optical elements may be selected from the group consisting of: spatial filters, gratings, mirrors, Fabry Perot etalons, frequency filters. These optical elements and their optical properties have been described above. Preferably, the method further comprises the step of positioning the holographic optical element in connection with a laser device, so that the holographic optical element and the laser device may cooperate to select a state having a high temporal and/or spatial coherency. That is, the holographic optical element may preferably be used to replace the feedback system in order to provide a compact, cheap, and mechanically stable laser system as described above, and as will be further described below. The method may further comprise the step of multiplexing a plurality of centre frequencies into the holographic optical element. In an embodiment where the feedback system comprises a grating, this may be performed in the following way. The feedback system may be adjusted to select one centre frequency and a corresponding grating may be induced in the holographic optical element. The laser device may then be turned off and the grating be tilted to select a new centre frequency. When the laser device is turned on again, a new hologram with a new centre frequency may be written into the holographic optical recording material. By repeating this procedure for each centre frequency, a plurality of frequencies are written into the holographic recording material. When all the desired frequencies have been written into the holographic recording material, the holographic optical element is developed, so as to obtain a holographic optical element having all the desired centre frequencies multiplexed into it. Thus, the method may further comprise the steps of, for each of the plurality of centre frequencies: adjusting the feedback system to emit a centre frequency feedback light beam so that the laser device and the feedback system cooperate to select a state having a high temporal and/or spatial coherency, and so that a specific centre frequency is obtained, recording a holographic optical element in the holographic recording material, repeating the adjusting and recording steps until each of the plurality of centre frequencies has been recorded, and performing the development after all the centre frequencies have been recorded and removing the feedback system when the holographic optical element has been developed. The developing step may be performed using a chemical or thermal fixing procedure. Alternatively, the holographic recording material may be of a kind which is ‘self-developing’. In this case the development is performed automatically and does not require an active act. This is known per se. The laser system may advantageously be a compact laser system. According to a third aspect the invention further provides a compact laser system for emission of an output light beam, the system comprising: a laser device for emission of a first light beam, and a holographic optical element being illuminated by at least a part of the first light beam, thereby causing a feedback light beam to be emitted from the holographic optical element and being reinjected into the active gain medium of the laser device, whereby the laser device and the holographic optical element cooperate to select a high spatial and/or high temporal coherent state of the laser device, whereby the laser system is controlled to emit an output light beam having an improved spatial and/or temporal coherence. As described above the laser device may be any suitable kind of laser device, such as a gas laser, a semiconductor laser, a superluminescent laser diode, a dye laser, a Nd-YAG laser, an argon ion laser, a titanium sapphire laser, an F-center laser, or any other suitable kind of laser. It may also be an array of lasers, said lasers being of any of the types mentioned above. The first light beam may be an electromagnetic beam, preferably a monochromatic electromagnetic beam. In case the laser device is a single laser, the first light may also be a coherent light beam. In case the laser device is an array of lasers or another laser device having a broad bandwidth gain medium, the first light beam will in most cases have a very low degree of coherence. The holographic optical element is illuminated by at least part of the first light beam. It may, of course, be illuminated by all of the first light beam. At least part of the holographic optical element may be illuminated, or all of the holographic optical element may be illuminated. The feedback light beam is emitted from the holographic optical element in response to the first light beam illuminating the holographic optical element. The feedback light beam may be an electromagnetic beam, such as an electromagnetic beam comprising frequencies within the visible frequency range, the ultraviolet frequency range, the infrared frequency range, the X-ray frequency range, or any other suitable frequency range. The feedback light beam may be e.g. a complete reflection of the first light beam. Alternatively, it may be a reflected part of the first light beam, such as a part defined by a specific frequency range, a specific polarisation, a specific spatial mode, etc. Alternatively, the feedback light beam may be a beam which is generated by the holographic optical element in response to the first light beam. The feedback light beam is reinjected into the active gain medium of the laser device. In this way the laser device and the holographic optical element cooperate to select a high spatial and/or temporal coherent state of the laser device. The output light beam from the system will then have a high spatial and/or temporal coherent state. In order to obtain a high power, the laser device is often an array of lasers as described above. As mentioned above, this will very often result in a first light beam having a low degree of coherence. Since the output light beam has a high spatial and/or temporal coherent state, it thus has an improved spatial and/or temporal coherence as compared to the first light beam being emitted from the laser device. Thereby, the compact laser system is adapted for improving the coherency of a high power laser beam. The holographic optical element may be adapted to reconstruct an original light beam from a feedback system. The feedback system may comprise a number of optical elements as described above, and it is preferably operated as described above. The holographic optical element may, thus, replace the bulky, expensive, and fragile optical elements of the feedback system. Since a holographic optical element is compact, cheap, and less fragile than most ordinary optical elements, the resulting laser system will also be compact, cheap, and less fragile than laser systems having an ordinary feedback system comprising a number of optical elements. Furthermore, the resulting laser system will not be subject to misalignments due to, e.g., vibrations or temperature variations to the same extend that an ordinary laser system is. The feedback system may comprise one or more optical elements selected from the group consisting of: spatial filters, gratings, lenses, mirrors, Fabry Perot etalons, frequency filters. Most of these optical elements as well as their optical properties have been described above. The original light beam from the feedback system which the holographic optical element is adapted to reconstruct, preferably comprises information relating to the optical properties of the optical elements of the feedback system. The holographic optical element is most preferably recorded in such a way that these optical properties may be reproduced by the holographic optical element. Thus, the output light beam from the compact laser system may be substantially identical to the output light beam from a more bulky laser system having an ordinary feedback system. In case one of the optical elements is a lens, the optical properties to be reproduced by the holographic optical element preferably comprise refractive index, reflectivity, including internal reflectivity, focal length, radius of curvature, or any other suitable optical properties of the lens. The lens may be an ordinary concave or convex lens, or it may be another kind of refractive optical element, such as a prism. The holographic optical element may be adapted to, in cooperation with the laser device, select at least one centre frequency from the first light beam. This corresponds to selecting a high temporal coherent state. However, the exact value of the centre frequency may also be selected in this embodiment. This may e.g. be obtained by recording the holographic optical element using a feedback system which may be tuned so as to select a specific frequency. The holographic optical element may be adapted to, in cooperation with the laser device, select a plurality of centre frequencies, each centre frequency being multiplexed into the holographic optical element. This may be obtained by consecutively tuning a system as described above to each of the plurality of centre frequencies, and recording and developing the holographic optical element in such a way that all the centre frequencies are multiplexed into the holographic optical element. This procedure will be further described below. The laser device may comprise a laser array, such as an array of diode lasers, gas lasers, semiconductor lasers, dye lasers, Nd-YAG lasers, argon ion lasers, or any other suitable kind of lasers. Alternatively, it may be a single laser as described above. The laser device may comprise at least one laser selected from the group consisting of: broad area lasers, laser diode arrays, laser diode bars, stacked laser arrays. Broad area lasers and laser diode arrays comprise a number of diode lasers arranged in a row. Laser diode bars also comprise a number of diode lasers arranged in a row. However, the lasers of a laser diode bar are spatially separated, so that the light sources may be considered as a number of discrete point sources. Stacked laser arrays comprise a number of laser diode bars being stacked, so as to form a two-dimensional array of diode lasers. The above-mentioned types of lasers all provide an output beam having a high power, but a low degree of coherence. For some applications, it may therefore be necessary to improve the coherency of the output beam. This may be done as previously described. According to a fourth aspect the invention further provides a method of generating an output light beam from a laser system, the laser system comprising a laser device and a holographic optical element, the method comprising the steps of: emitting, by means of the laser device, a first light beam in such a way that at least part of the holographic optical element is illuminated by at least part of the first light beam, injecting, by means of the holographic optical element and in response to the first light beam, a feedback light beam into the laser device, and outputting, by means of the holographic optical element and in response to the first light beam, an output light beam from the laser system, said output light beam having an improved spatial and/or temporal coherence state. The first light beam, the feedback light beam, as well as the output light beam may be electromagnetic beams as described above. All of, or at least part of, the holographic optical element may be illuminated by the first light beam, and it may be illuminated by all of, or at least part of, the first light beam. The feedback light beam may be a fully or a partial reflection of the first light beam, or it may be generated by the holographic optical element, as described above. The laser device and the holographic optical element cooperate to select a state having a high temporal and/or spatial coherence, so that the output light beam has an improved spatial and/or temporal coherence as compared to the first light beam which is initially emitted from the laser device. This has been described above. The holographic optical element may reconstruct an original light beam from a feedback system. This has already been described. The feedback system may comprise one or more optical elements selected from the group consisting of: spatial filters, gratings, lenses, mirrors, Fabry Perot etalons, frequency filters. These optical elements as well as their optical properties have been described above. The method may further comprise the step of, by means of the holographic optical element in cooperation with the laser device, selecting at least one centre frequency from the first light beam. As described above this corresponds to selecting a state having a high temporal coherence. However, a specific frequency is chosen in this case. The method may further comprise the step of, by means of the holographic optical element in cooperation with the laser device, selecting a plurality of centre frequencies, each centre frequency having previously been multiplexed into the holographic optical element. This has also been described above. According to a fifth aspect the invention further provides a method of producing a compact laser system for emission of an output light beam, the method comprising the steps of: inserting a holographic recording material into a laser cavity formed between a laser device and a feedback system, emitting, by means of the laser device, a first light beam, at least part of said first light beam illuminating at least part of the feedback system via said holographic recording material, adjusting the feedback system to emit a feedback light beam so that the laser device and the feedback system cooperate to select a state having a high temporal and/or spatial coherency, recording a holographic optical element in the holographic recording material, developing the holographic optical element so that the holographic optical element is capable of reconstructing the feedback light beam from the feedback system when said feedback system is removed, and removing the feedback system. The laser device may be any suitable kind of laser device as described above. The feedback system preferably comprises a number of optical elements each having specific optical properties. The first light beam as well as the feedback light beam may be electromagnetic beams as described above. The adjusting step is preferably performed by adjusting each of the optical elements of the feedback system. This may comprise tilting gratings to the correct angle, e.g. in order to obtain a specific frequency, positioning spatial filters correctly, e.g. in order to obtain a specific spatial mode, aligning the optical elements, e.g. in order to optimise the throughput of the system, and/or it may comprise any other suitable kind of adjusting of the feedback system. The adjusting step results in that the laser device and the feedback system, by means of the feedback light beam, cooperate to select a state having a high temporal and/or spatial coherency. The adjusting may be performed using spatial filtering in the Fourier plan. The holographic recording material may comprise a dichromatic gelatine, a silver bromide (AgBr) solution, photo resist, and/or a photorefractive medium, such as a lithium niobate crystal. When the holographic optical recording material has been developed to form the holographic optical element, the holographic optical element is capable of reconstructing the feedback light beam from the feedback system because the optical properties of the optical elements of the feedback system have been recorded into the holographic optical element. When the feedback system is removed, the laser device and the holographic optical element may therefore be able to cooperate to select a state having a high temporal and/or spatial coherency. That is, the output light beam emitted from the laser system with the feedback system removed will be substantially identical to the output light beam emitted from the laser system with the feedback system present instead of the holographic optical element. Thus, as described above, the holographic optical element may replace the rather bulky, expensive, etc. feedback system, thereby providing a laser system which is compact, cheap, etc. The method may further comprise the step of multiplexing a plurality of centre frequencies into the holographic optical element. Thus, the method may further comprise the steps of, for each of the plurality of centre frequencies: adjusting the feedback system to emit a centre frequency feedback light beam so that the laser device and the feedback system cooperate to select a state having a high temporal and/or spatial coherency, and so that a specific centre frequency is obtained, recording a holographic optical element in the holographic recording material, repeating the adjusting and recording steps until each of the plurality of centre frequencies has been recorded, and performing the development after all the centre frequencies have been recorded and removing the feedback system when the holographic optical element has been developed. This has already been described above. A laser system according to the present invention may be used for a number of various applications, such as frequency doubling, coupling of light into thin core or single mode laser fibres, material processing, the printing industry, biomedical application, and/or any other suitable applications in which a compact, low cost, and reliable laser system is useful. The first, second, third, fourth, and fifth aspects of the present invention may each be combined with one or more of the other aspects of the present invention.

Device for combustion of a carbon containing fuel in a nitrogen free atmosphere and a method for operating said device

The present invention relates to a device for combustion of a carbon containing fuel in a nitrogen free atmosphere, and a method for operating said device. The device may be integrated with a power generation plant (i.e. gas turbine(s)) to obtain an energy efficient process for generation of power with reduced emission of carbon dioxide and NOx to the atmosphere. Furthermore, the device may be integrated with a chemical plant performing endothermic reactions.

1-17. (Cancelled). 18. A device for combustion of a carbon containing fuel in a nitrogen free atmosphere, wherein said device comprises a hollow shell having an inlet for conveying said fuel, an inlet for conveying a compressed oxygen containing gas stream, an outlet for discharging an oxygen depleted gas stream and an outlet for discharging a bleed stream; and said shell encloses one or more heat exchange modules arranged to heat the incoming compressed oxygen containing gas stream; one or more mixed conducting membrane modules arranged to separate oxygen from said oxygen containing gas stream resulting in an oxygen rich gas stream and said oxygen depleted gas stream; a first and possibly a second combustion chamber for combustion of said fuel having an inlet connected to said inlet for fuel to convey fuel to said chamber, an inlet connected to said heat exchange module(s) to convey hot oxygen rich gas to said chamber and an outlet connected to said membrane module(s) to convey exhaust gas from the combustion chamber to the membrane module; a pressure booster installed prior to the first combustion chamber; means (11,21) for connecting said heat exchanger module(s) and membrane module(s); means (7,23) for connecting said heat exchanger module(s) and said membrane module(s) to the inlet for the compressed oxygen containing gas stream and the outlet for the oxygen depleted gas stream and means for conveying a part of said exhaust gas stream directly to said heat exchange module(s) and back to said inlet from the combustion chamber. 19. A device according to claim 18, wherein said heat exchange module(s), said membrane module(s), said means (7,11,21,23), an outlet for said hot oxygen rich gas stream, said outlet for discharged oxygen depleted gas stream, an inlet for said exhaust gas and said inlet for compressed oxygen containing gas stream are all installed in a pressure vessel (reactor). 20. A device according to claim 18, wherein said heat exchange module(s), said membrane module(s), said second combustion chamber, said means (7,11,21,23), an outlet for said hot oxygen rich gas stream, said outlet for discharged oxygen depleted gas stream, an inlet for said exhaust gas and said inlet for compressed oxygen containing gas stream are all installed in a pressure vessel. 21. A device according to claim 18, wherein said modules and said second combustion chamber are vertically interconnected one above the other. 22. A device according to claim 18, wherein said modules are vertically interconnected one above the other. 23. A device according to claim 18, wherein said membrane module is installed between two heat exchange modules. 24. A device according to claim 18, wherein said second combustion chamber is installed between one of the heat exchange module and a membrane module. 25. A device according to claim 19, wherein said outlet for said hot oxygen rich gas stream is connected to the inlet to the first combustion chamber and said inlet for said exhaust gas is connected to the outlet from the first combustion chamber. 26. A device according to claim 18, wherein said pressure booster is a fan or a compressor. 27. A device according to claim 18, wherein said heat exchange module(s) and said membrane module(s) comprise a multichannel monolithic structure. 28. A method for operating a device according to claim 18, wherein said method comprises the following steps: a compressed oxygen containing gas stream is fed to a first heat exchange module where it is heated by means of heat generated by combustion of a fuel in a combustion chamber; said heated gas stream is fed to a mixed conducting membrane module(s) where most of the oxygen is separated from said gas stream and an oxygen depleted gas stream is obtained; a sweep gas is fed to said membrane module to pick up oxygen and the oxygen enriched sweep gas is further fed to a pressure booster; the pressurized sweep gas stream enters the combustion chamber where it is mixed with a fuel for combustion; and said oxygen depleted gas stream is fed to another heat exchange module for further heating before leaving said device. 29. A method for operating a device according to claim 28, wherein said combustion product; the exhaust gas, is applied as sweep gas. 30. A method for operating a device according to claim 28, wherein a part of the exhaust gas is taken out as a bleed stream to prevent accumulation of mass in the device. 31. Use of a device and a method according to claim 18 in a plant for generation of power. 32. Use of a device and a method according to claim 18 in a chemical plant performing an endothermic reaction.

Apparatus and method for preparing cerium oxide nanoparticles

This invention provides a method for preparing cerium oxide nanoparticles with a narrow size distribution. The cerium oxide nanoparticles obtained by the method of the invention are nearly all crystalline. The method comprises providing a first aqueous solution comprising cerium nitrate and providing a second aqueous solution comprising hexamethylenetetramine. The first and second aqueous solutions are mixed to form a mixture, and the mixture is maintained at a temperature no higher than about 320° K to form nanoparticles. The nanoparticles that are formed are then separated from the mixture. A further aspect of the present invention is an apparatus for preparing cerium oxide nanoparticles. The apparatus comprises a mixing vessel having a first compartment for holding a first aqueous solution comprising cerium nitrate and a second compartment for holding a second aqueous solution comprising hexamethylenetetramine. The mixing vessel has a retractable partition separating the first and second compartments. When the retractable partition is retracted, rapid mixing of the first aqueous solution with the second aqueous solution takes place to form a mixture, and the mixture is maintained at a temperature no higher than about 320° K to form nanoparticles therein.

1. A method for preparing cerium oxide nanoparticles comprising the steps of: (a) providing a first aqueous solution comprising cerium nitrate; (b) providing a second aqueous mixture comprising hexamethylenetetramine; (c) rapidly mixing the first aqueous solution with the second aqueous solution to form a mixture; (d) maintaining the mixture at a temperature no higher than about 320° K to form nanoparticles in the mixture; and (e) separating the nanoparticles formed in the mixture from the mixture. 2. The method of claim 1, wherein the first aqueous solution is provided in a first compartment of a mixing vessel, and the second aqueous solution is provided in a second compartment of the mixing vessel, the first and second compartments being separated by retractable partition, and wherein the mixing step comprises retracting the retractable partition of the mixing vessel to cause mixing of the first aqueous solution with the second aqueous solution to form the mixture. 3. The method of claim 1, wherein one of the first and second aqueous solutions is provided in a mixing vessel having at least one inlet, and the other of the first and second aqueous solutions is pumped into the mixing vessels through the at least one inlet to cause rapid mixing of the first and second aqueous solutions to form the mixture. 4. The method of claim 1, wherein the first aqueous solution has a concentration of cerium nitrate in the range of about 0.005 M to about 0.04 M. 5. The method of claim 1, wherein the second aqueous solution has a concentration of hexamethylenetetramine in the range of about 0.05 M to about 1.5 M. 6. The method of claim 5, wherein the concentration of hexamethylenetetramine is in the range of about 0.5 M to about 1.5 M. 7. The method of claim 1, further comprising the step of siring the mixture while the mixture is maintained at a temperature no higher than about 320° K. 8. The method of claim 2, wherein the mixing vessel includes a mechanical stirrer and the mixture is stirred with the mechanical stirrer. 9. The method of claim 8, wherein the mechanical stirrer comprises a vertical stirring rod having a plurality of stirring elements attached thereto. 10. The method of claim 9, wherein the vertical stirring rod has a first aperture for fitting a first inlet feed for introducing the first aqueous solution and a second aperture for fitting a second inlet feed for introducing the second aqueous solution, wherein the first inlet feed leads into the first compartment and the second inlet feed leads into the second compartment of the mixing vessel when the retractable partition is in place. 11. The method of claim 10, wherein the vertical stirring rod further includes an outlet drain for the removal of liquid from the mixing vessel. 12. The method of claim 1, wherein the mixture is maintained at a temperature no higher than about 320° K for a time period between about 2 hours and about 24 hours. 13. The method of claim 12, wherein the time period is between about 5 hours and about 24 hours. 14. The method of claim 12, wherein the time period is between about 12 hours and about 24 hours. 15. The method of claim 1, further comprising the step of sintering the nanoparticles separated in step (e) in air at a temperature in the range of about 400° C. to about 800° C. 16. The method of claim 1, wherein step (e) comprises centrifuging the mixture to separate the nanoparticles from the mixture. 17. The method of claim 2 or 3, wherein the step of separating the nanoparticles from the mixture comprises the steps of positioning the mixing vessel inside a centrifuge and centrifuging the mixture in the mixing vessel. 18. The method of claim 1, wherein the cerium oxide nanoparticles include single crystalline cerium oxide nanoparticles. 19. The method of claim 2, wherein retracting the retractable partition takes place in about 0.1 seconds to about 5 seconds. 20. The method of claim 1, 7, or 12, wherein the mixture is maintained at a temperature of about 300° K to form nanoparticles in the mixture. 21. A method for preparing cerium oxide nanoparticles, comprising the steps of: (a) providing a first aqueous solution comprising cerium nitrate in a mixing vessel; (b) rapidly adding a second aqueous solution comprising hexamethylenetetramine to the first aqueous solution in the mixing vessel to form a mixture; and (c) maintaining the mixture at a temperature no higher than about 320° K to form the nanoparticles in the mixture; and (d) separating the nanoparticles formed in step (c) from the mixture. 22. The method of claim 21, wherein the mixing vessel has at least one inlet, and step (b) comprises rapidly pumping the second aqueous solution through the at least one inlet into the mixing vessel containing the first solution to form the mixture. 23. A method for preparing cerium oxide nanoparticles, comprising the steps of: (a) providing a first aqueous solution comprising hexamethylenetetramine in a mixing vessel; (b) rapidly adding a second aqueous solution comprising cerium nitrate to the first aqueous solution in the mixing vessel to form a mixture; (c) maintaining the mixture at a temperature no higher than about 320° K to form the nanoparticles in the mixture; and (d) separating the nanoparticles formed in step (c) from the mixture. 24. The method of claim 23, wherein the mixing vessel has at least one inlet, and step (b) comprises rapidly pumping the second aqueous solution through the inlet into the mixing vessel containing the first solution to form the mixture. 25. The method of claim 21 or 23, wherein the step of separating the nanoparticles from the mixture comprises centrifuging the mixture. 26. The method of claim 21 or 23, wherein the step of separating the nanoparticles from the mixture comprises positioning the mixing vessel inside a centrifuge, and centrifuging the mixture in the mixing vessel. 27. The method of claim 21 or 23, wherein the mixture is maintained at a temperature of about 300° K to form nanoparticles in the mixture. 28. An apparatus for the preparation of cerium oxide nanoparticles, comprising a mixing vessel having (a) a first compartment for holding a first aqueous solution comprising cerium nitrate; (b) a second compartment for holding a second aqueous solution comprising hexamethylenetetramine; and (c) a retractable partition separating the first and second compartments, wherein when the retractable partition is retracted, rapid mixing of the first and second aqueous solutions takes place to form a mixture, and the mixture in the mixing vessel is maintained at a temperature no higher than 3200K to form nanoparticles therein. 29. The apparatus of claim 28, wherein the retractable partition is a vertical partition. 30. The apparatus of claim 28, wherein the mixing vessel further comprises a mechanical stirrer for stirring the mixture. 31. The apparatus of claim 30, wherein the mechanical stirrer comprises a rotatable vertical stirring rod having a plurality of siring elements attached thereto. 32. The apparatus of claim 31, wherein the vertical stirring rod has a first aperture for fitting a first inlet feed and a second aperture for fitting a second inlet feed, wherein the first aqueous solution is provided through the first inlet feed into the first compartment and the second aqueous solution is provided through the second inlet feed into the second compartment. 33. The apparatus of claim 32, wherein the vertical stirring rod further comprises an outlet drain for the removal of liquid from the mixing vessel. 34. The apparatus of claim 28, further comprising a centrifuge, wherein the mixing vessel is adapted to be positioned inside the centrifuge. 35. The apparatus of claim 28, wherein the mixing vessel is maintained at a temperature of about 300° K to form nanoparticles therein. 36. A method for preparing cerium oxide nanoparticles containing a metal selected from the group consisting of platinum, gold, palladium, copper and nickel, wherein the method comprises the steps of: (a) providing a first aqueous solution comprising cerium nitrate; (b) providing a second aqueous solution comprising hexamethylenetetramine; (c) mixing the first and second aqueous solutions to form a mixture; (d) maintaining the mixture at a temperature no higher than about 320° K, to form nanoparticles therein; (e) separating the nanoparticles formed in step (d) from the mixture; and (f) soaking the nanoparticles separated from the mixture in a solution comprising ions or complex ions of the metal. 37. The method of claim 36, wherein the metal comprises platinum, and step (f) comprises soaking the nanoparticles in a solution comprising chloroplatinic acid. 38. The method of claim 36, wherein the mixture is maintained at a temperature of about 300° K to form nanoparticles therein.

<SOH> BACKGROUND OF THE INVENTION <EOH>1. Field of the Invention The invention is directed to a method and apparatus for the preparation of nanoparticles of cerium oxide. In particular, the invention is directed to a method and apparatus for the preparation of cerium oxide nanoparticles having a narrow size distribution. 2. Background Information Cerium oxide in the form of fine particles is useful as a catalyst for polymerization, for reforming fuels, and for abating polluting gas in automobile exhaust systems. The catalyst acts as an oxygen pressure regulator in the reduction of NO X to molecular nitrogen, the oxidation of hydrocarbons and carbon monoxide to water and carbon dioxide, and the conversion of H 2 S to H 2 and S. Cerium oxide has been used as a catalyst-component for the recombination of hydrogen and oxygen to water for sealed car batteries, which extends battery life. The oxide is a good ionic conductor and has been used as an electrolyte material for a solid oxide fuel cells and gas sensors, as discussed, for example, by Steele, B. C. H., Solids State Ionics , Vol. 12 (1984), p. 391. The oxide has a high dielectric constant and a high refractive index (useful for optical coatings), and can be used as an insulating layer on semiconductor substrates. Cerium oxide is also of interest as a catalyst in vehicle emissions systems, as discussed in Yao, Y. F. and Kummer, J. T., Journal of Catalysis, Vol. 103 (1987), p. 307, and has also found use as a solid oxide fuel cell electrolyte material, as shown in Mogesen, M., Sammes, N. M. and Tompsett, G. A., Solid State Ionics , Vol. 172 (2000), p. 63; in gas sensors, as described in Lampe, U., Gerblinger, J. and Meixner, H., Sensors and Actuators B—Chemical , Vol. 7 (1992), p. 787; in optical coatings, as described in Haas, G., Ramsey, J. B. and Thun, R., Journal of the Optical Society of America , Vol. 48 (1957), p. 324; in high-T c superconductor structures, as discussed in Walkenhorst, A., Schmitt, M., Adrian, H. and Petersen, K., Applied Physics Letters , Vol. 64 (1994), p. 1871; and silicon-on-insulator structures and high storage capacitor devices, as shown by Chikyow, T., Bedair, S. M., Tye, L. and El-Masry, N. A., Applied Physics Letters , Vol. 65 (1994), p. 1030. Because of the relative hardness of the material, cerium oxide nanoparticles are also useful as an abrasive for fine polishing of surfaces of certain materials, such as quartz and silicon. Some applications may benefit from using monodispersed cerium oxide nanoparticles, due to either possibly new properties when such particles are nanodimensional or the greater control in uniform structures. A sub-micron scale cerium oxide powder has been prepared and used to decrease the sintering temperature from 1500° C. to 1200° C., as described by Chen, P. L. and Chen, I. W., Journal of the American Ceramic Society , Vol. 76 (1993), p. 1577; however, there has been no report of any method for preparing cerium oxide nanoparticles having dimensions smaller than about 14.5 nm, and no report of cerium oxide particles having monodispersity. The electrical conductivity of multi-dispersed nanoparticles of cerium oxide prepared by a vacuum technique has been investigated by Chiang, Y. M., Lavik, E. B., Kosacki, I., Tuller, H. L. and Ying, J. Y., Electroceramics , Vol. 1 (1997), p. 7. The vacuum sputtering technique used by Chiang et al. usually yields cerium oxide particles of a large size distribution, which makes it very difficult to test and sort out particle-size effects on the catalytic process for certain reactions. Tsunekawa, S., Sahara, R, Kawazoe, Y. and Ishikawa, K, Applied Surface Science , Vol. 152 (1999), p. 53; and Tsunekawa, S., Ishikawa, K, Li, Z. Q., Kawazoe, Y. and Kasuya, Y., Physics Review Letters , Vol. 85 (2000), p. 3440, both claim to have prepared mono-sized nanoparticles of cerium oxide and reported lattice expansions with decreasing particle-size in a few nanosized cerium oxide particles. Both papers suggest that a decrease in the size of cerium oxide nanoparticles is accompanied by a significant increase in the lattice parameter. Neither paper, however, discloses the method of preparation of cerium oxide nanoparticles or the apparatus used. The foregoing discussion shows that there is a need in the art for an efficient method and apparatus for preparing significant quantities of cerium oxide nanoparticles with a relatively narrow size distribution.

<SOH> SUMMARY OF THE INVENTION <EOH>The aforementioned need is substantially met by the present invention, which in one aspect is a method for preparing cerium oxide nanoparticles. The method comprises providing a first aqueous solution comprising cerium nitrate and providing a second aqueous solution comprising hexamethylenetetramine. The first and second aqueous solutions are mixed to form a mixture, and the mixture is maintained at a temperature no higher than about 320° K to form nanoparticles therein. The nanoparticles that are formed are then separated from the mixture. Another aspect of the present invention is a method for preparing cerium oxide nanoparticles, where a first aqueous solution comprising cerium nitrate is provided in a first compartment of a mixing vessel and a second aqueous solution comprising hexamethylenetetramine is provided in a second compartment of the mixing vessel, the first and second compartments being separated by a retractable partition. The retractable partition is retracted to allow the first and second aqueous solutions to mix so as to form a mixture, and the mixture is maintained at a temperature no higher than about 320° K to form nanoparticles. The nanoparticles that are formed are then separated from the mixture. Still another aspect of the present invention is a method for preparing cerium oxide nanoparticles, where a first aqueous solution comprising one of cerium nitrate and hexamethylenetetramine is provided in a mixing vessel having at least one inlet. A second aqueous solution comprising the other one of cerium nitrate and hexamethylenetetramine is pumped into the mixing vessel through the at least one inlet so as to cause mixing of the first and second aqueous solutions to form a mixture. The mixture is maintained at a temperature no higher than about 320° K to form nanoparticles. The nanoparticles that are formed are then separated from the mixture. A further aspect of the present invention is an apparatus for preparing cerium oxide nanoparticles. The apparatus comprises a mixing vessel having a first compartment for holding a first aqueous solution comprising cerium nitrate and a second compartment for holding a second aqueous solution comprising hexamethylenetetramine. The mixing vessel has a retractable partition separating the first and second compartments. When the retractable partition is retracted, rapid mixing of the first aqueous solution with the second aqueous solution takes place to form a mixture, and the mixture is maintained in a mixing vessel at a temperature no higher than about 320° K to form nanoparticles therein. The method and apparatus of the invention have the advantage of being usable to prepare cerium oxide in a quantity which is limited only by the size of the mixing vessel. We have prepared up to about 70 gm of nanoparticles per batch. This is a very large amount when compared to the scale of nanoparticle synthesis of the prior art. By providing for a fast reaction rate and controlling the reaction time, cerium oxide nanoparticles can be prepared within the desired size distribution. The method and mixing vessel also have the advantage of providing cerium oxide nanoparticles which are crystalline. BRIEF DESCRIPTION OF THE FIGURES FIG. 1 is a graphical plot showing the variation of cerium oxide particle size as a function of the time of mixing of the reactants at 300° K FIGS. 2A-2C depict a side view and two top views, respectively, of one embodiment of the mixing vessel according to the present invention. FIG. 3 depicts a side view of another embodiment of the mixing vessel according to the present invention. FIG. 4 are graphical plots showing the variation of the light absorption spectrum of the reaction mixture with the cerium oxide particle size at different stages of the reaction. FIG. 5 is a graphical plot showing lattice parameter versus particle size of cerium oxide for a particle size less than 80 nm. FIG. 6 depicts a high resolution TEM image of cerium oxide nanoparticles showing (111) planes with 0.3 nm spacing. detailed-description description="Detailed Description" end="lead"?

Circuit board router apparatus and method thereof

A circuit board router (10) and method thereof. De-paneling of printed circuit boards (62) off a panel 860) is efficiently increased by a router (40) which is positioned at a location above the panel (60). A fixture positions the panel 860) below the router (40) on a base (16). A controller (64) activates a first drive mechanism (20), a second drive mechanism (26), and a third drive mechanism (32) to guide an X-arm (18), a Y-arm (24) and a Z-arm (10), respectively. The router (40), located on the Z-arm (30), moves downward to engage a router bit (42) to the panel (60) to depanel the printed circuit board (62) from the panel. A fixture chip (72), which has a preprogrammed pattern of the panel (60), is embedded inside the fixture (58). A radio frequency transmitter (80) transmits the pattern to a radio frequency receiver (82) that relays the pattern to the controller (64).

1. A circuit board router device for depaneling a printed circuit board comprising: a frame removably supporting a fixture adapted to hold a circuit board panel; a router assembly coupled to the frame, the router assembly including an X-arm that moves a router spindle along the X axis, a Y-arm that moves the router spindle along the Y axis, and a Z-arm that moves the router spindle along the Z axis, wherein the router spindle is operatively coupled to the Z-arm; a router bit affixed to the router spindle; a controller operationally associated with a first drive mechanism that drives the X-arm, a second drive mechanism that drives the Y-arm, and a third drive mechanism that drives the Z-arm, wherein the controller positions the router bit in accordance with positioning coordinates with respect to the fixture; an input/output device operatively associated with the frame, the input/output device including display capability for displaying diagnostic information relating to the router device, and further including data input capability for accepting programming information for the controller; and an information-carrying device in communication with the controller, the information-carrying device including pattern information identifying a router pattern to be utilized in depaneling circuit boards. 2. The circuit board router device of claim 1, wherein the information-carrying device is an integrated circuit device imbedded inside said fixture. 3. The circuit board router device of claim 1, wherein the fixture further comprises indicia identifying the pattern associated with the information-carrying device. 4. The circuit board router device of claim 1, wherein the pattern information from the information-carrying device is communicated to the controller by an information transmitter. 5. The circuit board router device of claim 4, wherein the information transmitter is a radio frequency transmitter associated with the fixture. 6. The circuit board router device of claim 1, further comprising an information receiver that receives pattern information from the information-carrying device. 7. The circuit board router device of claim 6, wherein the information receiver is a radio frequency receiver coupled to the controller. 8. The circuit board router device of claim 1, wherein the information-carrying device accepts pattern information programmed through the input/output device. 9. The circuit board router device of claim 8, wherein the input/output device is a touch-screen display. 10. The circuit board router device of claim 8, wherein the input/output device includes an associated keyboard adapted to receive router pattern information. 11. The circuit board router device of claim 1, wherein the information-carrying device is a disk drive, and pattern information is downloaded from the disk drive to the controller. 12. The circuit board router device of claim 1, wherein the information-carrying device is a CD-ROM drive, and pattern information is downloaded from the CD-ROM drive to the controller. 13. The circuit board router device of claim 1, further comprising a camera operationally associated therewith, wherein the camera is utilized to identify locations on the PCB panel to be routed, and a set of parameters are input to the controller for each location so identified to establish router pattern information. 14. The circuit board router device of claim 13, wherein the parameters include thickness data of the PCB, X-Y traverse speed data and X-Y cut speed data of the router bit, lower Z height data associated with the cut, upper Z height for router bit travel to the subsequent location, speed of the router spindle, and diameter of the router bit. 15. A method for operating a circuit board router device for depaneling a printed circuit board, the method comprising the steps of: (a) providing a frame removably supporting a fixture adapted to hold a circuit board panel to be routed; (b) providing a router assembly coupled to the frame, the router assembly including an X-arm that moves a router spindle along the X axis, a Y-arm that moves the router spindle along the Y axis, and a Z-arm that moves the router spindle along the Z axis, wherein the router spindle is operatively coupled to the Z-arm; (c) providing a router bit affixed to the router spindle; (d) providing a controller operationally associated with a first drive mechanism that drives the X-arm, a second drive mechanism that drives the Y-arm, and a third drive mechanism that drives the Z-arm, wherein the controller positions the router bit in accordance with positioning coordinates with respect to the fixture; (e) providing an input/output device operatively associated with the frame, the input/output device including display capability for displaying diagnostic information relating to the router device, and further including data input capability for accepting programming information for the controller; and (f) providing an information-carrying device in communication with the controller, the information-carrying device including pattern information identifying a router pattern to be utilized in depaneling circuit boards. 16. The method in accordance with claim 15, further comprising the steps of: (g) providing a camera utilized to identify locations on the PCB panel to be routed; and (h) inputting a set of parameters to the controller for each location so identified to establish router pattern information. 17. The method in accordance with claim 16, wherein the step (h) of inputting a set of parameters further comprises the steps of: (h1) calibrating the camera to the router spindle location; (h2) entering thickness data of the PCB into the controller; (h3) entering X-Y traverse speed data and X-Y cut speed data of the router bit into the controller; (h4) entering lower Z height data for the cut and the upper Z height for the travel to a subsequent location into the controller; and (h5) entering speed of the router spindle and diameter of the router bit into the controller.

<SOH> BACKGROUND OF THE INVENTION <EOH>In the industry, printed circuit boards (PCB's) when manufactured are assembled by affixing a plurality of PCB's to a panel. By affixing a plurality of PCB's to a panel, substantial savings of time, material and money have been obtained as handling a plurality of PCB's simplifies and speeds up the automated processing of the PCB's. As the commercial demands of PCB's in the electronics industry increases, the plurality of PCB's assembled on a single panel require more efficient handling by the processing equipment. An important consideration in the processing of the PCB's is the removal of the individual PCB from the panel for further processing or installation into the finished product, such as a computer or other electronic equipment. Efficiently removing the PCB's from the panel allows more panels to be processed, resulting in economic gain. Removing the PCB's from the panel is referred to as “depaneling” or “liberating” the PCB's from the panel. Methods presently used in the industry to depanel each individual PCB from the interconnected PCB's in the panel have typically included shearing, routing, break-away methods of routed tabs, scoring, perforation, and various punch and die techniques. Routing employs cutting rout slots in the panel around individual PCB's to define the perimeter of the individual PCB. As such, the routing leaves support tabs around the perimeter for holding the individual boards in place. Such tabs are then cut, broken, or routed to remove each board. Scoring utilizes grooving lines along portions of individual board perimeters. Such score lines are then used as weak areas to separate the board by breaking the PCB from the panel along the score lines. In addition, various perforations have been used to define the perimeters of the individual boards. Breaking along the lines of perforation is then used to depanel the individual boards. Other methods of depaneling include punch and die techniques wherein a custom made die is used to punch each individual board out of the panel. These methods of depaneling contain deficiencies, however. The present scorers reduce the rigidity of the panel. Accordingly, the panels are prone to sagging during further processing after one of the PCB's is separated. As a result of the sagging, the subsequent PCB's are not as accurately processed. Perforation and scoring yield very poor quality edges. Accordingly, the edges cannot be held to close tolerances. Additionally, the punch and die method requires expensive tooling as the punch and die is custom made with respect to the panel. Thus, panels having different configurations require different punches and dies. Additionally, the tooling needs to be replaced with each new panel, requiring further downtime of the punch and die. Thus, a need exists for a high volume and high speed depaneling of PCB's from panels containing a plurality of PCB's. A need also exists for a router which enables damage free depaneling of the PCB from the panel. Further, a need exists for a router that depanels the PCB from a location above the PCB. Additionally, a need exists for a router that can be programmed to read a panel configuration and depanel the PCB without changing any tooling. Devices are known in the industry that accept a panel of PC boards and depanel the individual PC boards. U.S. Pat. No. 5,894,648, issued to Hill, discloses a depaneling apparatus that removes the individual PCB from the panel and automatically positions the separated PCB to a registration area. The depaneler then automatically moves the PCB from the registration area to a subsequent processing station. In this depaneler, the PCB is depaneld by a router that cuts the PCB from underneath the panel. This depaneler contains deficiencies, however. Design constraints of an assembly line may not allow the routing mechanism to be underneath the panel. Further, locating the router under the area where the panel is to be processed limits access to the router. Thus, during maintenance or breakdowns, more time is needed to access the router, resulting in less operation time and increased maintenance costs. Further, in some assemblies, it may not be practical to automatically move the separated PCB to a further processing station. Further, the depaneler requires a loading track to position the panel for routing, which may not be practical with regard to the allowable workspace. Another approach is disclosed in U.S. Pat. No. 4,742,615 issued to Lopez, which recites a routing method and apparatus. This device, however, positions the router underneath the panel and routs from below, which may be impractical due to workspace limitations. Further, this device can only rout one predetermined set of panels as opposed to adapting to rout panels with different configurations. Another approach is disclosed in U.S. Pat. No. 5,067,229 issued to Nakamura, which recites a cutting device for electronic components. This cutting device also cuts from underneath the panel. Further, the device requires an identification pattern consisting of eight sections of coated and non-coated sections of the panel in order for the device to sense which type of panel is to be processed, adding to the complexity and cost of the cutting device.

<SOH> SUMMARY OF THE INVENTION <EOH>In one embodiment, the present invention comprises a circuit board router device to depanel a printed circuit board. The router device comprises a base positioned on top of a frame. Attached to the base is a router assembly. The router assembly comprises an X-arm to move the router spindle in the X axis, a Y-arm to move the router spindle in the Y axis, and a Z-arm to move the router spindle in the Z axis. The router assembly further comprises a router bit held by the spindle. The router spindle is attached to the Z-arm to engage a panel from a location above the panel. The panel holds a plurality of PCB's as a single unit. Tabs connect the PCB's to the panel in which the panel is positioned within a fixture. The fixture is placed underneath the router spindle to engage a router bit against the tabs to depanel the PCB's from the panel. The routed tabs and panel are discarded through a base aperture located on the base. The illustrated embodiment further comprises a controller to control a first drive mechanism, a second drive mechanism, and a third drive mechanism which drive the X-arm, the Y-arm and the Z-arm, respectively, to proper coordinates above the fixture. A display screen is connected to the frame, which is capable of programming the controller. The display screen is also capable of displaying diagnostic information of the router device. In one embodiment, the router device is pre-programmable to rout a particular pattern of the panel. In this embodiment, a fixture chip is embedded within the fixture in which the fixture has an identifying mark to indicate which pattern of panel is being positioned in the fixture. The fixture chip mates with a radio frequency transmitter which relays the programmed pattern of the fixture chip to a radio frequency receiver. The radio frequency receiver in turns relays the programmed pattern to the controller.

Interface materials and methods of production and use thereof

Layered interlace materials described herein comprise at least one crosslinkable thermal interface component and at least one compliant fibrous interface component coupled to the thermal interface component. A method of forming layered interface materials comprises: a) providing a crosslinkable thermal interface component; b) providing a compliant fibrous interface component; and c) physically coupling the thermal interface component and the compliant fibrous interface component. At least one additional layer, including a substrate layer, can be coupled to the layered interface material.

1. A layered interface material, comprising: at least one crosslinkable thermal interface component; and at least one compliant fibrous interface component coupled to the thermal interface component. 2. The layered interface material of claim 1, wherein the at least one thermal interface component comprises at least one rubber compound, at least one amine resin and at least one thermally conductive filler. 3. The layered interface material of claim 2, wherein the at least one thermal interface component further comprises at least one phase change material. 4. The layered interface material of claim 2, wherein the at least one rubber compound comprises at least one terminal hydroxy group. 5. The layered interface material of claim 2, wherein the at least one rubber compound comprises at least one saturated compound. 6. The layered interface material of claim 4, wherein the at least one rubber compound further comprises at least one saturated compound. 7. The layered interface material of claim 4, wherein the at least one rubber compound comprises hydrogenated polyalkyldiene mono-ol, hydrogenated polyalkyldiene diol, or a combination or mixture thereof. 8. The layered interface material of claim 7, wherein the hydrogenated polyalkyldiene mono-ol comprises hydrogenated polybutadiene mono-ol. 9. The layered interface material of claim 7, wherein the hydrogenated polyalkyldiene diol comprises hydrogenated polybutadiene diol. 10. The layered interface material of claim 2, wherein the at least one amine resin comprises a melamine resin. 11. The layered interface material of claim 10, wherein the melamine resin comprises an alkylated melamine resin. 12. The layered interface material of claim 11, wherein the alkylated melamine resin comprises butylated melamine resin. 13. The layered interface material of claim 2, wherein the at least one thermally conductive filler comprises a metal powder, a boron nitride compound or a combination thereof. 14. The layered interface material of claim 13, wherein the metal powder comprises aluminum powder, silver powder, copper powder or a combination thereof. 15. The layered interface material of claim 3, wherein the at least one phase change material comprises a wax. 16. The layered interface material of claim 15, wherein the wax comprises a paraffin wax. 17. The layered interface material of claim 2, further comprising at least one catalytic material. 18. The layered interface material of claim 3, further comprising at least one catalytic material. 19. The layered interface material of claim 1, wherein the compliant fibrous interface component comprises a plurality of flocked thermally conductive fibers. 20. The layered interface material of claim 19, wherein the plurality of flocked thermally conductive fibers are embedded in an adhesive material. 21. The layered material of claim 20, wherein the plurality of flocked thermally conductive fibers are embedded in a substantially vertical orientation with portions of the plurality of fibers extending out of the adhesive material. 22. The layered material of claim 21, wherein the plurality of flocked thermally conductive fibers comprise an encapsulant material disposed between the portions of the plurality of fibers, wherein the plurality of fibers extends out of the encapsulant material. 23. The layered material of claim 19, wherein the plurality of flocked thermally conductive fibers comprises carbon, graphite, metal, ceramic, conductive polymer, diamond or a combination thereof. 24. The layered material of claim 23, wherein the plurality of flocked thermally conductive fibers comprises carbon. 25. The layered material of claim 19, wherein the plurality of flocked thermally conductive fibers comprises a length of at least about 0.0005 inches. 26. The layered material of claim 25, wherein the plurality of flocked thermally conductive fibers comprises a length of at least about 0.001 inches. 27. The layered material of claim 26, wherein the plurality of flocked thermally conductive fibers comprises a length of at least about 0.01 inches. 28. The layered material of claim 27, wherein the plurality of flocked thermally conductive fibers comprises a length of at least about 0.1 inches. 29. The layered material of claim 28, wherein the plurality of flocked thermally conductive fibers comprises a length of at least about 1 inch. 30. The layered material of claim 19, wherein the plurality of flocked thermally conductive fibers comprises a fiber diameter of at least about 3 microns. 31. The layered material of claim 30, wherein the plurality of flocked thermally conductive fibers comprises a fiber diameter of at least about 30 microns. 32. The layered material of claim 32, wherein the plurality of flocked thermally conductive fibers comprises a fiber diameter of at least about 300 microns. 33. The layered material of claim 19, wherein the encapsulant comprises a gel material. 34. The layered material of claim 33, wherein the gel material comprises a silicon gel, a spray gasket material or a combination thereof. 35. The layered material of claim 19, wherein the plurality of thermally conductive fibers comprises a thermal conductivity of at least about 25 W/mK. 36. A layered component comprising the layered interface material of claim 1. 37. An electronic component comprising the layered interface material of claim 1. 38. A layered component comprising the layered interface material of claim 2. 39. An electronic component comprising the layered interface material of claim 2. 40. A layered component comprising the layered interface material of claim 3. 41. An electronic component comprising the layered interface material of claim 3. 42. A tape comprising the layered interface material of claim 3. 43. A method of producing a layered interface material, comprising: providing a crosslinkable thermal interface component; providing a compliant fibrous interface component; and physically coupling the thermal interface component and the compliant fibrous interface component. 44. A method of forming the crosslinkable thermal interface component of claim 43, comprising: providing at least one saturated rubber compound; providing at least one amine resin; crosslinking the at least one saturated rubber compound and the at least one amine resin to form a crosslinked rubber-resin mixture; adding at least one thermally conductive filler to the crosslinked rubber-resin mixture; and adding a wetting agent to the crosslinked rubber-resin mixture. 45. The method of claim 44, further comprising adding at least one phase change material to the crosslinked rubber-resin mixture. 46. A liquid thermal interface composition formed by the method of claim 45. 47. A solid thermal interface composition formed by the method of claim 45. 48. A tape comprising the thermal interface component of claim 45. 49. A method of forming the compliant fibrous interface component of claim 43, comprising: providing thermally conductive fibers having a length; providing a substrate; applying adhesive to the substrate; flocking the fibers to the substrate; embedding the fibers into the adhesive with a portion of the fibers extending out of the adhesive; curing the adhesive; disposing a curable encapsulant between the fibers extending out of the adhesive and beneath the free ends of the fibers; compressing the fibers with encapsulant between the fibers into the adhesive; and curing the encapsulant while under compression.

<SOH> BACKGROUND <EOH>Electronic components are used in ever increasing numbers of consumer and commercial electronic products. Examples of some of these consumer and commercial products are televisions, personal computers, internet servers, cell phones, pagers, palm-type organizers, portable radios, car stereos, or remote controls. As the demand for these consumer and commercial electronics increases, there is also a demand for those same products to become smaller, more functional, and more portable for consumers and businesses. As a result of the size decrease in these products, the components that comprise the products must also become smaller. Examples of some of those components that need to be reduced in size or scaled down are printed circuit or wiring boards, resistors, wiring, keyboards, touch pads, and chip packaging. Components, therefore, are being broken down and investigated to determine if there are better building materials and methods that will allow them to be scaled down to accommodate the demands for smaller electronic components. In layered components, one goal appears to be decreasing the number of the layers while at the same time increasing the functionality and durability of the remaining layers. This task can be difficult, however, given that several of the layers and components of the layers should generally be present in order to operate the device. Also, as electronic devices become smaller and operate at higher speeds, energy emitted in the form of heat increases dramatically. A popular practice in the industry is to use thermal grease, or grease-like materials, alone or on a carrier in such devices to transfer the excess heat dissipated across physical interfaces. Most common types of thermal interface materials are thermal greases, phase change materials, and elastomer tapes. Thermal greases or phase change materials have lower thermal resistance than elastomer tape because of the ability to be spread in very thin layers and provide intimate contact between adjacent surfaces. Typical thermal impedance values range between 0.6-1.6° C. cm 2 /w. However, a serious drawback of thermal grease is that thermal performance deteriorates significantly after thermal cycling, such as from 65° C. to 150° C., or after power cycling when used in VLSI chips. It has also been found that the performance of these materials deteriorates when large deviations from surface planarity causes gaps to form between the mating surfaces in the electronic devices or when large gaps between mating surfaces are present for other reasons, such as manufacturing tolerances, etc. When the heat transferability of these materials breaks down, the performance of the electronic device in which they are used is adversely affected. Thus, there is a continuing need to: a) design and produce thermal interface materials and layered materials that meet customer specifications while minimizing the size of the device and number of layers; b) produce more efficient and better designed materials and/or components with respect to the compatibility requirements of the material, component or finished product; and c) develop reliable methods of producing desired thermal interface materials and layered materials and components comprising contemplated thermal interface and layered materials.

<SOH> SUMMARY <EOH>Layered interface materials described herein comprise at least one crosslinkable thermal interface component and at least one compliant fibrous interface component coupled to the thermal interface component. A method of forming contemplated layered interface materials comprises: a) providing a crosslinkable thermal interface component; b) providing a compliant fibrous interface component; and c) physically coupling the thermal interface component and the compliant fibrous interface component. At least one additional layer, including a substrate layer, can be coupled to the layered interface material. A constituent of layered interface materials described herein comprises at least one crosslinkable thermal interface component that is produced by combining at least one rubber compound, at least one amine resin and at least one thermally conductive filler. This contemplated thermal interface component takes on the form of a liquid or “soft gel”. The gel state is brought about through a crosslinking reaction between the at least one rubber compound composition and the at least one amine resin composition. More specifically, the amine resin is incorporated into the rubber composition to crosslink the primary hydroxyl groups on the rubber compounds thus forming the soft gel phase. Therefore, it is contemplated that at least some of the rubber compounds will comprise at least one terminal hydroxyl group. Amine or amine-based resins are added or incorporated into the rubber composition or mixture and/or combination of rubber compounds primarily to facilitate a crosslinking reaction between the amine resin and the primary or terminal hydroxyl groups on at least one of the rubber compounds. The crosslinking reaction between the amine resin and the rubber compounds leads to a “soft gel” phase to the mixture, instead of a liquid state. Once the thermal interface component composition that comprises at least one rubber compound, at least one amine resin, and at least one thermally conductive filler has been prepared, the composition must be compared to the needs of the electronic component, vendor, or electronic product to determine whether a phase change material is needed to change some of the physical properties of the composition. Phase change materials are useful in thermal interface component applications because they store and release heat as they oscillate between solid and liquid form. A phase change material gives off heat as it changes to a solid state, and as it returns to a liquid, it absorbs heat. The phase change temperature is the melting temperature at which the heat absorption and rejection takes place. A method for forming the crosslinkable thermal interface components disclosed herein comprises a) providing at least one saturated rubber compound, b) providing at least one amine resin, c) crosslinking the at least one saturated rubber compound and the at least one amine resin to form a crosslinked rubber-resin mixture, d) adding at least one thermally conductive filler to the crosslinked rubber-resin mixture, and e) adding a wetting agent to the crosslinked rubber-resin mixture. This method can also further comprise adding at least one phase change material to the crosslinked rubber-resin mixture. A contemplated thermal interface component can be provided as a dispensable liquid paste to be applied by dispensing methods and then cured as desired. It can also be provided as a highly compliant, cured, elastomer film or sheet for pre-application on interface surfaces or on other materials, such as heat sinks, substrates, and/or a compliant fibrous interface material or component. It can further be provided and produced as a soft gel or liquid that can be applied to surfaces by any suitable dispensing method. Even further, the material can be provided as a tape that can be applied directly to interface surfaces, substrates, compliant fibrous interface materials or component and/or electronic components. Compliant fibrous interface components comprise a plurality of thermally conductive fibers, at least one encapsulant, and at least one optional adhesive material. Suitable thermally conductive fibers comprise diamond fibers, conductive polymer fibers, carbon fibers, graphite fibers and metal fibers, such as copper fibers and aluminum fibers. The thermally conductive fibers are cut to a particular length, usually depending on the needs/specifications of the customer or vendor, e.g. from at least about 0.0005 inches to at least about 1 inch. Thermally conductive fibers may also be cut to at least about 0.001 inches, to at least about 0.01 inches and/or to at least about 0.1 inches. Thermally conductive fibers may have a fiber diameter of at least about 3 microns, of at least about 30 microns and/or at least about 300 microns. Conductive fibers having a fiber diameter of at least about 10 microns are presently preferred. Applications of the contemplated layered interface materials, thermal interface components and compliant fibrous interface components described herein comprise incorporating the materials into a layered material, a layered component, an electronic component, a semiconductor component, a finished electronic product or a finished semiconductor product. Various objects, features, aspects and advantages of the present invention will become more apparent from the following detailed description of preferred embodiments of the invention.

Casing

The invention relates to casing for portable communication devices and light guides for such devices. The casing (2) has a light guide for over-laying a display located in the display region (4) to deliver front lighting to the display and extending across the input region (5), the light guide providing a recess in the input region for operation of a key of the key arrangement.

1. A casing for a portable communication device having an operating face for providing a key arrangement in an input region for user operation of the device and a display region, the casing comprising: a light guide extending across the input region, the light guide providing a recess in the input region for operation of a key of the key arrangement and a light permeable layer arranged on the lightguide defining the outer surface of the casing in the input region. 2. A casing according to claim 1 wherein there are a plurality of keys in the key arrangement. 3. A casing according to claim 1 wherein an opaque layer is located between the light guide and the light permeable layer. 4. A casing according to claim 1 wherein the light permeable layer comprises the light guide. 5. A casing according to claim 1 wherein the light permeable layer provides the front face of the device across the input and display regions. 6. A casing according to claim 1 wherein the light permeable layer is transparent. 7. A casing according to claim 1 wherein the light permeable layer is translucent. 8. A casing according to claim 1 wherein the light guide is a flexible material. 9. A casing according to claim 1 wherein the light permeable layer is arranged on the light guide in segments with lateral discontinuities. 10. A casing according to claim 9 wherein the lateral discontinuities extend across the full lateral extent of the substrate. 11. A casing according to claim 9 wherein the laterally extending discontinuities are shaped to receive keys of the key arrangement. 12. A casing according to claim 1 wherein the light permeable layer and the light guide have the same optical qualities. 13. A casing according to claim 1 wherein the light permeable layer and the light guide are the same colour. 14. A casing according to claim 1 wherein the light permeable layer is a material brittle with respect to the material of the light guide. 15. A casing according to claim 1 wherein the light permeable layer is a precious stone. 16. A casing according to claim 1 wherein the light permeable layer is formed from sapphire or diamond or glass. 17. A casing according to claim 1 wherein the light guide provides a lip that protrudes beyond the extent of the light permeable layer. 18. A casing according to claim 17 wherein the front face is retained in place by gripping the lip between elements of a casing of the portable device. 19. A casing according to claim 1 wherein light sources are provided along opposing sides of the light guide in the input region. 20. A casing according to claim 1 wherein the face is longer longitudinally than it is laterally. 21. A casing according to claim 1 wherein a light source is provided proximate the display region. 22. A casing according to claim 21 wherein the light source proximate the display region is a light pipe. 23. A casing according to claim 22 wherein the light pipe is fed with light from light sources located along the edge of the light guide. 24. A portable communication device comprising a casing in accordance with claim 1. 25. A portable communication device according to claim 24 wherein the communication device is a radio telephone. 26. A casing for a portable communication device having an operational face for providing a key arrangement in an input region for user operation of the device and a display region, the device comprising: a light guide for overlaying a display located in the display region to deliver front lighting for the display; and a light guide extending across the input region to deliver lighting to the key arrangement, the light guide providing a recess in the input region for operation of a key of the key arrangement. 27. (canceled) 28. (canceled)

Device and method for analyzing ion channels in membranes

The present invention relates to devices and methods for analyzing ion channels in membranes. The invention is characterized by a biochip comprising a substrate in which openings are provided in the form of an M×N matrix for receiving therein a cell membrane including at least one ion channel (I) or an artificial lipid membrane (Me), wherein M≧1 and N≧1.

1. A biochip (1; 2; 3) for analyzing ion channels, comprising a substrate (10; 20; 30) in which openings (19; 29; 39) are provided in the form of an M×N matrix for receiving therein a cell membrane (Me) including at least one ion channel (1) or an artificial lipid membrane including at least one ion channel, wherein M≧1 and N≧1. 2. A biochip (1; 2; 3) according to claim 1, wherein the surface of the biochip has in the area of each opening a means for improving the contact between the cell membrane and the biochip, said means being provided on the receiving side. 3. A biochip according to claim 2, wherein the means for improving the contact is implemented in the form of a patterning of the surface. 4. A biochip according to claim 3, wherein said patterning is provided in the form of one or a plurality of rings which is or which are arranged around each opening, or in the form of one or a plurality of squares or rectangles which is or which are arranged around each opening. 5. A biochip according to claim 1, wherein each opening is substantially circular. 6. A biochip according to claim 1, wherein the substrate comprises a base portion (10; 20; 30) which has a first thickness (d1) and window portions (11; 21; 31) which are formed in said base portion and which have a second thickness (d2), each opening being provided in a respective window portion. 7. A biochip according to claim 1, wherein the substrate comprises a semiconductor material, such as GaAs, Si or AlGaAs, or an insulator, such as a glass or quartz, or polymers, such as polydimethyl-siloxane (PDMS). 8. A biochip according to claim 6, wherein the substrate comprising the base portion and the window portions formed in said base portion consists of one material. 9. A biochip according to claim 1, wherein electrodes are provided on one or on both sides of the substrate. 10. A biochip according to claim 9, wherein the electrodes are implemented such that they are adapted to have applied thereto a temporally constant electromagnetic field and/or a high-frequency alternating electromagnetic field. 11. A biochip according to claim 1, wherein planar waveguides are integrated in the biochip for applying high-frequency alternating fields. 12. A biochip according to claim 1, wherein interdigital electrodes are provided on the biochip for generating surface-acoustic waves. 13. A biochip according to claim 1, wherein active and/or passive components are integrated on the substrate. 14. A biochip according to claim 13, wherein said active and/or passive components comprise a field effect amplifier means for preamplifying measuring signals. 15. A biochip according to claim 1, wherein an optical near-field means is provided for observing the ion channel or the ion channels. 16. A biochip according to claim 15, wherein the optical near-field means comprise scanning probe means. 17. A biochip according to claim 1, wherein microfluid channels are provided for on-chip perfusion. 18. A biochip according to claim 1, wherein the biochip has applied thereto a layer of flexible, non-conductive polymer on the receiving side, said layer comprising at least two openings through which at least the openings in the substrate are exposed. 19. A biochip according to claim 1, wherein the surface on the receiving side is hydrophobic. 20. A biochip according to claim 1, wherein channels extending parallel to the substrate surface are provided in or above said substrate surface. 21. A method of producing a biochip for analyzing ion channels comprising a substrate in which openings are formed, in the form of an M×N matrix, for receiving therein a cell membrane including at least one ion channel or an artificial lipid membrane including at least one ion channel, wherein M≧1 and N≧1, said method comprising the steps of: providing a substrate, forming at least one window portion in said substrate, and forming an opening in each window portion. 22. A method according to claim 21, wherein each window portion is formed by means of wet- or dry-etching methods. 23. A method according to claim 21, wherein each window portion is formed by means of laser thinning or by means of hot shaping. 24. A method according to claim 21, wherein each opening is formed by means of laser thinning or ion track etching. 25. A method according to claim 21, wherein each opening is formed by means of dry-etching methods or by means of a focused ion beam. 26. A method according to claim 21, comprising the following additional step: local or non-local heat treatment of the substrate for improving the contact with a cell membrane. 27. A method of analyzing ion channels in membranes, said method comprising the steps of: providing a biochip according to claim 1, applying one or a plurality of singulated cells in an aqueous suspension to the biochip, positioning not more than one cell on one opening. 28. A method according to claim 27, wherein the cells are applied with the aid of at least one pipette or cannula. 29. A method according to claim 28, wherein the ion channel currents are measured with the aid of electrodes integrated in each pipette or cannula. 30. A method of analyzing ion channels in membranes, said method comprising the steps of: providing a biochip according to claim 20, flushing one or a plurality of singulated cells in an aqueous suspension into the biochip via the channels extending parallel to the substrate surface, positioning not more than one cell on one opening. 31. A method according to claim 27, wherein, for positioning each cell, a vacuum is applied at the side of an opening located opposite the receiving side. 32. A method according to claim 27, wherein, for positioning each cell, an electric direct voltage and/or alternating voltage is/are applied perpendicularly to the substrate surface. 33. A method according to claim 27, wherein surface-acoustic waves are used for positioning each cell. 34. A method according to claim 27, wherein, for positioning each cell, mechanical, chemical, electric, magnetic or electromechanical gradients or fields are applied through the opening. 35. A method according to claim 27, wherein, for positioning each cell, additional cells or particles are added on the receiving side. 36. A method according to claim 27, said method comprising the following additional step: detecting each cell on an opening by measuring at least one electric parameter of said opening. 37. A method according to claim 27, said method comprising the following additional step: electrophysiological characterization of each cell. 38. A method according to claim 27, wherein active substances are applied or de-applied by flushing in or sucking off a solution. 39. A device for analyzing ion channels in membranes, comprising: a first biochip according to claim 1, and a second biochip provided with a means for positioning cells relative to the openings of said first biochip, wherein the respective surfaces on the receiving side are located in opposed relationship with and at a fixed or variable distance from one another. 40. device according to claim 39, wherein the cell positioning means comprises a means for generating surface waves. 41. A device according to claim 39, wherein the biochips are supported in direct contact with one another and wherein the surface of the second biochip located on the receiving side has integrated therein fluid channels which extend parallel to the surface and which are open towards said surface. 42. A measuring probe (4), comprising a biochip (1; 2; 3) according to claim 1, a holding device (45) having a central cavity or a plurality of cavities which communicate with the aperture or the apertures of the biochip (1; 2; 3) and provided on the side of the substrate that is located opposite to the side where the membrane (M) is applicable, wherein the opening of the holding device facing away from the substrate is implemented such that an electrode means (43) can be inserted therein. 43. A measuring probe according to claim 42, wherein the holding device consists of glass or polycarbonate. 44. A measuring probe according to claim 42, wherein the holding device is adapted to be screw-fastened to the biochip. 45. A measuring probe according to claim 42, wherein sealing means are provided between the holding device and the biochip. 46. A measuring probe according to claim 42, wherein the holding device is adhesively attached to the substrate. 47. A measuring probe according to claim 42, wherein the electrode means is adapted to be screwed into the glass tube. 48. A measuring probe according to claim 47, wherein sealing means are provided between the holding device and the electrode means. 49. A measuring probe according to claim 42, wherein a vacuum-generating means (46) is provided in said glass tube.

<SOH> FIELD OF THE INVENTION <EOH>The present invention relates to devices and methods for analyzing ion channels in membranes, in particular devices and methods for executing the so-called patch clamp technique with the aid of a biochip, especially for use in high throughput processes.

Mammalian tribbles signaling pathways and methods and reagents related thereto

The invention provides methods and reagents for modulating mitogen activated protein kinase pathways using mammalian tribbles homologs (htrb).

1. An isolated htrb-1 encoding nucleic acid comprising a nucleotide sequence which is at least about 90% identical to the nucleotide sequence set forth in SEQ ID No. 1 or the complement thereof. 2. The nucleic acid of claim 1, wherein the nucleic acid comprises a nucleotide sequence at least about 95% identical to the nucleotide sequence set forth in SEQ ID No. 1 or the complement thereof. 3. The nucleic acid of claim 1, wherein the nucleic acid comprises a nucleotide sequence at least about 99% identical to the nucleotide sequence set forth in SEQ ID No. 1 or the complement thereof. 4. The nucleic acid of claim 1, wherein the nucleic acid comprises a nucleotide sequence at least about 95% identical to the nucleotide sequence set forth in SEQ ID No. 1 or the complement thereof, and encodes an AP-1 inhibitory activity. 5. The nucleic acid of claim 1, which hybridize to an htrb-1 ORF encoding nucleic acid corresponding to nucleotides 282 to 1400 of SEQ ID No. 1. 6. The isolated nucleic acid of claim 1, which further encodes an htrb polypeptide that is at least about 75% identical to the htrb-1 polypeptide sequence set forth in SEQ ID No.2. 7. The isolated nucleic acid of claim 6, which further encodes an AP-1 inhibitory activity. 8. The isolated nucleic acid of claim 1, wherein the nucleic acid encodes an htrb bioactivity selected from the group consisting of: an inhibition of IL-8 basal expression, an inhibition of AP-1 transcriptional activation, an inhibition of MEKK-1 kinase signaling, an inhibition of MKK-7 kinase signaling, a cellular hypertrophy-promoting activity, an activation of ERK kinase signaling, and an inhibition of JNK kinase signaling. 9. An isolated nucleic acid comprising a nucleotide sequence that hybridizes under stringent conditions to a htrb-1 nucleotide sequence selected from the group consisting of: nucleotides 283 to 730 of SEQ ID No. 1; nucleotides 1 to 729 of SEQ ID No. 1; and nucleotides 1500 to 1916 of SEQ ID No. 1. 10. The nucleic acid of claim 9, which further encodes an htrb polypeptide that is at least about 50% identical to the htrb-1 polypeptide sequence set forth in SEQ ID No. 2. 11. The nucleic acid of claim 10, which further encodes an htrb-1 bioactivity. 12. The nucleic acid of claim 9, which further includes at least 25 contiguous nucleotides that are identical to said htrb nucleotide sequence. 13. An isolated nucleic acid that encodes the htrb-1 polypeptide sequence set forth in SEQ ID No. 2. 14. An isolated polypeptide comprising a polypeptide sequence of at least 10 contiguous amino acids from the htrb-1 sequence spanning amino acid residues 1 to 150 of SEQ ID No. 2. 15. The polypeptide of claim 14 comprising at least 20 contiguous amino acids from the htrb-1 sequence spanning amino acid residues 1 to 150 of SEQ ID No. 2. 16. An isolated polypeptide comprising an amino acid sequence that is at least 70% identical to the htrb-1 polypeptide sequence set forth in SEQ ID No. 2. 17. The polypeptide of claim 16, wherein the polypeptide sequence is at least 80% identical to the htrb-1 polypeptide sequence set forth in SEQ ID No. 2. 18. The polypeptide of claim 16, wherein the polypeptide sequence is at least 90% identical to the htrb-1 polypeptide sequence set forth in SEQ ID No. 2. 19. The polypeptide of claim 13, having at least one htrb-1 bioactivity. 20. The polypeptide of claim 19, wherein the htrb-1 bioactivity is selected from the group consisting of: an inhibition of IL-8 basal expression, an inhibition of AP-1 transcriptional activation, an inhibition of MEKK-1 kinase signaling, an inhibition of MKK-7 kinase signaling, a cellular hypertrophy-promoting activity, an activation of ERK kinase signaling, and an inhibition of JNK kinase signaling. 21. An isolated htrb-1 polypeptide having the sequence set forth in SEQ ID No. 2. 22. A method of modulating an AP-1 mediated inflammatory signal in a cell comprising providing the cell with a htrb agonist or antagonist. 23. The method of claim 22 wherein the htrb agonist or antagonist is a htrb polypeptide, a htrb peptidomimetic or a htrb nucleic acid. 24. The method of claim 23 wherein the htrb agonist or antagonist is selected from the group consisting of: htrb-1, htrb-1ΔN, htrb-1ΔC, htrb-1ΔNΔC, htrb-3, an htrb-1 5′ UTR and N-terminal variable region antisense construct, an htrb-3 5′ UTR and N-terminal variable region antisense construct, an htrb-1 3′UTR sense construct. 25. The method claim 22, wherein the AP-1 mediated inflammatory signal is selected from the group consisting of: a TNF induced inflammatory signal, and an interleukin induced inflammatory signal. 26. A method of inhibiting an AP-1 mediated inflammatory signal in a cell comprising contacting the cell with an htrb polypeptide of of claim 14. 27. The method of claim 26, wherein the htrb polypeptide is selected from the group consisting of: htrb-1, htrb-1ΔN, htrb-1ΔC, htrb-1ΔNΔC, htrb-3, htrb-3ΔN, htrb-3ΔC, and htrb-3ΔNΔC. 28. A method of activating an ERK-mediated signal in a cell comprising providing the cell with an htrb agonist activity. 29. (canceled) 30. The method of claim 28, wherein the hrtb agonist activity is provided by a htrb polypeptide selected from the group consisting of: htrb-1, htrb-1ΔN, htrb-1ΔC, htrb-1ΔNΔC, htrb-3, htrb-3ΔN, htrb-3ΔC, and htrb-3ΔNΔC. 31. The method of claim 28, wherein the ERK-mediated signal is selected from the group consisting of: an AP-1-mediated gene activation signal, an estrogen receptor-mediated gene activation signal, an FGF induced signal, and a PMA induced signal. 32. A method of identifying an interleukin regulatory gene comprising: (a) transfecting a mammalian reporter cell comprising an interleukin gene reporter with a low-complexity pool of a mammalian cDNA vector library; (b) screening the transfected reporter cell for positive clones by identifying transfected cells with either an increase or decrease in the interleukin gene reporter activity relative to the mammalian reporter cell transfected with the vector alone; and (c) identifying the interleukin regulatory gene from the positive clones by retransfecting the low complexity pool from said positive clones and sequencing the cDNA inserts from the positive clones obtained upon retransfection, thereby identifying an interleukin regulatory gene. 33. The method of claim 32, wherein the interleukin gene reporter is selected from the group consisting of: an IL-1A gene reporter, an IL-1B gene reporter, an IL-1RN gene reporter, and IL-8 gene reporter. 34. The method of claim 32, wherein the mammalian cell is selected from the group consisting of: a HeLa cell, an NIH 3T3 cell, a Raw cell, a peripheral blood lymphocyte. 35. The method of claim 32, wherein the mammalian cDNA library is selected from the group consisting of: a PBMC library, a HeLa cell library, a PMA-induced mammalian cell library, and a cytokine-induced mammalian cell library. 36. A method of identifying the gene targets of an interleukin regulatory gene in an inflammatory signaling network comprising: (a) expressing an interleukin regulatory gene clone, comprising an interleukin regulatory gene cDNA and an expression vector, in a population of mammalian cells; (b) isolating a population of nucleic acids representing expressed genes from said cells; (c) determining the gene expression profile of the interleukin regulatory gene expressing cells by microarray analysis of the population of nucleic acids representing expressed genes from said cells; and (d) comparing the gene expression pattern of mRNA expression from the cells transfected with the interleukin regulatory gene clone with that obtained by transfecting the vector alone in order to identify genes, other than the said interleukin regulatory gene, which are either up-regulated or down-regulated in the interleukin regulatory gene expressing cells, thereby identifying the gene targets of an interleukin regulatory gene in an inflammatory signaling network. 37. (canceled) 38. The method of claim 36, wherein the mammalian cell is selected from the group consisting of: a HeLa cell, an NIH 3T3 cell, a Raw cell, a peripheral blood lymphocyte. 39. The method of claim 36, wherein the population of nucleic acids representing expressed genes is an mRNA population. 40. The method of claim 36, wherein the population of nucleic acids representing expressed genes is a cDNA population. 41. The method of claim 36, wherein the microarray analysis provides a gene transcription profile or gene expression fingerprint.

<SOH> 1. BACKGROUND OF THE INVENTION <EOH>The function of immune and inflammatory genes play a central role in the pathology of many diseases including rheumatoid arthritis, inflammatory bowel disorder, psoriasis, and Alzheimer's disease. There is evidence to suggest that these immune and inflammatory genes function as a complex network of interdependent signaling components. These signaling components mediate signaling events which take place both extracellularly (e.g. through the action of various cytokines such as the interleukins) and intracellulary (e.g. through the action of signal transducing kinases and transcriptional regulators such as AP-1 and NF-B). A variety of means exist for regulating inflammatory responses involved in disease processes. For example, aspirin (salicylic acid) inhibit activation of NF-kB by blocking I-kB kinase, a key enzyme in NF-kB activation. Sulfasalazine and gold compounds also inhibit NF-kB activation. Glucocorticoids suppress expression of inflammatory genes by binding glucocorticoid receptors involved in NF-kB activation. Such drugs are commonly used to regulate inflammatory diseases such as rheumatoid arthritis. Nevertheless there is a need to develop drugs with particular anti-inflammatory specificities that are particularly adapted to controlling certain aberrant inflammatory processes while allowing nonpathological inflammatory processes to continue without interference. Indeed, a variety of anti-inflammatory medicaments would benefit the development of optimized drug treatments for specific patients with particular needs (see Davies & Skjodt (2000) Clin Pharmoacokinet 38: 377-92). Furthermore, continuing advances in understanding the molecular mechanisms of inflammation will benefit the development of more effective, more specific and less toxic drugs to control inflammatory diseases. An understanding of the relationships between the genes comprising this network would provide a broad array of drug targets for the control of autoimmune and inflammatory disease processes. Molecular agonists and antagonists could be designed to act alone or in concert at one or more points in this gene network in order to effect control of the disease process. A large body of work has recently been focused on signalling networks triggered by proinflammatory cytokines, bacterial cell walls and shear stress. In general, two major signalling cascades are activated by these stimuli. The major intracellular signaling cascades involved in immune and inflammatory gene network regulation are the mitogen activated protein kinase (MAPK, or stress kinase) cascade and the IkB kinase cascade as well as the JAK/STAT signal transduction pathway (see e.g. Rivest et al. (2000) Proc Soc Exp Biol Med 223: 22-38). Activation of NF-kB is thought to be mediated primarily via I-kB kinase (IKK), whereas that of AP-1/ATF can be mediated by stress-activated protein kinases (SAPKs; also termed Jun kinases or JNKs). IKKalpha and IKKbeta are two catalytic subunits of a core IKK complex that also contains the regulatory subunit NEMO (NF-kappaB essential modulator)/IKKgamma. The latter protein is essential for activation of the IKKs, but its mechanism of action is not known, although the molecular cloning of CIKS (connection to IKK and SAPK/JNK), a previously unknown protein that directly interacts with NEMO/IKKgamma in cells, may prove informative (see Leonardi et al. (2000) PNAS, USA 97: 10494-9). When ectopically expressed, CIKS stimulates IKK and SAPK/JNK kinases and it transactivates an NF-kappaB-dependent reporter. Activation of NF-kappaB is prevented in the presence of kinase-deficient, interfering mutants of the IKKs. CIKS may help to connect upstream signaling events to IKK and SAPK/JNK modules and CIKS could coordinate the activation of two stress-induced signaling pathways, functions reminiscent of those noted for tumor necrosis factor receptor-associated factor adaptor proteins. Individual stress kinase mediated pathways behave differently in different cell types. Specificity may be achieved in part by cell type specific expression of certain pathway components such as CIKS. It is important that all components contributing to the regulation and specificity of these mitogen activated protein kinase signalling pathways be identified as each represents a target for regulation of this important class of inflammatory signalling events.

<SOH> 2. SUMMARY OF THE INVENTION <EOH>The invention is based in part upon the cloning and identification of certain mammalian htrbs genes and encoded htrbs proteins which function as inhibitors of particular stress kinase pathways. The htrbs genes are mammalian homologs of the Drosophila tribbles gene, which coordinates mitosis with morphogenesis and cell fate determination in fruit fly development (see Mata et al. (2000) Cell 101: 511-22; and Grosshans & Wieschaus (2000) Cell 101: 523-31). The invention provides a human homolog of the Drosophila tribbles gene which has been termed htrb-1, for human tribbles homologue-1 (also known as homo SKIP1 (Gen Bank Accession NO. AF250310). The htrb-1 inhibits basal but not induced activity of the cytokine responsive interleukin-1 (IL-8) gene reporter, which is responsive to both NF-kB and AP-1 induction through binding sites for these transcriptional activators present in the IL-8 promoter. The htrb-1 gene of the invention specifically represses AP-1 but not NF-kB or JAK/STAT mediated transcriptional induction. Therefore the htrb-1 gene of the invention provides a convenient and a specific tool for modulating stress kinase-induced pathways. In preferred embodiments, the invention provides an isolated htrb-1 encoding nucleic acid comprising a nucleotide sequence which is at least about 90% identical to the nucleotide sequence set forth in SEQ ID No. 1 or the complement thereof and more preferably at least about 95% or 99% identical. In certain embodiments, the nucleic acid of the invention further an AP-1 activation inhibitory activity. The invention further provides isolated nucleic acid which encodes an htrb polypeptide, such as a polypeptide that is at least about 75% identical to the htrb-1 polypeptide sequence set forth in SEQ ID No. 2, and which, preferably, further encodes an AP-1 inhibitory activity. In certain preferred embodiments, the isolated nucleic acid of the invention encodes an htrb bioactivity such as an IL-8 basal expression inhibitory activity, and AP-1 transcriptional activation inhibitory activity, an MEKK-1 kinase signaling inhibitory activity, an MKK-7 kinase signaling inhibitory activity, an ERK kinase signaling inhibitory activity, a JNK kinase signaling inhibitory activity, or a cellular hypertrophy-promoting activity. Preferred nucleic acids of the invention include isolated nucleic acid with a nucleotide sequence that hybridizes under stringent conditions to certain particular htrb-1 nucleotide sequences such as: nucleotides 1 to 448 of SEQ ID No. 1; nucleotides 1 to 729 of SEQ ID No. 1; and nucleotides 1500 to 1916 of SEQ ID No. 1. The invention further provides isolated htrb polypeptides which include a polypeptide sequence of at least 10, and, more preferably, 20 or 30 contiguous amino acids from the htrb-1 sequence spanning amino acid residues 1 to 150 of SEQ ID No. 2. Preferably the htrb polypeptides of the invention are at least about 70%, and, more preferably 80, 90 95 or 99% identical to the htrb-1 sequence set forth in SEQ ID No. 2. In preferred embodiments, the htrb polypeptide encodes an htrb-1 bioactivity such as an ability to: inhibit IL-8 basal expression, inhibit AP-1 transcriptional activation, inhibit MEKK-1 kinase signaling, inhibit MKK-7 kinase signaling, inhibit ERK kinase signaling, inhibit JNK kinase signaling, or promote cellular hypertrophy. In particularly preferred embodiments, the invention provides methods of modulating an AP-1 mediated inflammatory signal in a cell by providing the cell with a htrb agonist or antagonist. The htrb agonist or antagonist can be an htrb polypeptide, an htrb peptidomimetic or an htrb nucleic acid. Preferred htrb nucleic acid agonist or antagonists of the invention include htrb-1, htrb-1 N htrb-1 C, htrb-1 N C, htrb-3, an htrb-1 5′ UTR and N-terminal variable region antisense construct, an htrb-3 5′ UTR and N-terminal variable region antisense construct, and an htrb-1 3′UTR sense construct. Preferred htrb polypeptide agonist or antagonists of the invention include htrb-1, htrb-1 N htrb-1 C, htrb-1 N C, htrb-3, htrb-3 N htrb-3 C, and htrb-3 N C. The method of the invention may be used to inhibit an AP-1 mediated inflammatory signal such as a TNF induced inflammatory signal, or an interleukin induced inflammatory signal. The method of the invention further provides a method of activating an ERK-mediated signal in a cell by providing the cell with an htrb agonist activity. The ERK-mediated signal may be, for example, an AP-1-mediated gene activation signal, an estrogen receptor-mediated gene activation signal, an FGF induced signal, or a PMA induced signal. A particularly preferred embodiment of the invention provides a method of identifying an interleukin regulatory gene by a particular cloning process. The process of the invention includes: (1) transfecting a mammalian reporter cell comprising an interleukin gene or inflammatory gene reporter with a low-complexity pool of a mammalian cDNA vector library; (2) screening the transfected reporter cell for positive clones by identifying transfected cells with either an increase or decrease in the interleukin gene reporter activity relative to the mammalian reporter cell transfected with the vector alone; and (3) identifying the interleukin regulatory gene from the positive clones by retransfecting the low complexity pool from said positive clones and sequencing the cDNA inserts from the positive clones obtained upon retransfection, so as to identify an interleukin regulatory gene. The interleukin or inflammatory gene reporter may be an IL-1A gene reporter, an IL-1B gene reporter, an IL-1RN gene reporter, or an IL-8 gene reporter. Preferred cells for use in this aspect of the invention include mammalian cells such as HeLa cells, NIH 3T3 cells, Raw cells, or peripheral blood lymphocytes. Preferred libraries for use in this aspect of the invention includes mammalian cDNA libraries such as PBMC libraries, HeLa cell libraries, PMA-induced mammalian cell libraries, or a mammalian cell library constructed from another cytokine-induced mammalian cell such as an IL-5, TGF-beta, interferon-alpha, or IL-12 induced mammalian cell. In preferred embodiments of this aspect of the invention, an interative doing process is used to derive still other inflammatory regulatory network genes. This process of the invention involves: first expressing an interleukin regulatory gene clone, comprising an interleukin regulatory gene cDNA and an expression vector, in a population of mammalian cells; next isolating a population of nucleic acids representing expressed genes from said cells; determining the gene expression profile of the interleukin regulatory gene expressing cells by microarray analysis of the population of nucleic acids representing expressed genes from said cells; and then comparing the gene expression pattern of mRNA expression from the cells transfected with the interleukin regulatory gene clone with that obtained by transfecting the vector alone in order to identify genes, other than the said interleukin regulatory gene, which are either up-regulated or down-regulated in the interleukin regulatory gene expressing cells, so as to identify the other gene targets of the interleukin regulatory gene making up the inflammatory signaling network. In preferred embodiments the method assesses altered expression of responsive genes by microarray analysis such as gene transcription profiling or gene expression fingerprinting.

Micromechanical flow sensor with tensile coating

A sensor integrated on a semiconductor device (1), in particular a flow sensor, comprises a measuring element (2) on a membrane (5). In order to prevent a buckling of the membrane (5) a tensile coating (9) is applied. The coating covers the membrane, but it preferably leaves all the active electronic components integrated on the semiconductor chip (1) uncovered, such that their electrical properties are not affected.

1-15. (canceled) 16. A sensor with a semiconductor device, on which a measuring element and a circuit with active electronic components are integrated, wherein the measuring element is arranged on a membrane above an opening or recess of the semiconductor device, wherein a tensile coating is arranged on the semiconductor device for tautening the membrane, wherein the tensile coating leaves at least a part of the active components of the circuit uncovered. 17. The sensor of claim 16 wherein the tensile coating leaves at least the active electronic components of the circuit uncovered. 18. The sensor of claim 16 wherein the tensile coating extends of the membrane. 19. The sensor of claim 16 wherein the active electronic components of the circuit comprise transistors. 20. The sensor of claim 16 wherein the circuit is designed for processing signals of the measuring element. 21. The sensor of claim 16 wherein the tensile coating extends beyond the membrane on at least two opposite sides. 22. The sensor of claim 16 wherein the tensile stress of the coating is at least 100 MPa. 23. The sensor of claim 16 wherein circuit parts are arranged on the membrane and wherein the tensile coating is arranged on the membrane and on the circuit parts. 24. The sensor of claim 16 wherein a protective layer for protecting the electronic components is arranged on the sensor, wherein the protective layer is under compressive stress and wherein the protective layer does not extend over the membrane. 25. The sensor of claim 24 wherein the protective layer and the tensile coating are of silicon nitride. 26. The sensor of claim 16 wherein metallic structures are arranged on the semiconductor device and wherein the tensile coating is separated from the metallic structures by at least one separating layer. 27. A method for producing a sensor having a semiconductor device on which a measuring element and a circuit with active electronic components are integrated, the measuring element being arranged on a membrane above an opening or recess of the semiconductor device, said method comprising the steps of applying a compressive protective layer on the semiconductor device, removing the compressive protective layer at least in a region of the membrane and applying the tensile coating at least in the region of the membrane. 28. The method of claim 27 wherein, below the protective layer, a topmost metal layer is arranged and wherein, for removing the protective layer, the protective layer is etched off by a first etching agent, wherein the topmost metal layer acts as an etch stop, whereupon the topmost metal layer is removed by a second etching agent. 29. Sensor of claim 16 wherein the circuit is designed for processing signals of the measuring element and not covered by the tensile coating. 30. Sensor of claim 16 wherein the tensile coating extends beyond all sides of the membrane. 31. Sensor of claim 16 wherein metallic structures are arranged on the semiconductor device and wherein the tensile coating is separated from the metallic structures by at least one separating layer of silicon oxide. 32. A flow sensor comprising a semiconductor device with a recess or opening therein, a membrane above the recess or opening, a measuring element integrated on the semiconductor device, and arranged on the membrane a circuit with active electronic components integrated on the semiconductor device, a tensile coating for tautening the membrane, wherein the tensile coating leaves at least a part of the active components of the circuit uncovered. 33. A sensor comprising a semiconductor device with a recess or opening therein, a membrane above the recess or opening, a measuring element integrated on the semiconductor device, and arranged on the membrane a circuit with active electronic components integrated on the semiconductor device, a tensile coating for tautening the membrane, wherein the tensile coating leaves at least a part of the active components of the circuit uncovered.

<SOH> BACKGROUND OF THE INVENTION <EOH>The invention relates to a sensor according to the preamble of claim 1 as well as to a method of its production. Sensors of this type are e.g. flow or temperature sensors, where at least a part of the measuring element is arranged on a membrane. This membrane has often a thickness of a few micrometers only and spans an opening or recess in the semiconductor device. Preferably, further active electronic components are integrated on the semiconductor device of sensors of this type, such as transistors for amplifiers or reference voltage sources. The membrane is usually formed by the layers deposited during the production of the circuit, wherein the semiconductor below the layers is etched away. The layers that are deposited in most of the conventional production processes, are, however, usually under compressive stress, i.e. pressure forces are acting within the plane of the layer, e.g. because the layers were applied at elevated temperatures and contracted less than the substrate while cooling down. The magnitude of the compressive stress depends on the manufacturing process and on the layer structure of the membrane. This compressive stress can lead to an undesired buckling of the membrane, which renders it mechanically unstable.