For Crystallization From Liquid Or Supercritical State Patents (Class 117/206)
  • Patent number: 6364947
    Abstract: In method for manufacturing a silicon single crystal in accordance with a Czochralski method, during the growth of the silicon single crystal, pulling is performed such that a solid-liquid interface in the crystal, excluding a peripheral 5 mm-width portion, exists within a range of an average vertical position of the solid-liquid interface ±5 mm. There is also disclosed a method for manufacturing a silicon single crystal in accordance with the Czochralski method, wherein during the growth of a silicon single crystal, a furnace temperature is controlled such that a temperature gradient difference &Dgr;G (=Ge−Gc) is not greater than 5° C./cm, where Ge is a temperature gradient (° C./cm) at a peripheral portion of the crystal, and Gc is a temperature gradient (° C./cm) at a central portion of the crystal, both in an in-crystal descending temperature zone between 1420° C. and 1350° C. or between a melting point of silicon and 1400° C.
    Type: Grant
    Filed: September 14, 2000
    Date of Patent: April 2, 2002
    Assignee: Shin-Etsu Handotai Co., Ltd.
    Inventors: Makoto Iida, Eiichi Iino, Masanori Kimura, Shozo Muraoka, Hideki Yamanaka
  • Patent number: 6352588
    Abstract: For producing ultra pure materials a first station has a porous gas distributor. A material supply supplies material to the porous gas distributor. A gas source supplies gas to the distributor and through the distributor to the material in contact with the distributor. A heater adjacent the porous gas distributor heats and melts the material as gas is passed through the material. Dopant and a treatment liquid is or solid supplied to the material. Treated material is discharged from the first station into a second station. A second porous gas distributor in the second station distributes gas through the material in the second station. A crucible receives molten material from the second station for casting, crystal growing in the crucible or for refilling other casting or crystal growth crucibles. The material and the porous gas distributor move with respect to each other. One porous gas distributor is cylindrical and is tipped.
    Type: Grant
    Filed: February 16, 2000
    Date of Patent: March 5, 2002
    Assignee: Optoscint, Inc.
    Inventor: Kiril A. Pandelisev
  • Patent number: 6319315
    Abstract: Provided is a method which can facilitate crystallization of a biological macromolecule such as protein. A silicon crystal whose valence electrons are controlled so that the concentration of holes or electrons in the surface part can be controlled in response to the environment of a buffer solution containing a biological macromolecule such as protein is brought into contact with the solution, for depositing a crystal of the biological macromolecule on the surface of the silicon crystal. A plurality of grooves or holes whose sizes differ from each other are formed on the silicon crystal, and the valence electrons are so controlled that crystallization of the biological macromolecule is facilitated inside rather than outside the grooves or holes. The crystal of the biological macromolecule grows in the grooves or holes coming into contact with the solution.
    Type: Grant
    Filed: May 8, 2000
    Date of Patent: November 20, 2001
    Assignee: Sumitomo Metal Industries, Ltd.
    Inventor: Akira Sanjoh
  • Patent number: 6315966
    Abstract: Continuously operated, two-part crystallizer which is particularly suitable for the resolution of racemic mixtures, and process for separating solid mixtures which are difficult to separate, in particular racemates.
    Type: Grant
    Filed: December 15, 1998
    Date of Patent: November 13, 2001
    Assignee: Haarmann & Reimer GmbH
    Inventors: Hans-Dieter Baumgard, Bernhard Haedke, Josef Himmelreich, Helmut Judat
  • Patent number: 6309461
    Abstract: A method and apparatus for producing crystals that minimizes birefringence even at large crystal sizes, and is suitable for production of CaF2 crystals. The method of the present invention comprises annealing a crystal by maintaining a minimal temperature gradient in the crystal while slowly reducing the bulk temperature of the crystal. An apparatus according to the present invention includes a thermal control system added to a crystal growth and annealing apparatus, wherein the thermal control system allows a temperature gradient during crystal growth but minimizes the temperature gradient during crystal annealing. An embodiment of the present invention comprises a secondary heater incorporated into a conventional crystal growth and annealing apparatus. The secondary heater supplies heat to minimize the temperature gradients in the crystal during the annealing process. The secondary heater can mount near the bottom of the crucible to effectively maintain appropriate temperature gradients.
    Type: Grant
    Filed: June 7, 1999
    Date of Patent: October 30, 2001
    Assignees: Sandia Corporation, Corning, Incorporated
    Inventors: Steven E. Gianoulakis, Robert Sparrow
  • Publication number: 20010027745
    Abstract: A device for promoting protein crystal growth (PCG) using microfluidic channels. A protein sample and a solvent solution are combined within a microfluidic channel having laminar flow characteristics which forms diffusion zones, providing for a well defined crystallization. Protein crystals can then be harvested from the device. The device is particularly suited for microgravity conditions.
    Type: Application
    Filed: March 30, 2001
    Publication date: October 11, 2001
    Inventors: Bernhard H. Weigl, Jurgen Sygusch
  • Patent number: 6258331
    Abstract: A simple and economic apparatus for crystal growth effective in crystallization of a biological macromolecule such as protein is provided. The apparatus for crystal growth includes first liquid storage parts and for holding a liquid to be used for crystal growth, passages and for transporting the liquid from the first liquid storage parts and to other places, and a second liquid storage part for receiving the liquid transported by the passages and. The first liquid storage parts and are formed on a substrate formed of a general-purpose material such as glass. The second liquid storage part is formed on a doped silicon substrate. Crystal growth occurs on the surface of the silicon substrate having a certain electric state.
    Type: Grant
    Filed: April 26, 2000
    Date of Patent: July 10, 2001
    Assignee: Sumitomo Metal Industries, Ltd.
    Inventor: Akira Sanjoh
  • Patent number: 6254677
    Abstract: An apparatus for and method of producing a large semiconductor crystal at a low cost are provided. The apparatus for producing a semiconductor crystal includes a reactor (1) having an open end at both ends thereof, that is formed of any material selected from the group consisting of silicon carbide, silicon nitride, aluminum nitride, and aluminum oxide, or of a composite material including a base material selected from the group consisting of silicon carbide, silicon nitride, aluminum nitride, boron nitride, aluminum oxide, magnesium oxide, mullite, and carbon as a base, and including an oxidation-proof or airtight film formed on the surface of the base. The apparatus further includes a resistance heater (3) arranged around the reactor (1) in the atmosphere, a flange (9) attached at the open end to seal the reactor (1), and a crucible (2) mounted in the reactor (1) to store material of a semiconductor crystal. The material stored in the crucible (2) is heated and melted to form a material melt (60).
    Type: Grant
    Filed: December 21, 1998
    Date of Patent: July 3, 2001
    Assignee: Sumitomo Electric Industries, Ltd.
    Inventors: Katsushi Hashio, Shin-ichi Sawada, Masami Tatsumi
  • Patent number: 6179914
    Abstract: A time-released dopant delivery system and method are provided in a Czochralski-type crystal-growing furnace to enable continuous doping of the melt over time. The dopant delivery system and method adjusts dopant levels within the melt as a function of time such that a controlled amount of dopant and, more typically, a substantially constant amount of dopant can be incorporated into the ingot over its length. By controlling the doping level in the ingot, the resistivity profile of the ingot can also be controlled over its length. In order to provide controlled dopant delivery, the dopant delivery system generally includes a vessel defining an internal cavity within which the dopant is disposed and an orifice through which the dopant, typically a molten dopant, is released. The dopant delivery system can also include means for submerging the vessel within the melt such that heat from the melt melts and therefore releases the dopant into the melt.
    Type: Grant
    Filed: February 2, 1999
    Date of Patent: January 30, 2001
    Assignee: SEH America, Inc.
    Inventor: Richard M. Aydelott
  • Patent number: 6174365
    Abstract: Provided are an apparatus and a method which can accelerate crystallization of a biological macromolecule such as protein. A plurality of solution storage parts are formed on a silicon substrate whose valence electrons are controlled by controlling the concentration and/or the type of impurity. These solution storage parts are connected with each other by passages. The storage part is made to hold a buffer solution containing molecules of protein or the like to be crystallized. The storage parts are also made to hold solutions capable of accelerating crystallization of protein or the like respectively. These solutions are shifted to the solution storage part through the passages for preparing a mixed solution in a different ratio in each storage part. Thus, different conditions for crystallization can be simultaneously formed in a short time with a small amount of sample. A crystal of protein or the like is grown in the storage part holding the mixed solution.
    Type: Grant
    Filed: January 6, 1999
    Date of Patent: January 16, 2001
    Assignee: Sumitomo Metal Industries, Ltd.
    Inventor: Akira Sanjoh
  • Patent number: 6153007
    Abstract: The present invention relates to a manufacturing method for a monocrystal and to a monocrystal manufacturing device. The present invention relates to a technology for manufacturing a granular monocrystal, wherein: melt of melted raw material is made into a supercooled spherical melt; while the melt is levitated under microgravitational conditions, the free energy of a portion of the surface of the melt is reduced, and a monocrystal is grown. A monocrystal manufacturing device 31 comprises: a gold image furnace 35, a chamber 33, a raw material supply/retention mechanism 38; a drop tube 36 and a drop tube 37; a rotating plate 39; a recovery vat 40; and the like. Raw material 32a of semiconductor material is heated and melted and allowed to free fall in a vacuum inside drop tubes 36, 37. During the drop, rotating plate 39 comes into contact with a portion of the surface of supercooled spherical melt 32b, and a crystal nucleus is generated.
    Type: Grant
    Filed: June 22, 1999
    Date of Patent: November 28, 2000
    Inventor: Josuke Nakata
  • Patent number: 6123769
    Abstract: A method which can control crystallization of a biopolymer such as protein is provided. A silicon crystal (15) whose valence electrons are controlled to be capable of controlling the concentration of holes or electrons of the surface part in response to the environment of a buffer solution (14) containing the biopolymer such as protein is brought into contact with the solution (14), for getting a crystal of the biopolymer deposited on the surface of the silicon crystal (15). Crystallization is controlled by an electrical state which is generated by the controlled valence electrons on the surface of the silicon crystal (15).
    Type: Grant
    Filed: September 15, 1999
    Date of Patent: September 26, 2000
    Assignee: Sumitomo Metal Industries, Ltd.
    Inventor: Akira Sanjoh
  • Patent number: 6120602
    Abstract: An apparatus and a method for producing single crystal semiconductor particulate in near spherical shape and the particulate product so formed is accomplished by producing uniform, monosized, near spherical droplets; identifying the position of an undercooled droplet in a nucleation zone; and seeding the identified droplet in the nucleation zone to initiate single crystal growth in the droplet.
    Type: Grant
    Filed: December 28, 1999
    Date of Patent: September 19, 2000
    Assignee: Starmet Corporation
    Inventors: Matthew D. Stephens, Steven A. Miller, Jessica Belcher
  • Patent number: 6090201
    Abstract: A piston-activated crystal-growing apparatus includes a crucible for containing a seed and a solidifiable liquid covering the seed. In operation, thermal gradient is established in the crucible, and a piston moves within the crucible in the direction of the crystal.
    Type: Grant
    Filed: April 2, 1998
    Date of Patent: July 18, 2000
    Assignee: Commissariat a l'Energie Atomique
    Inventors: Thierry Duffar, Pierre Dusserre
  • Patent number: 6074476
    Abstract: A system and method for forming spherical semiconductor crystals is disclosed. The system includes a receiver tube 18 for receiving semiconductor granules 104. The granules are then directed to a chamber 14 defined within an enclosure 20. The chamber maintains a heated, inert atmosphere with which to melt the semiconductor granules into a molten mass. A nozzle, 40, creates droplets from the molten mass, which then drop through a long drop tube 16. As the droplets move through the drop tube, they form spherical shaped semiconductor crystals 112. The drop tube is heated and the spherical shaped semiconductor crystals may be single crystals. An inductively coupled plasma torch positioned between the nozzle and the drop tube melts the droplets, but leaving a seed in-situ. The seed can thereby facilitate crystallization.
    Type: Grant
    Filed: December 10, 1998
    Date of Patent: June 13, 2000
    Assignee: Ball Semiconductor, Inc.
    Inventors: Murali Hanabe, Nainesh J. Patel, Evangellos Vekris
  • Patent number: 6039804
    Abstract: The present invention provides a crystallization unit including a solvent reservoir in gaseous communication with a plurality of chambers. Preferably, a plurality of crystallization units are arrayed in the form of a crystallization tray. A first preferred embodiment of the present invention provides a crystallization tray 10 including a rectangular array of crystallization units 26. Each crystallization unit includes a central reservoir 28 and four drop chambers 32 arranged in a cruciform configuration around central reservoir 28. Each drop chamber 32 is connected to central reservoir 28 by a diffusion channel 30. Each drop chamber 32 also includes a shoulder which is capable of supporting a cover slip from which a drop of solution, containing the substance to be crystallized, can be suspended.
    Type: Grant
    Filed: September 9, 1998
    Date of Patent: March 21, 2000
    Assignee: Emerald BioStructures, Inc.
    Inventors: Hidong Kim, Lansing Joseph Stewart
  • Patent number: 6027565
    Abstract: An apparatus for producing crystals of a macromolecule in microgravity includes a container 100 which is made of a material having a low thermal conductivity and an open end. A thermally conductive lid 102 is fitted on the open end of the container to close the container and a heat source/sink 114 is provided in thermal contact with the thermally conductive lid to generate a temperature gradient within the container. When a solution of the macromolecule is provided in the container, the temperature gradient induces and control the crystallization of the macromolecule. In operation, a temperature ramp from a start temperature to an end temperature is used to maintain and control the temperature gradient.
    Type: Grant
    Filed: October 9, 1997
    Date of Patent: February 22, 2000
    Inventors: Charles E. Bugg, Lawrence L. Delucas, Tattanhalli L. Nagabhushan, Paul P. Trotta, Michael D. Harrington, John Bradford Bishop, deceased, by Sue C. Bishop, executrix
  • Patent number: 6019842
    Abstract: The process of manufacturing silicon single crystals by the CZ method is significantly improved by the present apparatus wherein raw material (polycrystalline silicon) is automatically loaded into a quartz crucible. After a protection sheet (15) is employed to cover the inner side wall of the container (3), which has an inner diameter smaller than that of the quartz crucible (10), a present amount of polycrystalline silicon (17) is loaded from the loading means (6) into the container (3). The container (3) is then filled with pure water that is thereafter frozen into an ice block (22). Subsequently, the ice block (22) is raised up from the container (3). Thereafter, the protection sheet (15) is removed from the ice block (22) and the ice block (22) is loaded into the quartz crucible (10). The ice block (22) is then caused to melt and the quartz crucible (10) and polycrystalline silicon are caused to dry up. The above operations are performed by the conveying apparatus (1).
    Type: Grant
    Filed: September 9, 1998
    Date of Patent: February 1, 2000
    Assignee: Komatsu Electronics Metals Co., Ltd.
    Inventor: Yoshifumi Yatsurugi
  • Patent number: 6001176
    Abstract: A device for specific formation of nuclei or crystals on the surface of a dielectric in contact with a solution, especially on the functional groups of a polymer, in which there is a device for generating an electric field in the dielectric.
    Type: Grant
    Filed: September 25, 1996
    Date of Patent: December 14, 1999
    Assignees: Klaus Leiter, Gerhard Walder
    Inventors: Klaus Leiter, Gerhard Walder
  • Patent number: 5993902
    Abstract: An apparatus and a method for preventing buildup of silicon oxides and silicon carbides on the inner surface of exhaust sleeves utilized in Czochralski (Cz) silicon crystal pullers are provided. The apparatus and the method include the provision of a vapor impervious layer coated on the inner surface of an exhaust sleeve, and forming a barrier to silicon oxides and silicon carbides deposition on the inner surface, to prevent the buildup of silicon oxides and silicon carbides on the surface of exhaust sleeves, thereby allowing more uniform laminar flow of process gases in the Cz chamber and the exhaust sleeve, and extending the useful lifetime of exhaust sleeves.
    Type: Grant
    Filed: April 9, 1997
    Date of Patent: November 30, 1999
    Assignee: SEH America, Inc.
    Inventor: Gary Randolph Heid
  • Patent number: 5989337
    Abstract: An object of the present invention is to prevent introduction of cracks or defects into the grown single crystal and to obtain a compound semiconductor single crystal having a good crystallinity and no cracks. In the method, after ZnTe polycrystalline raw material and Te solvent are put in a crucible 3, they are heated by a heater 1 to make a solution by dissolving the ZnTe polycrystalline raw material in the Te solvent. The solution is solidified to grow a ZnTe single crystal by using the Bridgman method or the gradient freeze method, and thereafter, the remaining Te solvent in the crucible 3 is removed out of the crucible 3 by evaporation, and then the grown crystal is taken out of the crucible 3.
    Type: Grant
    Filed: April 15, 1997
    Date of Patent: November 23, 1999
    Assignee: Japan Energy Corporation
    Inventor: Kenji Sato
  • Patent number: 5972107
    Abstract: An apparatus for purifying metallurgical grade silicon to produce solar grade silicon has a container for holding molten silicon and one or more submergible torches for providing a flame surrounded by inert gas to heat the molten silicon so that the reaction time is prolonged, to create turbulence, and to introduce silica powder and water vapor for reactions with molten silicon. The molten silicon is then directionally solidified by providing the container in a coolant tank and controlling the coolant level with controllable valves so that further purification is achieved by segregating impurities.
    Type: Grant
    Filed: August 28, 1997
    Date of Patent: October 26, 1999
    Assignee: Crystal Systems, Inc.
    Inventors: Frederick Schmid, Chandra P. Khattak
  • Patent number: 5932005
    Abstract: The material of the crystal (2) formed by solidification is deposited in a crucible (1), whose wall is perforated by two ducts for the injection of pressure at different heights (6, 7). A differential pressure is created between the two ducts, the pressure of the lower duct (7) being higher by a value roughly equal to the hydrostatic pressure of the remaining liquid (3), so that a clearance (5) is spontaneously formed between the crystal (2) and the crucible (1) and problems caused by differential thermal contractions on cooling are avoided.
    Type: Grant
    Filed: December 11, 1997
    Date of Patent: August 3, 1999
    Assignees: Commissariat A L'Energie Atomique, Centre National D'Etudes Spatiales
    Inventors: Thierry Duffar, Jacques Abadie, Pierre Dusserre
  • Patent number: 5908604
    Abstract: The invention provides an apparatus for growing zeolite crystals from an aqueous solution in a metallic pressure tank for admitting pressure to the aqueous solution. Devices for feeding microwave energy into the aqueous solution comprise a capacitor between whose plates the aqueous solution is situated, one of the capacitor plates being formed by a wall of the pressure tank and the other capacitor plate being arranged in the interior of the pressure tank.
    Type: Grant
    Filed: December 23, 1996
    Date of Patent: June 1, 1999
    Assignee: Dornier GmbH
    Inventors: Christian Stenzel, Harald Lenski, Werner Wiesbeck, Frank Demmerle
  • Patent number: 5904772
    Abstract: A device for isolation of see crystals during processing of solutions. The device enables a seed crystal to be introduced into the solution without exposing the solution to contaminants or to sources of drying and cooling. The device constitutes a seed protector which allows the seed to be present in the growth solution during filtration and overheating operations while at the same time preventing the seed from being dissolved by the under saturated solution. When the solution processing has been completed and the solution cooled to near the saturation point, the seed protector is opened, exposing the seed to the solution and allowing growth to begin.
    Type: Grant
    Filed: August 18, 1997
    Date of Patent: May 18, 1999
    Assignee: The Regents of the University of California
    Inventors: Kenneth E. Montgomery, Natalia P. Zaitseva, James J. Deyoreo, Russell L. Vital
  • Patent number: 5900058
    Abstract: An apparatus for producing a single crystal by the Czochralski method is disclosed in which an exhaust system is provided with a water sealing bubbler. On the upstream side of the bubbler is provided a buffer or a vacuum breaker or a buffer and a vacuum breaker. The structure prevents the sealing water in the bubbler from flowing backward, so that danger of steam explosion can be avoided.
    Type: Grant
    Filed: December 5, 1996
    Date of Patent: May 4, 1999
    Assignee: Shin-Etsu Handotai Co., Ltd.
    Inventors: Kouji Mizuishi, Atsushi Iwasaki
  • Patent number: 5772761
    Abstract: The invention concerns a crystallization furnace for a material with low thermal conductivity arid/or low hardness.This furnace can obtain high quality single crystals.This furnace comprises a heating chamber (1), heating means (13) to create a temperature profile along the center line of said chamber and thus define at least one heating zone (3), and at least one cooling zone (5) and a crucible (9) filled with a solution of a solute to be crystallized in a solvent, said crucible (9) being fixed and placed in the heating chamber (1) in the heating zone (3), characterized in that the furnace also comprises:a crystallization device (27) comprising a temperature homogenizer (29A) and a heat sink (29B) separated by a thermally insulating spacer (31), said temperature homogenizer, heat sink and insulating spacer being rigidly attached to each other, andmeans (37) of displacing said crystallization device (27) along the center line of the chamber and around said crucible (9).
    Type: Grant
    Filed: November 8, 1996
    Date of Patent: June 30, 1998
    Assignee: Commissariat a l'Energie Atomique
    Inventor: Gerard Petroz
  • Patent number: 5766342
    Abstract: The method for forming a silicon film of this invention includes the steps of introducing a compound containing silicon and chlorine and being in a liquid form under normal pressure and at an ordinary temperature into a reaction chamber, and spraying the compound in the liquid form in a fine particle state to a surface of a substrate supported in the reaction chamber, and decomposing the compound in the fine particle state by energy applied from outside of the reaction chamber, and depositing a silicon film on the substrate supported in the reaction chamber.
    Type: Grant
    Filed: October 17, 1995
    Date of Patent: June 16, 1998
    Assignee: Matsushita Electric Industrial Co., Ltd.
    Inventors: Munehiro Shibuya, Masatoshi Kitagawa, Yuji Mukai, Takashi Hirao, Akihisa Yoshida
  • Patent number: 5759267
    Abstract: In an improved liquid phase epitaxial growth method and apparatus in which a plurality of substrates are placed in a deposition chamber having at least one first vent hole; a solution for liquid phase growth is held in a solution chamber having at least one second vent hole and at least two sub-chambers separated by a partition plate and communicated with each other via a communicating portion; and before the substrates and the solution for liquid phase growth are brought into contact with each other, the deposition chamber and the solution chamber are revolved for causing the solution for liquid phase growth to move through the communicating portion so as to increase and decrease the volume of space portions of the respective sub-chambers and thereby replacement of a heat-treatment gas in the deposition chamber and the solution chamber is undertaken to achieve heat treatment.
    Type: Grant
    Filed: October 10, 1996
    Date of Patent: June 2, 1998
    Assignee: Shin-Etsu Handotai Co., Ltd.
    Inventors: Munehisa Yanagisawa, Susumu Higuchi, Yuji Yoshida, Masahiko Saito
  • Patent number: 5679151
    Abstract: Method of forming a single crystal of ZnSe. A charge of material is loaded in a container. The charge of material is melted to create a melt of material. A single crystal is grown from the melt of material. Then, the grown crystal is brought out of contact with the wall surface of the container. The temperature of the crystal is varied across its phase transition temperature range while establishing a temperature gradient from one end of the grown crystal to the other end. This method is carried out, using a crystal grower comprising the container and an elevation member. The container is disposed inside a high-pressure vessel. The container tapers off downward and is provided with a hole extending from its lower end. The elevation member is inserted into the hole from below to push the grown crystal in a crucible upward. The container is composed of plural separable parts.
    Type: Grant
    Filed: February 21, 1996
    Date of Patent: October 21, 1997
    Assignee: Kabushiki Kaisha Kobe Seiko Sho
    Inventors: Seiichiro Ohmoto, Katsuhiro Uehara, Hiroshi Okada, Yoshihiko Sakashita, Takao Kawanaka
  • Patent number: 5662870
    Abstract: A system for the solid phase polymerization of polymers wherein cold amorphous polymer is introduced to a crystallizer and heated to crystallize the polymer, the crystallized polymer is discharged to a reactor to achieve polymerization of the polymer, and the hot polymer product of the reactor is discharged to a fluid bed cooler for cooling of the polymerized product. The fluid bed cooler includes an inlet for the hot polymer and an inlet for the cooling gas, and the cooled polymer and the heated gas are discharged from the cooler after contact of the gas with the polymer. The cooler includes a bed portion through which the polymer moves while in contact with the cooling gas, and an upper chamber which collects the heated gas.
    Type: Grant
    Filed: November 27, 1995
    Date of Patent: September 2, 1997
    Assignee: Hosokawa Bepex Corporation
    Inventor: John J. Walsh
  • Patent number: 5650008
    Abstract: Growth of homogeneous single crystals is carried out by a modified Bridgman-type process using a second melt of a different composition to replenish the first melt of a predetermined composition held in the crystal growth container. By controlling the replenishing rate and suppressing diffusion between the two melts, composition variations in the first melt and hence the growing crystal are compensated. The second melt may be maintained at a predetermined higher temperature than the first melt. The first melt may be agitated during crystal growth by rotation. A liquid encapsulant may be used.
    Type: Grant
    Filed: December 1, 1995
    Date of Patent: July 22, 1997
    Assignee: Advanced Materials Processing, LLC
    Inventors: Sindo Kou, Ying Tao
  • Patent number: 5578279
    Abstract: There is disclosed a dual jet crystallizer apparatus comprising a crystallization or mixing chamber having opposed angularly disposed arms which removably receive jet nozzles. One end of the chamber is provided with means to discharge crystallized product therefrom while the other end is equipped with means to adjust the crystallization volume within the chamber. The angular arms are disposed within specified angular tolerances with respect to the longitudinal axis of the chamber. One of the jet nozzles is provided with means at one end to receive and deliver to the chamber compound to be crystallized while one end of the other jet nozzle is provided with means to receive and deliver to the chamber a crystallization agent for the compound. The opposite ends of each of the jet nozzles have means to removably secure them to the angular arms and the ends thus secured have a nozzle tip section formed therein defining an orefice having an elongated bore.
    Type: Grant
    Filed: June 5, 1995
    Date of Patent: November 26, 1996
    Assignee: Merck & Co., Inc.
    Inventors: Richard Dauer, Jonathan E. Mokrauer, Walter J. McKeel
  • Patent number: 5531185
    Abstract: A manufacturing apparatus which thermal design is easy, and which is small in size and light in weight is provided which is operated by a person in a micro-gravity environment. The manufacturing apparatus has a manufacturing unit having an operation side on which an operation is performed directly by the hand of an operator who faces the front of the facility, and a housing section for supporting the manufacturing unit slidably along the operation side and in such a manner as to be pulled out from the front of the apparatus to the outside. The manufacturing unit is housed with the operation side being vertical, and slides substantially horizontally. Also, an observation facility is disposed between two manufacturing unit housed in a constant-temperature tank so that the two facing sides of the member are observed simultaneously.
    Type: Grant
    Filed: September 30, 1994
    Date of Patent: July 2, 1996
    Assignee: Fujitsu Limited
    Inventors: Koji Asano, Atsushi Shiraishi, Hidefumi Ueda
  • Patent number: 5454344
    Abstract: A system for crystallization of polymers involving the use of a stationary housing with a rotor mounted for rotation within the housing. The rotor supports a plurality of spaced apart hollow discs and heated fluid is delivered to the interior of the discs. The polymer material to be treated is fed into the housing for heat exchange contact with the exterior surfaces of the discs. The rotation of the discs in addition serves as the propelling force for the material along the length of the housing at which point the material is discharged. The speed of rotation of the rotor is controlled to influence agitation and conveying of material in the housing to thereby control the crystallization reaction. A holdup mechanism which operates independently of the speed control is located adjacent the discharge location to contribute to the fixing of the residence time.
    Type: Grant
    Filed: November 16, 1994
    Date of Patent: October 3, 1995
    Assignee: Hosokawa Bepex Corporation
    Inventors: Ilya Pikus, Greg J. Kimball, Masayuki Inoue
  • Patent number: 5423288
    Abstract: An apparatus for producing seed crystals in melts has a vertically oriented, closed vessel having a vessel base and having at least one inlet for the melt and having at least one outlet opening for the inoculated melt provided with seed crystals. A preferably annular region of the vessel wall is constructed as a cooling surface. In the interior of the vessel there is arranged a scraping unit which comprises a motor-driven rotating shaft which extends axially through the vessel as far as a point just short of the vessel base. At its end towards the vessel base, the shaft is provided with at least one scraping arm which, starting from the lower end of the shaft close to the vessel base, extends first in the direction towards the vessel wall and thence substantially parallel to the annular cooling surface and axially parallel to the drive shaft.
    Type: Grant
    Filed: February 24, 1994
    Date of Patent: June 13, 1995
    Assignee: Ciba-Geigy Corporation
    Inventors: Ricardo Schneeberger, Hans Horisberger, Rudolf Buttiker
  • Patent number: 5423287
    Abstract: Crystal growing cell including first and second casings. The first casing has a first solution chamber for containing a first solution therein. The first solution chamber has an opening. The second casing has a closing member placed therein for movement in a first direction and in a second direction opposite to the first direction. The second casing has a third casing placed therein. The third casing is fixed to the first casing around the opening to form a second solution chamber for containing a second solution therein. The closing member is moved in the first direction to close the opening so as to separate the first solution chamber from the second solution chamber. The closing member is moved in the second direction to open the opening so as to connect the first solution chamber to the second solution chamber.
    Type: Grant
    Filed: November 22, 1993
    Date of Patent: June 13, 1995
    Assignees: Nissan Motor Company, Ltd., National Space Development Agency of Japan
    Inventors: Ron Usami, Shunji Nagaoka, Tsutomu Udaka, Kazunori Kawasaki, Shoji Muramatsu
  • Patent number: 5419278
    Abstract: In accordance with the present invention, a vapor equilibrium apparatus for growing and screening suitable protein crystals is provided which consists of a plastic tray having a plurality of roughly cylindrical chambers that act as reservoirs for vapor equilibrating solutions and include a plurality of rib members having flattened upper ends recessed from the top of the chamber which form retaining levels wherein glass cover slips can be retained horizontally across the chambers in order to carry out the vapor equilibrating process. The upper ends can also be formed in a step-shaped fashion so as to provide multiple retaining levels of differing inner diameters which can retain glass cover slips of different sizes in the same chamber.
    Type: Grant
    Filed: May 25, 1994
    Date of Patent: May 30, 1995
    Inventor: Daniel C. Carter
  • Patent number: 5410984
    Abstract: A system for crystallization of polymers involving the use of a stationary housing with a rotor mounted for rotation within the housing. The rotor supports a plurality of spaced apart hollow discs and heated fluid is delivered to the interior of the discs. The polymer material to be treated is fed into the housing for heat exchange contact with the exterior surfaces of the discs. The rotation of the discs in addition serves as the propelling force for the material along the length of the housing at which point the material is discharged. The speed of rotation of the rotor is controlled to influence agitation and conveying of material in the housing to thereby control the crystallization reaction. A holdup mechanism which operates independently of the speed control is located adjacent the discharge location to contribute to the fixing of the residence time.
    Type: Grant
    Filed: March 1, 1993
    Date of Patent: May 2, 1995
    Assignee: Bepex Corporation
    Inventors: Ilya Pikus, Greg J. Kimball, Masayuki Inoue
  • Patent number: 5408953
    Abstract: The average size of ammonium sulfate crystals is increased by passing undersized ammonium sulfate crystals through a multistage apparatus in which the crystals are contacted with an aqueous ammonium sulfate spray in a first heated chamber to increase the average size of the crystals, the enlarged crystals thereafter passing through a second heated chamber to dry the enlarged crystals.
    Type: Grant
    Filed: April 25, 1994
    Date of Patent: April 25, 1995
    Assignee: BASF Corporation
    Inventors: Walter G. Thomson, Jonathan K. Kramer
  • Patent number: 5400741
    Abstract: A varisized diffusion cell device (10) comprising a plurality of diffusion cells (18) arranged in rows (20A) to (20F) having progressively greater depths for growing high quality, diffraction grade crystals, is described. In use, the diffusion cells receive a quantity of crystallizing agent (32) that dissolves and diffuses through a head of solvent solution (34) to equilibrate with a drop (38) containing a subject macro-molecular material for growing crystals. The various depths of the diffusion cells provide various diffusion rates and therefore various equilibration rates. Through empirical methods, an optimum diffusion rate for a given crystal growth system can easily be determined.
    Type: Grant
    Filed: May 21, 1993
    Date of Patent: March 28, 1995
    Assignee: Medical Foundation of Buffalo, Inc.
    Inventors: George T. DeTitta, Joseph R. Luft
  • Patent number: 5396863
    Abstract: Installation for the crystallization of an inorganic substance in a crystal slurry, by desupersaturation of a supersaturated solution, the installation comprising a crystallization chamber which has a vertical axis and is divided into a central zone (4) and an annular zone (5), a device (9, 10) designed to bring about a vertical translation of the slurry in the central zone (4) and a translation in the opposite direction in the annular zone (5), a device (8) for withdrawing slurry, comprising a tube (23, 24) which opens into one of the abovementioned zones, a member (14) for mechanical shearing of the slurry, comprising, a disc (17) carrying a ring of shearing teeth (19), and a tube (6, 31) passing through the cover (30) and serving to introduce anhydrous sodium carbonate, the tube (31) having a prolongation inside the crystallization chamber, over which prolongation a film of water is caused to circulate.
    Type: Grant
    Filed: March 9, 1993
    Date of Patent: March 14, 1995
    Assignee: Solvay (Societe Anonyme)
    Inventors: Leon Ninane, Claude Breton
  • Patent number: 5394827
    Abstract: A direct contact cryogenic crystallizer having a vertically oriented draft tube into which cryogenic fluid is injected at a high velocity along with warm gas and through which a crystal slurry is drawn for subsequent cooling and agitation for the production of crystals.
    Type: Grant
    Filed: July 15, 1994
    Date of Patent: March 7, 1995
    Assignee: Praxair Technology, Inc.
    Inventor: Alan T. Cheng
  • Patent number: 5362455
    Abstract: A direct contact cryogenic crystallizer having a vertically oriented draft tube into which cryogenic fluid is injected at a high velocity along with warm gas and through which a crystal slurry is drawn for subsequent cooling and agitation for the production of crystals.
    Type: Grant
    Filed: January 29, 1993
    Date of Patent: November 8, 1994
    Assignee: Praxair Technology, Inc.
    Inventor: Alan T. Cheng