At Pressure Above 1 Atmosphere (e.g., Hydrothermal Processes) Patents (Class 117/71)
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Patent number: 7156917Abstract: An apparatus for growing a biological macromolecular crystal by vaporizing biological macromolecular solution into an oversaturated state. The apparatus includes a first sealed room that receives first crystallizing agent solution, and a communicating tube that communicates with the first sealed room and has a small sectional area for suppressing convection of air. A plurality of droplets of solution dissolving a biological macromolecule and a crystallizing agent therein are held in the communicating tube with the plurality of droplets being separated from each other.Type: GrantFiled: April 28, 2004Date of Patent: January 2, 2007Assignees: IHI Aerospace Co., Ltd.Inventors: Hideaki Moriyama, Norio Sugi, Kazunori Kawasaki, Shoji Muramatsu
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Patent number: 7115165Abstract: ?-ZrNCl polycrystalline powder prepared by chemical transport method and NH4Cl are mixed in a molar ratio of 1:2. The mixture is encapsulated in a Au capsule (6 mm in inner diameter and 6 mm in depth) of a reaction vessel 2, which is then enclosed in a highly heat-conductivitive sodium chloride block as an electrically insulating pressure medium 6. The mixture held in the sodium chloride block is placed in a carbon tube 8 for serving as a heater. In a cubic-pressing apparatus using a pyrophyllite 12 as a pressure-transmitting medium, the mixture is heated at 900° C. for 2 hours under an applied pressure of 3 GPa. After the mixture is allowed to stand until it is cooled down to room temperature, the Au capsule is taken out and light green ?-ZrNCl single crystals are obtained. A large single crystal among them had a hexagonal plate-like habit and is transparent with dimensions about 2 mm in diameter, and 0.3 mm in thickness.Type: GrantFiled: October 11, 2001Date of Patent: October 3, 2006Assignee: Japan Science and Technology CorporationInventors: Shoji Yamanaka, Xuean Chen
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Patent number: 6841000Abstract: Aqueous mineralizer solutions having retrograde solubility for ZnO contain a mineral acid in which ZnO is soluble and at least one compound of a coordinating ligand for Zn2+ ions wherein the coordinating ligand compound is present in an amount that is effective to inhibit Zn(OH)+ ion formation as ZnO is dissolved in the solution. Reduced temperature methods using the mineralizer solutions to grow pure or doped ZnO crystals, pure or doped ZnO thick or thin films, and pure or doped ZnO crystalline powders are also disclosed. Cation doped ZnOs prepared by the inventive methods are also disclosed.Type: GrantFiled: October 1, 2002Date of Patent: January 11, 2005Assignee: Ceramare CorporationInventors: Larry Eugene McCandlish, Robert Uhrin
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Patent number: 6760396Abstract: The method of protectively coating metallic uranium which comprises dipping the metallic uranium in a molten alloy comprising about 20-75% of copper and about 80-25% of tin, dipping the coated uranium promptly into molten tin, withdrawing it from the molten tin and removing excess molten metal, thereupon dipping it into a molten metal bath comprising aluminum until it is coated with this metal, then promptly withdrawing it from the bath.Type: GrantFiled: February 4, 1946Date of Patent: July 6, 2004Assignee: The United States of America as represented by the United States Department of EnergyInventors: Ernest R. Boller, Lowell D. Eubank
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Patent number: 6491753Abstract: To obtain large, high-quality crystals of a metal orthophosphate, in particular GaPO4 or AlPO4, from a nutrient solution with the use of seeds, a seed crystal is used having at least two rod- or wafer-shaped legs which form an angle with each other and define a main growth region, and which are positioned eccentrically in the single crystal grown. Contagious faces of two seed legs, which have been chosen for crystal growing, enclose an angle <180°. In this way the yield of the high-quality crystal region will be increased.Type: GrantFiled: December 27, 2000Date of Patent: December 10, 2002Assignee: AVL List GmbHInventors: Peter Krempl, Wolfgang Wallnöfer, Ferdinand Krispel, Herbert Thanner
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Patent number: 6398867Abstract: A gallium nitride growth process forms crystalline gallium nitride. The process comprises the steps of providing a source gallium nitride; providing mineralizer; providing solvent; providing a capsule; disposing the source gallium nitride, mineralizer and solvent in the capsule; sealing the capsule; disposing the capsule in a pressure cell; and subjecting the pressure cell to high pressure and high temperature (HPHT) conditions for a length of time sufficient to dissolve the source gallium nitride and precipitate the source gallium nitride into at least one gallium nitride crystal. The invention also provides for gallium nitride crystals formed by the processes of the invention.Type: GrantFiled: October 6, 1999Date of Patent: June 4, 2002Assignee: General Electric CompanyInventors: Mark Philip D'Evelyn, Kristi Jean Narang
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Patent number: 6048396Abstract: This invention provides a method for producing calcite-type calcium carbonate single crystal available for optical elements, which can be carried out under relatively low temperature and low pressure conditions. The crystal growth process which comprises; a first step of filling a sealed pressure container of an autoclave with solvent and calcium carbonate as a raw material for growth, a second step of dissolving the starting rate in the solvent under predetermined conditions of pressure and temperature, a third step of crystallizing the calcium carbonate on a seed crystal suspended in the upper portion of the pressure container, on account of the difference of solubility caused by temperature gradient in the container; the method is characterized by that the aqueous solution of ammonium salt of mono-carboxylic acid is used as the solvent.Type: GrantFiled: July 3, 1997Date of Patent: April 11, 2000Assignee: Toyo Denka Kogyo Co., Ltd.Inventors: Kazumichi Yanagisawa, Isao Matsushita
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Patent number: 6001171Abstract: ST-cut and AT-cut quartz seed bodies (18,40) for quartz crystal synthesis and method (100) for making the same are disclosed. An extended quartz seed body (18) having an angle of about 42.75.degree. rotated about a X axis (20) from a +Z axis (22) to a -Y axis (24) and defining a ST-cut is provided and a quartz crystal bar (32) is grown thereupon. Analogously, an extended quartz seed body (40) having an angle of about 35.25.degree. rotated about a X axis (20) from a +Z axis (22) to a -Y axis (24) and defining an AT-cut is provided and a quartz crystal bar (48) is grown thereupon. In each case, the subsequent quartz crystal bar (32,48) may be wafered parallel to the seed body (18,40) thereby; reducing waste (68), recovering the seed body (18,40) for reuse, producing wafers (70) without intervening seed portions, and increasing factory capacity.Type: GrantFiled: December 15, 1997Date of Patent: December 14, 1999Assignee: CTS CorporationInventors: Joseph F. Balascio, Thien T. Nguyen, David J. Weary, Theodore E. Lind
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Patent number: 5968265Abstract: A method for producing cubic SiC monocrystals includes dissolving SiC powder or other starting material in a solvent at high overpressures and growing the monocrystals on a seed crystal.Type: GrantFiled: January 27, 1998Date of Patent: October 19, 1999Assignee: Siemens AktiengesellschaftInventors: Rene Stein, Roland Rupp, Johannes Volkl
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Patent number: 5902396Abstract: Single crystals of binary and ternary compounds of alkaline earth and a chalcogen, with or without a transition element, are grown by: charging a reaction vessel with an alkaline earth chalcogenide, with or without a transition element or a halide thereof, an acidic mineralizer, and anhydrous ammonia to where the fill factor in the reaction vessel is 30-95%; sealing the reaction vessel to the outside atmosphere; heating the contents of the reaction vessel to a temperature of at least 300.degree. C. until single crystal materials visible to the eye form in the reaction vessel; cooling the contents of the reaction vessel; and extracting the single crystal materials from the reaction vessel.Type: GrantFiled: November 5, 1997Date of Patent: May 11, 1999Assignee: The United States of America as represented by the Secretary of the NavyInventor: Andrew P. Purdy
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Patent number: 5788765Abstract: Crystals formed of a solid-solution of K.sub.2 Ni(SO.sub.4).sub.2 6H.sub.2 O provide very good materials for filtering ultraviolet light and will not deteriorate in temperatures as high as 110.degree. C. They are particularly useful in sensing devices which seek to identify the presence of ultraviolet light in the UV missile warning band.Type: GrantFiled: August 30, 1996Date of Patent: August 4, 1998Assignee: Northrop Grumman CorporationInventors: Narsingh B. Singh, William D. Partlow, Steven Strauch, Albert M. Stewart, John F. Jackovitz, David W. Coffey
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Patent number: 5714005Abstract: ST-cut and AT-cut quartz seed bodies (18,40) for quartz crystal synthesis and method for making the same are disclosed. An extended quartz seed body (18) having an angle of about 42.75.degree. rotated about a X axis (20) from a +Z axis (22) to a -Y axis (24) and defining a ST-cut is provided and a quartz crystal bar (32) is grown thereupon. Analogously, an extended quartz seed body (40) having an angle of about 35.25.degree. rotated about a X axis (20) from a +Z axis (22) to a -Y axis (24) and defining an AT-cut is provided and a quartz crystal bar (48) is grown thereupon. In each case, the subsequent quartz crystal bar (32,48) may be wafered parallel to the seed body (18,40) thereby; reducing waste (68), recovering the seed body (18,40) for reuse, producing wafers (70) without intervening seed portions, and increasing factory capacity.Type: GrantFiled: December 20, 1995Date of Patent: February 3, 1998Assignee: Motorola Inc.Inventors: Joseph F. Balascio, Thien T. Nguyen, David J. Weary, Theodore E. Lind
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Patent number: 5533465Abstract: A seal apparatus is disclosed for sealing an outlet of a pressurized chamber from fluid loss from the chamber and contamination to the chamber. The apparatus includes certain combinations of (a) a chamber outlet structure; (b) a removable cover; (c) means for reversibly connecting the cover to the chamber outlet structure; and (d) a compressible self-energizing ring having a surface which consists essentially of a material selected from the group consisting of noble metals, noble metal alloys and polytetrafluoroethylene, which has a hardness selected to substantially avoid deformation when the cover is sealed to the chamber outlet structure.Also disclosed are certain pressure vessels for hydrothermal crystal growth using a crystal growth media, which comprise (a) a vessel base and (b) a removable vessel cover.Type: GrantFiled: January 20, 1995Date of Patent: July 9, 1996Assignee: E. I. Du Pont de Nemours and CompanyInventors: August Ferretti, Oral R. Van Buskirk
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Patent number: 5456204Abstract: The present invention is a filtering flow guide for hydrothermal reaction vessels--such as crystal growth apparatus--which improves crystal production efficiency and crystal quality without significantly slowing down flow velocities or crystal growth times. One embodiment of the flow guide fits inside a conventional hydrothermal autoclave for crystal growth, and includes at least one central inlet conduit by which crystal nutrient solution flows from the autoclave's dissolving zone into its growth chamber. A plurality of funnels encircle the inlet conduit, the funnels contiguous with each other along their lateral edges and with the inlet conduit's intake opening at the funnels' innermost edges. Each funnel may be substantially shaped as a hollow, inverted triangular pyramid with a nadir instead of an apex, the nadir opening into a filter-containing outlet.Type: GrantFiled: May 28, 1993Date of Patent: October 10, 1995Assignee: Alfa Quartz, C.A.Inventors: Vesselin S. Dimitrov, Navtej S. Saluja, Alfredo Riviere V.
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Patent number: 5411723Abstract: A process is disclosed for treating a crystal of MTiOXO.sub.4 which has crystal structure deficiencies of M and O, wherein M is selected from the group consisting of K, Rb, Tl and NH.sub.4 and mixtures thereof and X is selected from the group consisting of P, As and mixtures thereof, which includes the step of heating said crystal in the presence of a mixture of MTiOXO.sub.4 and at least one inorganic compound of one or more monovalent cations selected from the group consisting of Rb+, K+, Cs+ and Ti+ (said inorganic compound(s) being selected to provide a source of vapor phase monovalent cation and being present in an amount sufficient to provide at least a 0.1 mole % excess of the monovalent cation in relation to the M in the MTiOXO.sub.4 in said mixture) at a temperature of from about 400.degree. C. to 950.degree. C. and a pressure of at least 14 psi, and in the presence of a gaseous source of oxygen for a time sufficient to decrease the optical damage susceptibility of said crystal.Type: GrantFiled: September 22, 1993Date of Patent: May 2, 1995Assignee: E. I. Du Pont de Nemours and CompanyInventor: Patricia A. Morris
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Patent number: 5375556Abstract: In order to obtain large, high-quality crystals or crystal layers of a me orthophosphate, in particular, GaPO.sub.4 or AlPO.sub.4, from a nutrient solution with the use of a seed plate, the proposal is put forward that in the initial phase of the growth process a seed plate of alpha-quartz (.alpha.-SiO.sub.2) be introduced into the nutrient solution, and that fluoride ions (F.sup.-) be added to this solution, at least for formation of the primary crystal layer on the quartz seed plate.Type: GrantFiled: August 23, 1993Date of Patent: December 27, 1994Assignee: AVL Gesellschaft fur Verbrennungskraftmaschinen und Messtechnik m.b.H.Inventors: Peter W. Krempl, Gabriele Voborsky, Uwe Posch, Wolfgang Wallnofer
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Patent number: 5322591Abstract: The growth of bismuth silicate crystals occurs in a high pressure vessel or autoclave using a hydrothermal growth process. The nutrient material is placed in a sealed container of noble metal, liner, along with a solvent to a selected fill level. A filler fluid is also placed between the liner and the pressure vessel. The oriented seeds are placed in the cooler top seed zone over a baffle that slows the movement of supersaturated liquid from the hotter lower nutrient zone. Using a selected heating schedule for the top and the bottom zones, a plurality of large crystals are grown in the seed zone. The temperature differential is about 5.degree. C.Type: GrantFiled: March 26, 1991Date of Patent: June 21, 1994Assignee: The United States of America as represented by the Secretary of the Air ForceInventors: Meckie T. Harris, J. Emery Cormier, John J. Larkin, Alton F. Armington