At Pressure Above 1 Atmosphere (e.g., Hydrothermal Processes) Patents (Class 117/71)
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Patent number: 12024795Abstract: A method for growth of group III metal nitride crystals includes providing a manifold comprising including one or more transfer vessels, a source vessel containing a condensable mineralizer composition, and a receiving vessel, chilling a metallic surface within the one or more transfer vessels, the metallic surface comprising a composition that does not form a reaction product when exposed to the condensable mineralizer composition, transferring a quantity of the condensable mineralizer composition to the one or more transfer vessels via a vapor phase and causing condensation of the condensable mineralizer composition within the one or more transfer vessels, measuring the quantity of the condensable mineralizer composition within the at least one transfer vessel, transferring at least a portion of the condensable mineralizer composition to the receiving vessel, and forming at least a portion of a group III metal nitride boule by an ammonothermal crystal growth process that comprises exposing a seed crystal toType: GrantFiled: October 29, 2021Date of Patent: July 2, 2024Assignee: SLT Technologies, Inc.Inventors: Mark P. D'Evelyn, Paul M. Von Dollen, Lisa M. Gay, Douglas W. Pocius, Jonathan D. Cook
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Patent number: 10975492Abstract: A method for growing a crystalline composition, the first crystalline composition may include gallium and nitrogen. The crystalline composition may have an infrared absorption peak at about 3175 cm?1, with an absorbance per unit thickness of greater than about 0.01 cm?1. In one embodiment, the composition ay have an amount of oxygen present in a concentration of less than about 3×1018 per cubic centimeter, and may be free of two-dimensional planar boundary defects in a determined volume of the first crystalline composition.Type: GrantFiled: January 11, 2019Date of Patent: April 13, 2021Assignee: SLT TECHNOLOGIES, INC.Inventors: Mark Philip D'Evelyn, Kristi Jean Narang, Dong-Sil Park, Huicong Hong, Xian-An Cao, Larry Qiang Zeng
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Patent number: 10940104Abstract: To provide an oil in water type solid cosmetic composition which can be solidified into a stable solid shape, has a desired sensation of elasticity, has favorable take up properties when taken up with a finger, and imparts a superior sensation of freshness when utilized, as an oil in water type preparation. An oil in water type solid cosmetic includes: (a) 0.1 to 5% by mass of a hydrophobically modified polyether urethane; (b) 0.01 to 5% by mass of a hydrophilic plate shaped powder; (c) a hydrophobic powder; (d) an oil component; and (e) water.Type: GrantFiled: April 27, 2017Date of Patent: March 9, 2021Assignee: SHISEIDO COMPANY, LTD.Inventor: Shun Kubota
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Patent number: 10461214Abstract: To provide a method for producing a Group III nitride semiconductor light-emitting device using a substrate containing Al such as AlN substrate while suppressing polarity inversion. The production method comprising an oxide film formation step, a first Group III nitride layer formation step, a first semiconductor layer formation step, a light-emitting layer formation step, and a second semiconductor layer formation step. In the production method, an AlN substrate or AlGaN substrate is employed. In the oxide film formation step, an oxide film containing Al atoms, N atoms, and O atoms is formed. In the first Group III nitride layer formation step, an AlN layer or AlGaN layer is formed as the first Group III nitride layer under the condition that the substrate temperature 1200° C. to 1450° C.Type: GrantFiled: December 19, 2017Date of Patent: October 29, 2019Assignee: TOYODA GOSEI CO., LTD.Inventors: Yoshiki Saito, Daisuke Shinoda
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Patent number: 10358739Abstract: A method of synthesizing zinc selenide crystals. The method includes forming an aqueous growth medium by combining a mineralizer solution of an alkali nutrient with a feedstock including zinc and selenium. A seed crystal is added to the growth medium. The aqueous growth medium and seed crystal are pressurized and a thermal gradient applied such that a temperature of a first portion of the aqueous growth medium is greater than a second portion of the aqueous growth medium. The zinc and selenium are dissolved into the mineralizer solution from the feedstock in the first portion of the aqueous growth medium and spontaneously forms at least one single crystal of zinc selenide on the seed crystal in the first portion of the aqueous growth medium.Type: GrantFiled: October 26, 2017Date of Patent: July 23, 2019Inventors: James Matthew Mann, Martin M. Kimani, Eric Michael Hunt, Michael R. Snure
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Patent number: 10293318Abstract: A pressure release mechanism for use with a capsule for processing materials or growing crystals in supercritical fluids is disclosed. The capsule with the pressure release mechanism is scalable up to very large volumes and is cost effective according to a preferred embodiment. In conjunction with suitable high pressure apparatus, the capsule with pressure release mechanism is capable of processing materials at pressures and temperatures of 20-2000 MPa and 25-1500° C., respectively. Of course, there can be other variations, modifications, and alternatives.Type: GrantFiled: September 19, 2016Date of Patent: May 21, 2019Assignee: SLT TECHNOLOGIES, INC.Inventors: Mark Philip D'Evelyn, Rajeev Tirumala Pakalapati
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Patent number: 10156214Abstract: An intake manifold provided in an internal combustion engine to be mounted in a vehicle includes: a plurality of intake-air branch pipes; an EGR chamber configured such that EGR gas is introduced into the EGR chamber; and a plurality of EGR ports communicating the plurality of intake-air branch pipes with the EGR chamber. A chamber bottom face is provided with a plurality of recessed zones so as to correspond to the plurality of EGR ports, each of the plurality of recessed zones is provided near an opening of its corresponding EGR port on an EGR-chamber side, and all planes constituting the each of the plurality of recessed zones is configured to be inclined so as to be placed on a mounting lower side toward a position closer to the opening, as compared with a position away from the opening.Type: GrantFiled: June 29, 2017Date of Patent: December 18, 2018Assignee: TOYOTA JIDOSHA KABUSHIKI KAISHAInventor: Yasunori Kanzaki
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Patent number: 10047456Abstract: A monolithic crystal having the atomic formula WnXmYpZr, with at least one dimension greater than about 10 mm. A method for top seed, solution growth of a monolithic crystal, wherein the method includes the steps of: preparing a precursor, forming a seed crystal, and forming the monolithic crystal. Some configurations of the method include the differential control of the crystal flux temperature in a furnace and the rotational frequency of a seed crystal in the crystal flux.Type: GrantFiled: May 20, 2015Date of Patent: August 14, 2018Assignee: UNIVERSITY OF HOUSTON SYSTEMInventors: P. Shiv Halasyamani, Weiguo Zhang
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Patent number: 9909230Abstract: In one instance, the invention provides a method of growing bulk crystal of group III nitride using a seed crystal selected by (a) measuring x-ray rocking curves of a seed crystal at more than one point, (b) quantifying the peak widths of the measured x-ray rocking curves, and (c) evaluating the distribution of the quantified peak widths. The invention also includes the method of selecting a seed crystal for growing bulk crystal of group III nitride. The bulk crystal of group III nitride can be grown in supercritical ammonia or a melt of group III metal using at least one seed selected by the method above.Type: GrantFiled: January 22, 2016Date of Patent: March 6, 2018Assignee: SixPoint Materials, Inc.Inventors: Tadao Hashimoto, Edward Letts, Daryl Key
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Patent number: 9724666Abstract: An apparatus to contain the reaction vessel in which gallium nitride crystals (henceforth referred to as bulk crystals) can be grown using the ammonothermal method at high pressure and temperature is disclosed. The apparatus provides adequate containment in all directions, which, for a typical cylindrical vessel, can be classified as radial and axial. Furthermore, depending on the specifics of the design parameters, the apparatus is capable of operating at a temperature up to 1,200 degrees Celsius, a pressure up to 2,000 MPa, and for whatever length of time is necessary to grow satisfactory bulk crystals. The radial constraint in the current disclosure is provided by using several stacked composite rings. The design of the apparatus is scalable to contain reaction volumes larger than 100 cubic centimeters.Type: GrantFiled: October 19, 2012Date of Patent: August 8, 2017Assignee: Soraa, Inc.Inventors: Pakalapati Tirumala Rajeev, Douglas W. Pocius, Mark P. D'Evelyn
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Publication number: 20150132926Abstract: Large-scale manufacturing of gallium nitride boules using m-plane or wedge-shaped seed crystals can be accomplished using ammonothermal growth methods. Large-area single crystal seed plates are suspended in a rack, placed in a large diameter autoclave or internally-heated high pressure apparatus along with ammonia and a mineralizer, and crystals are grown ammonothermally. The orientation of the m-plane or wedge-shaped seed crystals are chosen to provide efficient utilization of the seed plates and of the volume inside the autoclave or high pressure apparatus.Type: ApplicationFiled: January 16, 2015Publication date: May 14, 2015Inventors: MARK P. D'EVELYN, DIRK EHRENTRAUT, DERRICK S. KAMBER, BRADLEY C. DOWNEY
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Publication number: 20150122172Abstract: An apparatus for processing materials at high temperatures comprises a high strength enclosure; a plurality of high strength radial segments disposed adjacent to and radially inward from the high strength enclosure; a liner disposed adjacent to and radially inward from the radical segments; a chamber defined interior to the liner; a heating device disposed within the chamber; and a capsule disposed within the chamber, the capsule configured to hold a supercritical fluid. The apparatus may be used for growing crystals, e.g., GaN, under high temperature and pressure conditions.Type: ApplicationFiled: July 28, 2011Publication date: May 7, 2015Applicant: MOMENTIVE PERFORMANCE MATERIALS, INC.Inventors: Kirsh Afimiwala, Larry Zeng
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Method of growing GaN whiskers from a gallium-containing solvent at low pressure and low temperature
Patent number: 8999060Abstract: Millimeter-scale GaN single crystals in filamentary form, also known as GaN whiskers, grown from solution and a process for preparing the same at moderate temperatures and near atmospheric pressures are provided. GaN whiskers can be grown from a GaN source in a reaction vessel subjected to a temperature gradient at nitrogen pressure. The GaN source can be formed in situ as part of an exchange reaction or can be preexisting GaN material. The GaN source is dissolved in a solvent and precipitates out of the solution as millimeter-scale single crystal filaments as a result of the applied temperature gradient.Type: GrantFiled: March 12, 2013Date of Patent: April 7, 2015Assignee: The United States of America, as represented by the Secretary of the NavyInventors: Boris N. Feigelson, Jennifer K. Hite, Francis J. Kub, Charles R. Eddy, Jr. -
Patent number: 8979999Abstract: A method for large-scale manufacturing of gallium nitride boules. Large-area single crystal seed plates are suspended in a rack, placed in a large diameter autoclave or internally-heated high pressure apparatus along with ammonia and a mineralizer, and grown ammonothermally. The seed orientation and mounting geometry are chosen to provide efficient utilization of the seed plates and of the volume inside the autoclave or high pressure apparatus. The method is scalable up to very large volumes and is cost effective.Type: GrantFiled: August 3, 2009Date of Patent: March 17, 2015Assignee: Soraa, Inc.Inventor: Mark P. D'Evelyn
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Publication number: 20150034150Abstract: The invention provides a process for producing a mesoporous single crystal of a semiconductor, wherein the shortest external dimension of said single crystal, measured along any of the crystallographic principal axes of said single crystal, is x, wherein x is equal to or greater than 50 nm, which process comprises growing a single crystal of a semiconductor within a mesoporous template material until said shortest external dimension of the single crystal is equal to or greater than x. Further provided is a mesoporous single crystal obtainable by the process of the invention. The invention also provides a mesoporous single crystal of a semiconductor, wherein the shortest external dimension of said single crystal measured along any of the principal axes of said single crystal is equal to or greater than 50 nm. Further provided is a composition comprising a plurality of mesoporous single crystals of the invention. The invention also provides a semiconducting layer of a mesoporous single crystal of the invention.Type: ApplicationFiled: March 1, 2013Publication date: February 5, 2015Inventors: Henry James Snaith, Edward James Crossland
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Publication number: 20150023862Abstract: A first object of the present invention is to provide a method for efficiently growing a nitride single crystal even under low pressure conditions. The present invention relates to a method for producing a nitride single crystal, comprising growing a nitride crystal on the surface of a seed crystal having a hexagonal crystal structure by setting a pressure in a reaction vessel having the seed crystal, a nitrogen-containing solvent, a mineralizer containing a fluorine atom, and a raw material placed therein to 5 to 200 MPa and performing control so that the nitrogen-containing solvent is in at least either a supercritical state or a subcritical state.Type: ApplicationFiled: September 29, 2014Publication date: January 22, 2015Applicants: Mitsubishi Chemical Corporation, Tohoku University, The Japan Steel Works, Ltd.Inventors: Toru ISHIGURO, Quanxi BAO, Chiaki YOKOYAMA, Daisuke TOMIDA, Shigefusa CHICHIBU, Rinzo KAYANO, Mutsuo UEDA, Makoto SAITO, Yuji KAGAMITANI
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Patent number: 8916124Abstract: When a group III nitride crystal is grown in a pressurized atmosphere of a nitrogen-containing gas from a melt 50 including at least a group III element, nitrogen and an alkali metal or an alkali earth metal, a melt-holding vessel 160 that holds the above-described melt 50 is swung about two axes different in direction from each other such as an X-axis and a Y-axis.Type: GrantFiled: November 27, 2008Date of Patent: December 23, 2014Assignee: Ricoh Company, Ltd.Inventors: Hisashi Minemoto, Osamu Yamada, Takeshi Hatakeyama, Hiroaki Hoshikawa, Yasunori Tokunou
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Publication number: 20140360938Abstract: A zeolite membrane composite for use in separation of a highly-permeative component through permeation from a vapor mixture or a liquid mixture comprising multiple components, the zeolite membrane composite comprising an inorganic porous support and a zeolite membrane provided thereon, wherein the zeolite membrane contains zeolite of a CHA-type aluminosilicate, and in a X-ray diffraction pattern obtained through irradiation to the zeolite membrane surface with X-ray, a peak intensity at around 2?=17.9° has a value of less than 0.5 times a peak intensity at around 2?=20.8° and a peak intensity at around 2?=9.6° has a value of 2.0 times or more and less than 4.0 times a peak intensity at around 2?=20.8°.Type: ApplicationFiled: August 25, 2014Publication date: December 11, 2014Applicant: MITSUBISHI CHEMICAL CORPORATIONInventors: Mikio Hayashi, Miki Yamada, Takahiko Takewaki
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Publication number: 20140360939Abstract: A porous support-zeolite membrane composite comprising an inorganic porous support and a zeolite membrane provided on, wherein the zeolite membrane contains a zeolite having a microporous structure of 8-membered oxygen ring or less, and a molar ratio of SiO2/Al2O3 in the zeolite membrane surface is larger by at least 20 than a molar ratio of SiO2/Al2O3 in the zeolite membrane itself, or a water adsorption of the porous support-zeolite membrane composite at a relative pressure of 0.8, as determined from a water vapor adsorption isotherm of the porous support-zeolite membrane composite, is at least 82% of a water adsorption of the porous support-zeolite membrane composite under the same condition as above after one-week immersion of the porous support-zeolite membrane composite in an aqueous 90 mass % acetic acid solution at room temperature.Type: ApplicationFiled: August 25, 2014Publication date: December 11, 2014Applicant: MITSUBISHI CHEMICAL CORPORATIONInventors: MIKI YAMADA, Takahiko Takewaki, Mikio Hayashi, Naoko Fujita, Hidekazu Miyagi
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Publication number: 20140346976Abstract: The present invention relates to a method for manufacturing a plurality of nanostructures comprising the steps of providing a plurality of protruding base structures (104) arranged on a surface of a first substrate (102), providing a seed layer mixture, comprising a solvent/dispersant and a seed material, in contact with the protruding base structures, providing a second substrate arranged in parallel with the first substrate adjacent to the protruding base structures, thereby enclosing a majority of the seed layer mixture between the first and second substrates, evaporating the solvent, thereby forming a seed layer (110) comprising the seed material on the protruding base structures, removing the second substrate, providing a growth mixture, comprising a growth agent, in contact with the seed layer, and controlling the temperature of the growth mixture so that nanostructures (114) are formed on the seed layer via chemical reaction in presence of the growth agent.Type: ApplicationFiled: October 5, 2012Publication date: November 27, 2014Inventors: Qiu-Hong Hu, Shang-Ray Yang, Kjell Bohlin
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Publication number: 20140326175Abstract: The present disclosure proves for new design of reactors used for ammonothermal growth of III nitride crystals. The reactors include a region intermediate a source dissolution region and a crystal growth region configured to provide growth of high quality crystals at rates greater than 100 ?m/day. In one embodiment, multiple baffle plates having openings whose location is designed so that there is no direct path through the intermediate region, or with multiple baffle plates having differently sized openings on each plate so that the flow is slowed down and/or exhibit greater mixing are described. The disclosed designs enable obtaining high temperature difference between the dissolution region and the crystallization region without decreasing conductance through the device.Type: ApplicationFiled: July 14, 2014Publication date: November 6, 2014Applicant: SixPoint Materials, Inc.Inventors: Tadao HASHIMOTO, Masonari IKARI, Edward LETTS
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Publication number: 20140302664Abstract: Preparation of semiconductor nanocrystals and their dispersions in solvents and other media is described. The nanocrystals described herein have small (1-10 nm) particle size with minimal aggregation and can be synthesized with high yield. The capping agents on the as-synthesized nanocrystals as well as nanocrystals which have undergone cap exchange reactions result in the formation of stable suspensions in polar and nonpolar solvents which may then result in the formation of high quality nanocomposite films.Type: ApplicationFiled: June 20, 2014Publication date: October 9, 2014Applicant: PIXELLIGENT TECHNOLOGIES, LLCInventors: Zehra Serpil GONEN WILLIAMS, Yijun Wang, Robert J. Wiaceck, Xia Bai, Linfeng Gou, Selina I. Thomas, Wei Xu, Jun Xu, Rakesh Patel
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Publication number: 20140295649Abstract: Preparation of semiconductor nanocrystals and their dispersions in solvents and other media is described. The nanocrystals described herein have small (1-10 nm) particle size with minimal aggregation and can be synthesized with high yield. The capping agents on the as-synthesized nanocrystals as well as nanocrystals which have undergone cap exchange reactions result in the formation of stable suspensions in polar and nonpolar solvents which may then result in the formation of high quality nanocomposite films.Type: ApplicationFiled: June 20, 2014Publication date: October 2, 2014Applicant: PIXELLIGENT TECHNOLOGIES, LLCInventors: Zehra Serpil GONEN WILLIAMS, Yijun Wang, Robert J. Wiacek, Xia Bai, Linfeng Gou, Selina I. Thomas, Wei Xu, Jun Xu, Rakesh Patel
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Publication number: 20140251202Abstract: This invention relates to synthetically derived zinc phlogopite substrates, of superior aspect ratio, effect pigments comprising such synthetically derived substrates and methods of forming said substrates. More specifically the disclosure describes an improved hydrothermal synthesis of zinc phlogopite suitable as a substrate for interference pigments, barrier and flame retardant applications.Type: ApplicationFiled: March 11, 2014Publication date: September 11, 2014Inventors: Meaghan Clark McGuire, Ivor Bull, Geoffrey Mark Johnson, Enzo Cordola
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Publication number: 20140219907Abstract: Single-crystal diamond is composed of carbon in which a concentration of a carbon isotope 12C is not lower than 99.9 mass % and a plurality of inevitable impurities other than carbon. The inevitable impurities include nitrogen, boron, hydrogen, and nickel, and a total content of nitrogen, boron, and hydrogen of the plurality of inevitable impurities is not higher than 0.01 mass %. In order to manufacture single-crystal diamond, initially, a hydrocarbon gas in which a concentration of the carbon isotope 12C is not lower than 99.9 mass % is subjected to denitrification.Type: ApplicationFiled: August 30, 2012Publication date: August 7, 2014Applicant: SUMITOMO ELECTRIC INDUSTRIES, LTD.Inventors: Kazuhiro Ikeda, Hitoshi Sumiya
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Publication number: 20140209012Abstract: Provided is a base substrate with which a Group-III nitride crystal having a large area and a large thickness can be grown while inhibiting crack generation. A single-crystal substrate for use in growing a Group-III nitride crystal thereon, which satisfies the following expression (1), wherein Z1 (?m) is an amount of warpage of physical shape in a growth surface of the single-crystal substrate and Z2 (?m) is an amount of warpage calculated from a radius of curvature of crystallographic-plane shape in a growth surface of the single-crystal substrate: ?40<Z2/Z1<?1: Expression (1).Type: ApplicationFiled: March 28, 2014Publication date: July 31, 2014Applicant: MITSUBISHI CHEMICAL CORPORATIONInventors: Kenji FUJITO, Yasuhiro Uchiyama
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Publication number: 20140205840Abstract: There is provided a novel method for producing a nitride single crystal with both a rapid crystal growth rate and high crystal quality, as well as a novel autoclave that can be used in the method. The invention provides a method for producing a Ga-containing nitride single crystal by an ammonothermal method, comprising introducing at least a starting material, an acidic mineralizer and ammonia into an autoclave, and then growing a Ga-containing nitride single crystal under conditions wherein the temperature (T1) at the single crystal growth site is 600° C. to 850° C., the temperature (T1) at the single crystal growth site and the temperature (T2) at the starting material feeder site are in the relationship T1>T2, and the pressure in the autoclave is 40 MPa to 250 MPa, as well as an autoclave that can be used in the method.Type: ApplicationFiled: June 23, 2011Publication date: July 24, 2014Applicants: TOHOKU UNIVERSITY, ASAHI KASEI KABUSHIKI KAISHAInventors: Kensuke Aoki, Kazuo Yoshida, Katsuhito Nakamura, Tsuguo Fukuda
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Publication number: 20140174340Abstract: The present invention discloses methods to create higher quality group III-nitride wafers that then generate improvements in the crystalline properties of ingots produced by ammonothermal growth from an initial defective seed. By obtaining future seeds from carefully chosen regions of an ingot produced on a bowed seed crystal, future ingot crystalline properties can be improved. Specifically the future seeds are optimized if chosen from an area of relieved stress, on a cracked ingot or from a carefully chosen N-polar compressed area. When the seeds are sliced out, miscut of 3-10° helps to itnprove structural quality of successive growth. Additionally a method is proposed to improve crystal quality by using the ammonothermal method to produce a series of ingots, each using a specifically oriented seed from the previous ingot. When employed, these methods enhance the quality of Group III nitride wafers and thus improve the efficiency of any subsequent device.Type: ApplicationFiled: February 27, 2014Publication date: June 26, 2014Applicant: SIXPOINT MATERIALS, INC.Inventors: Edward LETTS, Tadao HASHIMOTO, Masanori IKARI
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Patent number: 8728622Abstract: Provided is a base substrate with which a Group-III nitride crystal having a large area and a large thickness can be grown while inhibiting crack generation. A single-crystal substrate for use in growing a Group-III nitride crystal thereon, which satisfies the following expression (1), wherein Z1 (?m) is an amount of warpage of physical shape in a growth surface of the single-crystal substrate and Z2 (?m) is an amount of warpage calculated from a radius of curvature of crystallographic-plane shape in a growth surface of the single-crystal substrate: ?40<Z2/Z1<?1: Expression (1).Type: GrantFiled: July 13, 2012Date of Patent: May 20, 2014Assignee: Mitsubishi Chemical CorporationInventors: Kenji Fujito, Yasuhiro Uchiyama
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Patent number: 8729672Abstract: To grow a gallium nitride crystal, a seed-crystal substrate is first immersed in a melt mixture containing gallium and sodium. Then, a gallium nitride crystal is grown on the seed-crystal substrate under heating the melt mixture in a pressurized atmosphere containing nitrogen gas and not containing oxygen. At this time, the gallium nitride crystal is grown on the seed-crystal substrate under a first stirring condition of stirring the melt mixture, the first stirring condition being set for providing a rough growth surface, and the gallium nitride crystal is subsequently grown on the seed-crystal substrate under a second stirring condition of stirring the melt mixture, the second stirring condition being set for providing a smooth growth surface.Type: GrantFiled: April 12, 2013Date of Patent: May 20, 2014Assignee: NGK Insulators, Ltd.Inventors: Takanao Shimodaira, Takayuki Hirao, Katsuhiro Imai
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Publication number: 20140116326Abstract: Reactor designs for use in ammonothermal growth of group-III nitride crystals. Internal heating is used to enhance and/or engineer fluid motion, gas mixing, and the ability to create solubility gradients within a vessel used for the ammonothermal growth of group-III nitride crystals. Novel baffle designs are used for control and improvement of continuous fluid motion within a vessel used for the ammonothermal growth of group-III nitride crystals.Type: ApplicationFiled: January 7, 2014Publication date: May 1, 2014Applicant: THE REGENTS OF THE UNIVERSITY OF CALIFORNIAInventors: Siddha Pimputkar, Derrick Shane Kamber, James S. Speck, Shuji Nakamura
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Publication number: 20140087209Abstract: The present invention provides a method of growing an ingot of group III nitride. Group III nitride crystals such as GaN are grown by the ammonothermal method on both sides of a seed to form an ingot and the ingot is sliced into wafers. The wafer including the first-generation seed is sliced thicker than the other wafers so that the wafer including the first-generation seed does not break. The wafer including the first-generation seed crystal can be used as a seed for the next ammonothermal growth.Type: ApplicationFiled: March 15, 2013Publication date: March 27, 2014Applicants: Seoul Semiconductor Co., Ltd., SixPoint Materials, Inc.Inventors: Tadao Hashimoto, Edward Letts, Sierra Hoff
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Publication number: 20140087113Abstract: The present invention provides a method of growing an ingot of group III nitride. Group III nitride crystals such as GaN are grown by the ammonothermal method on both sides of a seed to form an ingot and the ingot is sliced into wafers. The wafer including the first-generation seed is sliced thicker than the other wafers so that the wafer including the first-generation seed does not break. The wafer including the first-generation seed crystal can be used as a seed for the next ammonothermal growth.Type: ApplicationFiled: March 15, 2013Publication date: March 27, 2014Applicants: Seoul Semiconductor Co., Ltd., SixPoint Materials, Inc.Inventors: Tadao Hashimoto, Edward Letts, Sierra Hoff
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Patent number: 8679443Abstract: A method of treating a diamond, the method comprising: (i) providing a liquid metal saturated with carbon with respect to graphite precipitation; (ii) lowering the temperature of the liquid metal such that the liquid metal is saturated with carbon with respect to diamond precipitation; (iii) immersing a diamond in the liquid metal; and (iv) removing the diamond from the metal.Type: GrantFiled: July 19, 2010Date of Patent: March 25, 2014Assignee: Designed Materials LtdInventors: Philip H. Taylor, A. Marshall Stoneham
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Publication number: 20140054589Abstract: The present invention discloses a semi-insulating wafer of GaxAlyIn1-x-yN (0?x?1, 0?x+y?1) which is doped with bismuth (Bi). The semi-insulating wafer has the resistivity of 104 ohm-cm or more. Although it is very difficult to obtain a single crystal ingot of group III nitride, the ammonothermal method can grow highly-oriented poly or single crystal ingot of group III nitride having the density of dislocations/grain boundaries less than 105 cm?2. The invention also disclose the method of fabricating the semi-insulating group III nitride bulk crystals and wafers.Type: ApplicationFiled: February 28, 2013Publication date: February 27, 2014Applicants: Seoul Semiconductor Co., Ltd., SixPoint Materials, Inc.Inventors: Tadao HASHIMOTO, Edward LETTS, Sierra HOFF
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Publication number: 20140050646Abstract: B3NO3 of the present invention has a rock salt type crystal structure to thereby have a bulk modulus higher than that of c-BN.Type: ApplicationFiled: August 15, 2012Publication date: February 20, 2014Applicant: Sumitomo Electric Industries, Ltd.Inventor: Akitaka SAWAMURA
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Publication number: 20130344277Abstract: Single crystals are described that contain several regimes within the crystal that perform different functions related to the enhanced performance of a laser gain medium. At least one regime of the single crystals can be utilized to suppress amplified spontaneous emission and parasitic oscillation in a laser gain medium. A single crystal can include core and cladding regions, the cladding region providing amplified spontaneous emission suppression. The core region of the crystal can include as dopant one or more ions that take part in the lasing when suitably pumped. The amplified spontaneous emission suppression region can include as dopant one or more ions that can prevent additional spontaneous emission that can to depletion of the upper laser states, thus reducing laser performance including one or more ions that absorb spontaneously emitted photons and/or a higher concentration of the active lasing ions of the core.Type: ApplicationFiled: June 21, 2013Publication date: December 26, 2013Inventors: Joseph Kolis, Colin McMillen
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Publication number: 20130343715Abstract: Single heterogeneous crystals are described that contain multiple regimes, adjacent regimes varying from one another with regard to function. Also disclosed is a hydrothermal epitaxial growth process that can be utilized to form the single heterogeneous crystals. The single heterogeneous crystals can exhibit enhanced performance when used as a laser gain medium as compared to previously known single crystals and multi-crystal constructs. The heterogeneous single crystal can be utilized for thin disk lasers and can minimize the thermal distortion effects at high powers. The heterogeneous crystal can also serve as an embedded waveguide.Type: ApplicationFiled: June 21, 2013Publication date: December 26, 2013Inventors: Joseph Kolis, Colin McMillen
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Patent number: 8609059Abstract: To provide a production method for a nitride crystal, where a nitride crystal can be prevented from precipitating in a portion other than on a seed crystal and the production efficiency of a gallium nitride single crystal grown on the seed crystal can be enhanced. In a method for producing a nitride crystal by an ammonothermal method in a vessel containing a mineralizer-containing solution, out of the surfaces of said vessel and a member provided in said vessel, at least a part of the portion coming into contact with said solution is constituted by a metal or alloy containing one or more atoms selected from the group consisting of tantalum (Ta), tungsten (W) and titanium (Ti), and has a surface roughness (Ra) of less than 1.80 ?m.Type: GrantFiled: May 29, 2012Date of Patent: December 17, 2013Assignees: Mitsubishi Chemical Corporation, Tohoku University, The Japan Steel Works, Ltd.Inventors: Yutaka Mikawa, Makiko Kiyomi, Yuji Kagamitani, Toru Ishiguro, Yoshihiko Yamamura
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Patent number: 8603242Abstract: One embodiment of the present invention is a method for producing a silicon (Si) and/or germanium (Ge) foil, the method including: dissolving a Si and/or Ge source material in a molten metallic bath at an elevated temperature T2, wherein the density of Si and/or Ge is smaller than the density of the molten metallic bath; cooling the molten metallic bath to a lower temperature T1, thereby causing Si and/or Ge to separate out of the molten metallic bath and to float and grow as a Si and/or Ge foil on a top surface of the molten metallic bath; and separating the floating Si and/or Ge foil from the top surface of the molten metallic bath.Type: GrantFiled: February 25, 2010Date of Patent: December 10, 2013Inventors: Uri Cohen, Michael Roitberg
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Patent number: 8574532Abstract: A semiconductor crystal is produced through crystal growth in the presence of a solvent in a supercritical and/or subcritical state in a reactor, wherein at least a part of the surface of the reactor and the surface of the member to be used inside the reactor is coated with a platinum group-Group 13 metal alloy coating film.Type: GrantFiled: December 27, 2011Date of Patent: November 5, 2013Assignee: Mitsubishi Chemical CorporationInventors: Hideo Fujisawa, Yutaka Mikawa
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Patent number: 8574525Abstract: Boron-containing compounds, gasses and fluids are used during ammonothermal growth of group-Ill nitride crystals. Boron-containing compounds are used as impurity getters during the ammonothermal growth of group-Ill nitride crystals. In addition, a boron-containing gas and/or supercritical fluid is used for enhanced solubility of group-Ill nitride into said fluid.Type: GrantFiled: November 4, 2009Date of Patent: November 5, 2013Assignee: The Regents of the University of CaliforniaInventors: Siddha Pimputkar, Derrick S. Kamber, James S. Speck, Shuji Nakamura
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Publication number: 20130263775Abstract: A method and apparatus for growing crystals in a reactor vessel, wherein the reactor vessel uses carbon fiber containing materials as a structural element to contain the materials for growing the crystals as a solid, liquid or gas within the reactor vessel, such that the reactor vessel can withstand pressures or temperatures necessary for the growth of the crystals. The carbon fiber containing materials encapsulate at least one component of the reactor vessel, wherein stresses from the encapsulated component are transferred to the carbon fiber containing materials. The carbon fiber containing materials may be wrapped around the encapsulated component one or more times sufficient to maintain a desired pressure differential between an exterior and interior of the encapsulated component.Type: ApplicationFiled: April 10, 2013Publication date: October 10, 2013Applicant: The Regents of the University of CaliforniaInventors: Siddha Pimputkar, Paul Von Dollen, Shuji Nakamura, James S. Speck
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Publication number: 20130221279Abstract: Preparation of semiconductor nanocrystals and their dispersions in solvents and other media is described. The nanocrystals described herein have small (1-10 nm) particle size with minimal aggregation and can be synthesized with high yield. The capping agents on the as-synthesized nanocrystals as well as nanocrystals which have undergone cap exchange reactions result in the formation of stable suspensions in polar and nonpolar solvents which may then result in the formation of high quality nanocomposite films.Type: ApplicationFiled: October 26, 2011Publication date: August 29, 2013Applicant: PIXELLIGENT TECHNOLOGIES, LLCInventors: Wei Xu, Zehra Serpil Gonen Williams, Yijun Wang, Robert J. Wiacek, Xia Bai, Linfeng Gou, Selina L. Thomas, Jun Xu
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Publication number: 20130206057Abstract: Present invention discloses a high-pressure vessel of large size formed with a limited size of e.g. Ni—Cr based precipitation hardenable superalloy. Vessel may have multiple zones. For instance, the high-pressure vessel may be divided into at least three regions with flow-restricting devices and the crystallization region is set higher temperature than other regions. This structure helps to reliably seal both ends of the high-pressure vessel, at the same time, may help to greatly reduce unfavorable precipitation of group III nitride at the bottom of the vessel. Invention also discloses novel procedures to grow crystals with improved purity, transparency and structural quality. Alkali metal-containing mineralizers are charged with minimum exposure to oxygen and moisture until the high-pressure vessel is filled with ammonia. Several methods to reduce oxygen contamination during the process steps are presented.Type: ApplicationFiled: March 4, 2013Publication date: August 15, 2013Applicant: SIXPOINT MATERIALS, INC.Inventor: SIXPOINT MATERIALS, INC.
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Publication number: 20130207053Abstract: Preparation of semiconductor nanocrystals and their dispersions in solvents and other media is described. The nanocrystals described herein have small (1-10 nm) particle size with minimal aggregation and can be synthesized with high yield. The capping agents on the as-synthesized nanocrystals as well as nanocrystals which have undergone cap exchange reactions result in the formation of stable suspensions in polar and nonpolar solvents which may then result in the formation of high quality nanocomposite films.Type: ApplicationFiled: October 26, 2012Publication date: August 15, 2013Inventors: Zehra Serpil Gonen Williams, Yijun Wang, Robert J. Wiacek, Xia Bai, Linfeng Gou, Selina I. Thomas, Wei Xu, Jun Xu
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Patent number: 8449672Abstract: This disclosure pertains to a process for making single crystal Group III nitride, particularly gallium nitride, at low pressure and temperature, in the region of the phase diagram of Group III nitride where Group III nitride is thermodynamically stable comprises a charge in the reaction vessel of (a) Group III nitride material as a source, (b) a barrier of solvent interposed between said source of Group III nitride and the deposition site, the solvent being prepared from the lithium nitride (Li3N) combined with barium fluoride (BaF2), or lithium nitride combined with barium fluoride and lithium fluoride (LiF) composition, heating the solvent to render it molten, dissolution of the source of GaN material in the molten solvent and following precipitation of GaN single crystals either self seeded or on the seed, maintaining conditions and then precipitating out.Type: GrantFiled: April 25, 2008Date of Patent: May 28, 2013Assignee: The United States of America as represented by the Secretary of the NavyInventors: Boris N. Feigelson, Richard L. Henry
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Patent number: 8440017Abstract: To grow a gallium nitride crystal, a seed-crystal substrate is first immersed in a melt mixture containing gallium and sodium. Then, a gallium nitride crystal is grown on the seed-crystal substrate under heating the melt mixture in a pressurized atmosphere containing nitrogen gas and not containing oxygen. At this time, the gallium nitride crystal is grown on the seed-crystal substrate under a first stirring condition of stirring the melt mixture, the first stirring condition being set for providing a rough growth surface, and the gallium nitride crystal is subsequently grown on the seed-crystal substrate under a second stirring condition of stirring the melt mixture, the second stirring condition being set for providing a smooth growth surface.Type: GrantFiled: August 12, 2011Date of Patent: May 14, 2013Assignee: NGK Insulators, Ltd.Inventors: Takanao Shimodaira, Takayuki Hirao, Katsuhiro Imai
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Patent number: 8435347Abstract: A high pressure apparatus and related methods for processing supercritical fluids is described. The apparatus includes a capsule, a heater, at least one ceramic ring with one or more scribe marks and/or cracks present. The apparatus optionally has a metal sleeve containing each ceramic ring. The apparatus also has a high-strength enclosure, end flanges with associated insulation, and a power control system. The apparatus is capable of accessing pressures and temperatures of 0.2-2 GPa and 400-1200° C., respectively.Type: GrantFiled: September 27, 2010Date of Patent: May 7, 2013Assignees: Soraa, Inc., Elmhurst Research, Inc.Inventors: Mark P. D'Evelyn, Joseph A. Kapp, John C. Lawrenson
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Publication number: 20130108537Abstract: A high-quality nitride crystal can be produced efficiently by charging a nitride crystal starting material that contains tertiary particles having a maximum diameter of from 1 to 120 mm and formed through aggregation of secondary particles having a maximum diameter of from 100 to 1000 ?m, in the starting material charging region of a reactor, followed by crystal growth in the presence of a solvent in a supercritical state and/or a subcritical state in the reactor, wherein the nitride crystal starting material is charged in the starting material charging region in a bulk density of from 0.7 to 4.5 g/cm3 for the intended crystal growth.Type: ApplicationFiled: October 26, 2012Publication date: May 2, 2013Inventors: Yutaka MIKAWA, Hideo FUJISAWA, Kazunori KAMADA, Hirobumi NAGAOKA, Shinichiro KAWABATA, Yuji KAGAMITANI