Ternary Compound Patents (Class 423/285)
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Patent number: 9005562Abstract: A method of purifying ammonia borane is provided whereby crude ammonia borane is dissolved in a basic aqueous solution, the solution is heated to decompose and precipitate impurities found in the crude ammonia borane, and the impurities are separated by filtration. The aqueous solution containing dissolved ammonia borane is then cooled to a temperature of from 10° C. to ?10° C., to precipitate the ammonia borane, which is recovered and dried to yield a high-purity product.Type: GrantFiled: December 28, 2012Date of Patent: April 14, 2015Assignees: BoroScience International, Inc., WeylChem Sustainable Materials, LLCInventors: Bernard Franklin Spielvogel, Kevin Joel Drost
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Publication number: 20140186252Abstract: A method of purifying ammonia borane is provided whereby crude ammonia borane is dissolved in a basic aqueous solution, the solution is heated to decompose and precipitate impurities found in the crude ammonia borane, and the impurities are separated by filtration. The aqueous solution containing dissolved ammonia borane is then cooled to a temperature of from 10° C. to ?10° C., to precipitate the ammonia borane, which is recovered and dried to yield a high-purity product.Type: ApplicationFiled: December 28, 2012Publication date: July 3, 2014Applicants: WEYLCHEM SUSTAINABLE MATERIALS, LLC, BOROSCIENCE INTERNATIONAL, INC.Inventors: BoroScience International, Inc., WeyIChem Sustainable Materials, LLC
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Publication number: 20130225863Abstract: A method for synthesizing ammonia borane includes (a) preparing a reaction mixture in one or more solvents, the reaction mixture containing sodium borohydride, at least one ammonium salt, and ammonia; and (b) incubating the reaction mixture at temperatures between about 0° C. to about room temperature in an ambient air environment under conditions sufficient to form ammonia borane. Methods for synthesizing ethylenediamine bisborane, and methods for dehydrogenation of ethylenediamine bisborane are also described.Type: ApplicationFiled: July 6, 2011Publication date: August 29, 2013Applicant: PURDUE RESEARCH FOUNDATIONInventors: Padi Veeraraghavan Ramachandran, Pravin D. Gagare, Hitesh Mistry, Bidyut Biswas
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Publication number: 20130121905Abstract: The present invention relates to a method for obtaining borazane, said method being suitable for obtaining borazane containing a low level of impurities. The borazane (obtained by reaction of at least one ammonium salt with at least one alkali and/or alkaline earth metal borohydride) in solution in THF is selectively precipitated with a non-solvent. The precipitated borazane can further be purified by selective dissolution. The borazane obtained after selective precipitation and dissolution contains less than 1% by weight of impurities and/or does not exhibit exothermic decomposition in the solid state with a temperature range of the endothermic melting peak above 110° C.Type: ApplicationFiled: May 20, 2011Publication date: May 16, 2013Applicant: HERAKLESInventors: Jean-Philippe Goudon, Joël Renouard
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Patent number: 8367027Abstract: Method of producing ammonia borane, comprising providing a reagent comprising a dehydrogenated material in a suitable solvent; and combining the reagent with a reducing agent comprising hydrazine, a hydrazine derivative, or combinations thereof, in a reaction which produces a mixture comprising ammonia borane.Type: GrantFiled: April 19, 2010Date of Patent: February 5, 2013Assignee: Los Alamos National Security, LLCInventors: Andrew Sutton, John C. Gordon, Kevin C. Ott, Anthony K Burrell
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Patent number: 8329130Abstract: The present invention provides a method for synthesis of crystalline polymeric boron-nitrogen compounds comprising a step of dehydrogenation of a boron-nitrogen-hydrogen compound on catalyst, wherein the boron-nitrogen-hydrogen compound is selected from the group consisting of ammonia borane, metal amidoboranes, amine boranes or mixtures thereof, and the catalyst is selected from the group consisting of transition metals, transition metal salts or alloys.Type: GrantFiled: July 20, 2010Date of Patent: December 11, 2012Assignee: Dalian Institute of Chemical Physics, Chinese Academy of SciencesInventors: Ping Chen, Teng He, Zhitao Xiong, Guotao Wu
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Publication number: 20120273733Abstract: A plasma treatment has been used to modify the surface of BNNTs. In one example, the surface of the BNNT has been modified using ammonia plasma to include amine functional groups. Amine functionalization allows BNNTs to be soluble in chloroform, which had not been possible previously. Further functionalization of amine-functionalized BNNTs with thiol-terminated organic molecules has also been demonstrated. Gold nanoparticles have been self-assembled at the surface of both amine- and thiol-functionalized boron nitride Nanotubes (BNNTs) in solution. This approach constitutes a basis for the preparation of highly functionalized BNNTs and for their utilization as nanoscale templates for assembly and integration with other nanoscale materials.Type: ApplicationFiled: June 19, 2012Publication date: November 1, 2012Applicant: The Regents of the University of CaliforniaInventors: Toby Sainsbury, Takashi Ikuno, Alexander K. Zettl
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Patent number: 8206673Abstract: A method of preparing a boron-nitrogen compound includes combining an ammonium salt and an ionic compound in the absence of solvent to form a mixture. The ionic compound includes a cation and an anion. The anion is represented by the general formula B(R1)4?, wherein each R1 is independently selected from the group of hydrogen, alkyl groups, aryl groups, and combinations thereof. The method also includes agitating the mixture in the absence of solvent to form a reaction product, and separating the boron-nitrogen compound from the reaction product.Type: GrantFiled: September 15, 2010Date of Patent: June 26, 2012Assignee: Wildcat Discovery TechnologiesInventors: Steven Kaye, Conor Riley
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Patent number: 8168342Abstract: A method of producing NH2(R2), the method comprising reacting a metal hydride with a compound having the general formula: M1X(BH4)y(NH2(R2))n wherein M1 comprises one or more of Li, Na, K, Rb, Cs, Be, Mg, Ca, Sr, Ba, La, Al, Ga and Sc; 0<n?4; R2 comprises —H, alkyl and an aromatic substituent; and x and y are selected so as to maintain electroneutrality.Type: GrantFiled: July 9, 2007Date of Patent: May 1, 2012Assignee: The Science and Technology Facilities CouncilInventors: Martin Owen Jones, Simon R. Johnson, Peter P. Edwards, William I. f David
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Publication number: 20120014857Abstract: Methods of synthesizing ammonia borane are provided. The methods comprise reacting at least one amine borane with ammonia such that ammonia borane is produced. Ammonia borane has a chemical formula of NH3.BH3 and provides a good source of storage hydrogen making it useful in a variety of applications including a potential hydrogen source for fuel cells. The methods can further comprise separating the ammonia borane from the other products of the reaction. Exemplary methods can produce ammonia borane having purity greater than about 90 percent. In further examples, the methods can produce ammonia borane having purity greater than about 95 percent or greater than about 99 percent.Type: ApplicationFiled: June 13, 2011Publication date: January 19, 2012Applicant: THE OHIO STATE UNIVERSITYInventors: Sheldon Gerald Shore, Xuenian Chen
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Patent number: 8038980Abstract: According to at least one aspect of the present invention, an ammonia borane containing hydrogen storage material is provided to be present with substantially reduced formation of borazine or diborane. In at least one embodiment, the hydrogen storage material includes at least one ammonia borane (NH3BH3); and at least one amide of the formula M(NH2)x, wherein M is a cationic element or a combination of two or more cationic elements from groups 1 to 14 of the periodic table and x represents a total cationic charge to charge balance M.Type: GrantFiled: July 8, 2009Date of Patent: October 18, 2011Assignee: Ford Motor CompanyInventors: Jun Yang, Andrea Sudik, Donald J. Siegel, Shinichi Hirano, Andrew Robert Drews, Christopher Mark Wolverton
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Publication number: 20110158881Abstract: The present invention provides a method for synthesis of crystalline polymeric boron-nitrogen compounds comprising a step of dehydrogenation of a boron-nitrogen-hydrogen compound on catalyst, wherein the boron-nitrogen-hydrogen compound is selected from the group consisting of ammonia borane, metal amidoboranes, amine boranes or mixtures thereof, and the catalyst is selected from the group consisting of transition metals, transition metal salts or alloys.Type: ApplicationFiled: July 20, 2010Publication date: June 30, 2011Applicant: Dalian Institute of Chemical Physics, Chinese Academy of SciencesInventors: Ping Chen, Teng He, Zhitao Xiong, Guotao Wu
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Publication number: 20110064640Abstract: A method of preparing a boron-nitrogen compound includes combining an ammonium salt and an ionic compound in the absence of solvent to form a mixture. The ionic compound includes a cation and an anion. The anion is represented by the general formula B(R1)4?, wherein each R1 is independently selected from the group of hydrogen, alkyl groups, aryl groups, and combinations thereof. The method also includes agitating the mixture in the absence of solvent to form a reaction product, and separating the boron-nitrogen compound from the reaction product.Type: ApplicationFiled: September 15, 2010Publication date: March 17, 2011Applicant: Wildcat Discovery TechnologiesInventors: Steven Kaye, Conor Riley
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Patent number: 7897129Abstract: The present invention discloses new methods for synthesizing ammonia borane (NH3BH3, or AB). Ammonium borohydride (NH4BH4) is formed from the reaction of borohydride salts and ammonium salts in liquid ammonia. Ammonium borohydride is decomposed in an ether-based solvent that yields AB at a near quantitative yield. The AB product shows promise as a chemical hydrogen storage material for fuel cell powered applications.Type: GrantFiled: April 28, 2009Date of Patent: March 1, 2011Assignee: Battelle Memorial InstituteInventors: S. Thomas Autrey, David J. Heldebrant, John C. Linehan, Abhijeet J. Karkamkar, Feng Zheng
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Patent number: 7846410Abstract: Method of producing ammonia borane, comprising providing polyborazylene; digesting the polyborazylene with a dithiol-containing agent to produce a boro-sulfide compound and a byproduct; converting the byproduct to the boro-sulfide product of step (b) by reaction with a first alkyl-tin hydride; and, converting the boro-sulfide compound produced in steps (b) and (c) to ammonia borane by reaction with a second alkyl-tin hydride.Type: GrantFiled: January 14, 2009Date of Patent: December 7, 2010Assignee: Los Alamos National Security, LLCInventors: Benjamin L. Davis, John C. Gordon
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Publication number: 20100272623Abstract: A method of preparing an ammonia borane compound selected from the group consisting of: ammonia borane, ammonia alkyl borane, ammonia aryl borane and mixtures thereof, the method including the steps of: a) incorporating a reaction mixture into a pressure vessel, the reaction mixture including anhydrous liquid ammonia and a boron containing compound that can react under pressure with the liquid ammonia to form the ammonia borane compound; and, b) causing the reaction mixture to warm from a first temperature greater than or equal to ?33° C. to a second temperature under pressure to form the ammonia borane compound.Type: ApplicationFiled: April 20, 2010Publication date: October 28, 2010Applicant: K-Energetics Corp.Inventors: Alexander LUKACS, III, Leonard Macadams, Kevin Christmas
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Publication number: 20100272622Abstract: Method of producing ammonia borane, comprising providing a reagent comprising a dehydrogenated material in a suitable solvent; and combining the reagent with a reducing agent comprising hydrazine, a hydrazine derivative, or combinations thereof, in a reaction which produces a mixture comprising ammonia borane.Type: ApplicationFiled: April 19, 2010Publication date: October 28, 2010Applicant: LOS ALAMOS NATIONAL SECURITY, LLCInventors: Andrew Sutton, John C. Gordon, Kevin C. Ott, Anthony K. Burrell
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Patent number: 7695704Abstract: A process for producing borazane from boron-nitrogen and boron-nitrogen-hydrogen containing BNH-waste products. The process includes reacting the BNH-waste products with a hydrogen halide, having the formula HX, wherein X is selected from the group consisting of F, Cl, Br, I, and combinations thereof, to form any of the following: a boron trihalide, having the formula BX3, an ammonium halide, having the formula NH4X, and hydrogen. The boron trihalide is then reacted with the hydrogen to form diborane, having the formula B2H6, and hydrogen halide. The ammonium halide is then converted to ammonia, having the formula NH3, and hydrogen halide. The diborane is then reacted with the ammonia to form borazane, having the formula BH3NH3.Type: GrantFiled: February 13, 2007Date of Patent: April 13, 2010Assignees: GM Global Technology Operations, Inc., Albert Ludwigs Universitat FreiburgInventors: Gert Wolf, Felix Baitalow, Gerhard Roewer, Steffen Hausdorf, Gerd Arnold, Ulrich Eberle, Dieter Hasenauer, Florian O. Mertens
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Patent number: 7645902Abstract: A method of dehydrogenating an amine-borane using an acid-catalyzed reaction. The method generates hydrogen and produces a solid polymeric [R1R2B—NR3R4]n product. The method of dehydrogenating amine-boranes may be used to generate H2 for portable power sources.Type: GrantFiled: June 22, 2006Date of Patent: January 12, 2010Assignee: Los Alamos National Security, LLCInventors: Frances Helen Stephens, Ralph Thomas Baker
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Publication number: 20090291039Abstract: The present invention discloses new methods for synthesizing ammonia borane (NH3BH3, or AB). Ammonium borohydride (NH4BH4) is formed from the reaction of borohydride salts and ammonium salts in liquid ammonia. Ammonium borohydride is decomposed in an ether-based solvent that yields AB at a near quantitative yield. The AB product shows promise as a chemical hydrogen storage material for fuel cell powered applications.Type: ApplicationFiled: April 28, 2009Publication date: November 26, 2009Applicant: BATTELLE MEMORIAL INSTITUTEInventors: S. Thomas Autrey, David J. Heldebrant, John C. Linehan, Abhijeet J. Karkamkar, Feng Zheng
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Publication number: 20090191110Abstract: Method of producing ammonia borane, comprising providing polyborazylene; digesting the polyborazylene with a dithiol-containing agent to produce a boro-sulfide compound and a byproduct; converting the byproduct to the boro-sulfide product of step (b) by reaction with a first alkyl-tin hydride; and, converting the boro-sulfide compound produced in steps (b) and (c) to ammonia borane by reaction with a second alkyl-tin hydride.Type: ApplicationFiled: January 14, 2009Publication date: July 30, 2009Inventors: Benjamin L. Davis, John C. Gordon
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Patent number: 7544837Abstract: A method of dehydrogenating an amine-borane having the formula R1H2N—BH2R2 using base metal catalyst. The method generates hydrogen and produces at least one of a [R1HN—BHR2]m oligomer and a [R1N—BR2]n oligomer. The method of dehydrogenating amine-boranes may be used to generate H2 for portable power sources, such as, but not limited to, fuel cells.Type: GrantFiled: October 30, 2006Date of Patent: June 9, 2009Assignee: Los Alamos National Security, LLCInventors: Johanna Marie Blacquiere, Richard Jeffrey Keaton, Ralph Thomas Baker
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Publication number: 20090104102Abstract: Methods of synthesizing ammonia borane are provided. The methods comprise reacting at least one amine borane with ammonia such that ammonia borane is produced. Ammonia borane has a chemical formula Of NH3—BH3 and provides a good source of storage hydrogen making it useful in a variety of applications including a potential hydrogen source for fuel cells. The methods can further comprise separating the ammonia borane from the other products of the reaction. Exemplary methods can produce ammonia borane having purity greater than about 90 percent. In further examples, the methods can produce ammonia borane having purity greater than about 95 percent or greater than about 99 percent.Type: ApplicationFiled: April 2, 2007Publication date: April 23, 2009Inventors: Sheldon Gerald Shore, Xuenian Chen
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Publication number: 20080175781Abstract: Metal hydride materials react with BZ3 compounds in the presence of ligand to form BH3-L compounds. A compound of the formula HBZ2 is prepared from a compound of the formula BZ3 by reacting a first amount of a compound of the formula HBZ2 with a metal hydride material “MH” and a compound “L” to form a material of the formula BH3-L, and then reacting the BH3-L thus formed with a compound of the formula BZ3 to form HBZ2 in a second amount greater than the first amount of HBZ2. Z is selected from alkoxy, aryloxy, amido, arylamido, doubly substituted alkoxy, doubly substituted aryloxy, doubly substituted amido, doubly substituted arylamido, alkoxy-amido, and aryloxy-arylamido. When Z is bidentate, then HBZ2 has a ring structure. “L” is selected from ethers, aromatic ethers, amines, aromatic amines, heterocyclic nitrogen compounds, sulfides, aromatic sulfides, and heterocyclic sulfur compounds. “L” becomes a ligand in the BH3-L material.Type: ApplicationFiled: September 13, 2007Publication date: July 24, 2008Inventors: David L. Thorn, William Tumas
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Patent number: 7361213Abstract: A hybrid hydrogen storage composition includes a first phase and a second phase adsorbed on the first phase, the first phase including BN for storing hydrogen by physisorption and the second phase including a borazane-borazine system for storing hydrogen in combined form as a hydride.Type: GrantFiled: August 22, 2005Date of Patent: April 22, 2008Assignee: UT-Battelle, LLCInventors: Chaitanya K. Narula, J. Michael Simonson, Leon Maya, Robert T. Paine
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Publication number: 20020058142Abstract: There is provided a low dielectric constant material, which is excellent in thermal resistance, has low dielectric constant, and is applicable to a semiconductor device or electric appliances, an insulation film between semiconductor layers using the same, and the semiconductor device. The material is the low dielectric constant material having thermal resistance, which contains borazine skeletal molecules shown by the following formula (1) and the like in an inorganic or organic material molecule.Type: ApplicationFiled: August 31, 2001Publication date: May 16, 2002Applicant: MITSUBISHI DENKI KABUSHIKI KAISHAInventors: Sei Tsunoda, Hideharu Nobutoki, Noboru Mikami
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Patent number: 6025454Abstract: Direct thermal syntheses in the absence of catalyst, of poly(borazylenes) and of oligomers of borazine with polyhedral boranes, carboranes or heteroboranes are disclosed. The products of these syntheses are precursors to BN or other boron-containing ceramics.Type: GrantFiled: December 5, 1996Date of Patent: February 15, 2000Assignee: The Trustees of the University of PennsylvaniaInventors: Larry G. Sneddon, Jeffrey Scott Beck, Paul Joseph Fazen
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Patent number: 5833939Abstract: A low-temperature phase oxide single crystal having a nominal composition of Ba(B.sub.1-x M.sub.x).sub.2 O.sub.4 is synthesized by partially substituting B of BaB.sub.2 O.sub.4 with one or more additive elements M and by growing the single crystal in a Ba(B.sub.1-x M.sub.x).sub.2 O.sub.4 composition compound (where M is one or more additive elements selected from the group consisting of Al, Ga and In, and 0.001<x<0.15).Type: GrantFiled: December 3, 1996Date of Patent: November 10, 1998Assignee: National Research Institute for MetalsInventors: Hideo Kimura, Takenori Numazawa, Mitsunori Sato
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Patent number: 5612013Abstract: A method for synthesizing borazine in high yields by the reaction of certain ammonium salts, such as ammonium sulfate, and a borohydride, such as sodium borohydride, in solvent at moderate temperatures (e.g., 120.degree.-140.degree. C.) is disclosed.Type: GrantFiled: February 10, 1995Date of Patent: March 18, 1997Assignee: Trustees of the University of PennsylvaniaInventors: Larry G. Sneddon, Thomas Wideman
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Patent number: 5502142Abstract: Direct thermal syntheses in the absence of catalyst, of poly(borazylenes) and of oligomers of borazine with polyhedral boranes, carboranes or heteroboranes are disclosed. The products of these syntheses are precursors to BN or other boron-containing ceramics.Type: GrantFiled: October 26, 1993Date of Patent: March 26, 1996Assignee: The Trustees of the University of PennsylvaniaInventors: Larry G. Sneddon, Jeffrey S. Beck, Paul J. Fazen
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Patent number: 5399377Abstract: Borazine oligomers in liquid form are produced and used to create composites of fibers bonded to boron nitride as a matrix and also to coat or increase the density of various fiber composites.Type: GrantFiled: December 31, 1992Date of Patent: March 21, 1995Assignee: The Board of Trustees of the University of IllinoisInventors: James Economy, Dong-pyo Kim
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Patent number: 5055280Abstract: A process for producing fibers of a transition metal boride, which comprises reacting a mixture of a vapor of an evaporable boron compound an a vapor of an evaporable transition metal compound in the presence of a catalyst composed of at least one metal selected from the group consisting of Pt, Pd, Cu, Au and Ni.Type: GrantFiled: September 16, 1988Date of Patent: October 8, 1991Assignee: National Research Institute For MetalsInventors: Isao Nakatani, Kiyoshi Ozawa
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Patent number: 5026809Abstract: Preceramic polymers formed by reacting B.sub.10 H.sub.14-n R.sub.n, (where R is a lower alkyl group having from 1 to about 8 carbon atoms, a substituted or unsubstituted cycloalkyl group having from 3 to about 8 carbon atoms, a substituted or unsubstituted lower alkenyl group having from 2 to about 8 carbon atoms, or a substituted or unsubstituted lower aryl group having from 6 to about 10 carbon atoms, and n is a number from zero to about six) with a diamine of the formulaR.sup.1 R.sup.2 N--(E).sub.q --NR.sup.4 R.sup.5,where R.sup.1, R.sup.2, R.sup.4 and R.sup.Type: GrantFiled: June 2, 1989Date of Patent: June 25, 1991Assignee: Massachusetts Institute of TechnologyInventors: Seyferth Dietmar, William S. Rees, Jr.
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Patent number: 4871826Abstract: New soluble preceramic polymers formed by reacting B.sub.10 H.sub.14-n R.sub.n, (where R is a lower alkyl group having from 1 to about 8 carbon atoms, a substituted or unsubstituted cycloalkyl group having from 3 to about 8 carbon atoms, a substituted or unsubstituted lower alkenyl group having from 2 to about 8 carbon atoms, or a substituted or unsubstituted lower aryl group having from 6 to about 10 carbon atoms, and n is a number from zero to about six) with a diamine in an organic solvent are disclosed. Preferably the diamine has the formulaR.sup.1 R.sup.2 N-R.sup.3 -NR.sup.4 R.sup.5where R.sup.1, R.sup.2, R.sup.4 and R.sup.5 are H, a lower alkyl group having from 1 to about 8 carbon atoms, a substituted or unsubstituted cycloalkyl group having from 3 to about 8 carbon atoms, a substituted or unsubstituted lower alkenyl group having from 2 to about 8 carbon atoms, a substituted or unsubstituted lower aryl group having from 6 to about 10 carbon atoms, or a di- or triorganosilyl. R.sup.Type: GrantFiled: June 22, 1987Date of Patent: October 3, 1989Assignee: Massachusetts Institute of TechnologyInventors: Dietmar Seyferth, William S. Rees, Jr.
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Patent number: 4801439Abstract: A process for preparing tractable preceramic precursors of Group IIIA metal/Group VA nonmetal compounds, such as BN, in which a first reactant containing a Group VA nonmetal to hydrogen bond, such as ammonia or an amine is reacted with a second reactant containing a Group IIIA metal to hydrogen bond, such as a metal hydride, in the presence of a metal catalyst that catalyzes dehydrocoupling of the bonds to form the precursor. Further reaction of the precursor in the presence of the catalyst forms oligomeric/polymeric forms of the precursor.Type: GrantFiled: September 15, 1986Date of Patent: January 31, 1989Assignee: SRI InternationalInventors: Yigal D. Blum, Richard M. Laine
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Patent number: 4746501Abstract: A process for making ammonolytic precursors to nitride and carbonitride ceramics. Extreme reaction conditions are not required and the precursor is a powder-like substance that produces ceramics of improved purity and morphology upon pyrolysis.Type: GrantFiled: August 6, 1987Date of Patent: May 24, 1988Assignee: United States Department of EnergyInventor: Leon Maya
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Patent number: 4150097Abstract: A method for synthesizing borazine by preparing a liquid mixture of ammonia borane and a high boiling point solvent which is inert to ammonia borane, and heating said mixture to obtain borazine and hydrogen. Volatized borazine is stripped from the hydrogen during synthesis and any borazine entrained in the solvent is removed by distillation.Type: GrantFiled: March 30, 1978Date of Patent: April 17, 1979Assignee: Mine Safety Appliances CompanyInventors: William V. Hough, Clarence R. Guibert, Gerald T. Hefferan
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Patent number: 4099924Abstract: Mechanical components such as dies and crucibles, which come in contact with a silicon melt during the formation of single crystalline shaped silicon particles, e.g. thin sheets or ribbons, are coated with silicon oxynitride deposited by chemical vapor deposition techniques.Type: GrantFiled: March 16, 1977Date of Patent: July 11, 1978Assignee: RCA CorporationInventors: Samuel Berkman, Michel Thomas Duffy, Kyong-Min Kim, Glenn Wherry Cullen