Aluminum Containing Patents (Class 423/412)
  • Patent number: 5693305
    Abstract: A method for making aluminum nitride whiskers comprising reacting a reactant bed of aluminum, alumina, ammonium chloride, with a metal-containing carbon catalyst in the presence of a nitrogen gas flow, such that a direct nitridation reaction, a carbothermal reaction and a transport species reaction occur concurrently.
    Type: Grant
    Filed: October 19, 1995
    Date of Patent: December 2, 1997
    Assignee: Advanced Refractory Technologies, Inc.
    Inventors: Vithal Revankar, Arvind Goel
  • Patent number: 5674465
    Abstract: The invention relates to a continuous process for the preparation of aluminum nitride by the carbonitriding of alumina. According to this process, a reaction that uses alumina, carbon, and a resin that generates carbon by pyrolysis is performed in a methodical reactor. The invention relates to a continuous process for the preparation of aluminum nitride by the carbonitriding of alumina.
    Type: Grant
    Filed: January 24, 1996
    Date of Patent: October 7, 1997
    Assignee: Elf Atochem S.A.
    Inventors: Pierre Ravenel, Roland Bachelard, Jean-Pierre Disson, Philippe Joubert
  • Patent number: 5646078
    Abstract: An aluminum nitride powder comprising polycrystalline particles which have clearly observed grain boundaries, an agglomerated particle size of 0.1 to 100 .mu.m when measured by a particle size distribution analyzer, a tapped bulk density of 0.55 to 2.0 g/cm.sup.3, and a ratio of a number average particle size calculated from a SEM photograph image to a particle size calculated from a BET specific surface area of 1.1 to 3.
    Type: Grant
    Filed: July 12, 1995
    Date of Patent: July 8, 1997
    Assignee: Sumitomo Chemical Company, Limited
    Inventors: Masahide Mohri, Shinichiro Tanaka, Takeshi Miyai
  • Patent number: 5626827
    Abstract: Disclosed are basic aluminum antiperspirant materials having univalent complex oxoanions (e.g., nitrate); methods of making such materials; antiperspirant compositions containing such basic aluminum materials, another antiperspirant active material (e.g., a basic zirconium halide salt), and optionally a neutral amino acid; and methods of making such compositions. Size exclusion high performance liquid chromatography chromatograms of the disclosed basic aluminum materials have a peak 4 relative area of at least 25%, a peak 3 relative area of less than 60%, the sum of the peaks 3 and 4 being at least 50%; and less than 10% of the chromatographic peaks eluting at peaks 1 and 2. The disclosed basic aluminum materials have less than 25% of the aluminum in the form of Al.sup.b polyhydroxyaquoaluminum, and have a .sup.27 Al NMR spectrum in which the area of the 71.5-73.5 ppm resonance line includes more than 50% of the combined areas of the 62.5-63.5 ppm and 71.5-73.
    Type: Grant
    Filed: June 1, 1995
    Date of Patent: May 6, 1997
    Assignee: The Mennen Company
    Inventors: Morton L. Barr, Paul J. Vincenti, Elaine L. Vanderhoof
  • Patent number: 5573742
    Abstract: A process and apparatus for making high purity aluminum nitride from organometallic aluminum, such as an alkylaluminum compound. A gaseous alkylaluminum compound and gaseous ammonia are introduced into a heated reaction zone where the gases are mixed and high purity aluminum nitride is produced. The high purity aluminum nitride is collected in the form of a powder or deposited as a thick, dense layer on an appropriate substrate mounted in the reaction chamber. A carrier gas such as hydrogen gas, may be used to conduct the alkylaluminum compound from a suitable reservoir containing liquid alkylaluminum compound to the reaction chamber. A preferred alkylaluminum compound is triethylaluminum.
    Type: Grant
    Filed: October 29, 1987
    Date of Patent: November 12, 1996
    Assignee: Martin Marietta Corporation
    Inventor: Joseph J. Gebhardt
  • Patent number: 5559203
    Abstract: An aluminum-nitrogen polymer is prepared by reacting an organic nitrile with a dialkylaluminum hydride to form an organoaluminum imine, and heating the imine to a temperature of 50.degree. to 200.degree. C. for at least 2 hours. The polymeric product can be subjected to an additional heat treatment to form a more highly cross-linked polymer. After either heat treatment the polymeric product can be further reacted with a primary amine or ammonia. The organoaluminum imine as well as the aminated or non-aminated polymers can be pyrolyzed to form an aluminum nitride-containing ceramic.
    Type: Grant
    Filed: August 11, 1995
    Date of Patent: September 24, 1996
    Assignee: Lanxide Technology Company, LP
    Inventor: James A. Jensen
  • Patent number: 5538705
    Abstract: Aluminum nitride (AlN) is continuously produced by continuously carbonitriding a continuously replenished charge of alumina, for example successive charges of alumina/carbon extrudates, in a reaction zone comprising at least one conduit, the ratio of the exchange surface area/volume of which at least one conduit ranging from 5 to 50 m.sup.-1, preferably from 10 to 50 m.sup.-1, and continuously withdrawing product AlN therefrom.
    Type: Grant
    Filed: September 13, 1994
    Date of Patent: July 23, 1996
    Assignee: ELF Atochem S.A.
    Inventors: Pierre Ravenel, Jean-Pierre Disson, Roland Bachelard
  • Patent number: 5525320
    Abstract: Processes for the direct manufacture of nitride powders suitable for low temperature sintering are provided. An elemental vapor is contacted with a nitriding gas at temperatures between 1400 and 1973 K and atmospheric pressure to produce nitride powder.
    Type: Grant
    Filed: July 11, 1994
    Date of Patent: June 11, 1996
    Assignee: University of Cincinnati
    Inventors: Sotiris E. Pratsinis, M. Kamal Akhtar, Guizhi Wang, Siddhartha Panda
  • Patent number: 5525321
    Abstract: The invention relates to a continuous process for the preparation of aluminium nitride by the carbonitriding of alumina.According to this process, the reaction, which employs alumina, carbon and nitrogen, is carried out in a moving-bed reactor characterized in that the reaction area has a plurality of conduits.
    Type: Grant
    Filed: September 16, 1994
    Date of Patent: June 11, 1996
    Assignee: Elf Atochem S.A.
    Inventors: Pierre Ravenel, Roland Bachelard
  • Patent number: 5468697
    Abstract: Ultrafine particles of aluminum nitride having a morphologically anisotropic structure of columns, plates, or whiskers such that the ratio of thickness or width to length or the ratio of thickness to width or length of particle is not less than 1 are produced by thermally melting a binary alloy of metallic aluminum and a rare earth element in a nitriding atmosphere containing nitrogen. By this method are produced composite ultrafine particles which substantially comprise ultrafine particles of aluminum nitride having the morphologically anisotropic structure and ultrafine particles of the rare earth nitride which functions as a sintering auxiliary therefor. The composite ultrafine particles or an aggregate thereof are usable as a raw material for the production of a sintered article, a reinforcing material for various metal-based composite materials, a blast powder, and the like.
    Type: Grant
    Filed: March 15, 1994
    Date of Patent: November 21, 1995
    Assignees: Yoshida Kogyo K.K., Tsuyoshi Masumoto, Akihisa Inoue, Honda Giken Kogyo Kabushiki Kaisha
    Inventors: Tadashi Yamaguchi, Katsutoshi Nosaki, Akihisa Inoue, Tsuyoshi Masumoto
  • Patent number: 5460794
    Abstract: A method of manufacturing a powdery AlN comprising steps of: a) providing an airtight vessel, b) preparing a powdery Al and a solid-state nitride, c) wrapping up the powdery Al and the solid-state nitride with an igniting agent, d) putting the wrapped Al and nitride into the vessel, e) evacuating the airtight vessel and filling therein with an N gas, and f) igniting the igniting agent. Since the powdery Al and solid-state nitride are completely wrapped up with an igniting agent, the reaction can be more rapidly and fully completed under a relatively low pressure. In addition, the present method can be used to obtain an AlN having a high purity.
    Type: Grant
    Filed: August 11, 1993
    Date of Patent: October 24, 1995
    Assignee: National Science Council
    Inventors: Shyan-Lung Chung, Chang-Lin Tu, Wei-Chang Lee
  • Patent number: 5459113
    Abstract: A sinterable aluminum nitride powder composition is prepared by adding about 0.05-10.0 parts by weight of at least one compound selected from the group consisting of calcium tungstate and calcium molybdate and optionally about 1.0-7.0 parts by weight of at least one compound selected from the group consisting of yttria, calcium oxide, and calcium carbonate to 100 parts by weight of an aluminum nitride powder prepared by the alumina reduction method without decarbonization and having a residual carbon content of about 2%-10% by weight. The resulting powdery composition is subjected to mixing and deagglomeration in a dry process so as to form a powder mixture having a bulk density of about 0.3-0.5 g/cm.sup.3, and then to decarbonization by heating in an oxidizing atmosphere. The aluminum nitride powder composition has a pressurized bulk density of about 1.50-1.75 g/cm.sup.3 as measured at a pressure of 500 kg/cm.sup.2 and an average particle diameter of about 1.0-3.0 .mu.
    Type: Grant
    Filed: February 1, 1994
    Date of Patent: October 17, 1995
    Assignee: Sumitomo Metal Ceramics Inc.
    Inventors: Toshio Nozaki, Seigo Ohiwa, Hiroshi Iwase, Masanori Oguni
  • Patent number: 5455322
    Abstract: This invention provides a process for manufacturing aluminum-nitrogen polymers (i.e., polymers having a backbone of alternating aluminum and nitrogen atoms) in which portions of the polymer have an organic substituent on each aluminum and nitrogen atom. The novel polymers so produced are useful for making green shapes pyrolyzable to AlN articles suitable for high performance applications. The process generally comprises reacting an organic nitrile having the formula R.sup.1 CN with a trialkylaluminum compound having the formula R.sup.2 R.sup.3 R.sup.4 Al, and optionally heating the reaction product, to form an organoaluminum imine, and heating the organoaluminum imine to a temperature of at least 300.degree. C. and less than 600.degree. C. for at least two hours to form an aluminum-nitrogen polymer. The polymer or the imine can be pyrolyzed to form an aluminum nitride ceramic article. In the foregoing formulae, R.sup.
    Type: Grant
    Filed: July 13, 1994
    Date of Patent: October 3, 1995
    Assignee: Lanxide Technology Company, LP
    Inventor: James A. Jensen
  • Patent number: 5453407
    Abstract: A method for producing nitride ceramic powders includes steps of a) providing a powder, b) providing a nitride, c) providing a salt of ammonium halide, d) mixing the powder, the nitride, and the salt to form a reactant, e) wrapping up the reactant with an igniting agent, f) placing the reactant wrapped up with the igniting agent in a vessel, g) evacuating the vessel, h) igniting the igniting agent for initiating a combustion reaction to form the nitride ceramic powders. Such method can permit excellent nitride ceramic powders to be effectively produced.
    Type: Grant
    Filed: February 14, 1994
    Date of Patent: September 26, 1995
    Assignee: National Science Council
    Inventors: Shyau L. Chung, Wei-Chang Lee
  • Patent number: 5411762
    Abstract: A ceramic material based on Sialon, in particular on .beta.'-Sialon is obtained by reducing an aluminosilicate precursor by means of a gas phase comprising a mixture of hydrogen and nitrogen doped with a gaseous carbon compound. The gaseous carbon compound is a gas containing carbon in combined form, e.g. an alkane, and its concentration by volume in the gas is less than 3%. The method is particularly suitable for forming Sialon-based coatings on substrates that are solid or fibrous. For composite materials constituted by a fiber preform densified by means of a matrix, the method can be used to form an interphase coating on the fibers of the preform prior to densifying the preform, or the method can be used to form a matrix that is based on Sialon.
    Type: Grant
    Filed: February 2, 1994
    Date of Patent: May 2, 1995
    Assignee: Societe European De Propulsion
    Inventors: Jacques Thebault, Alain Seron, Francois Beguin
  • Patent number: 5401697
    Abstract: A method of processing water-sensitive ceramic powders, particularly carbothermically produced aluminum nitride, whereby the ceramic powder is deagglomerated in a dry milling step with addition of an alkylamine which is liquid at room temperature is disclosed. The alkylamine is added in an amount sufficient to produce a monomolecular layer on the surface of the ceramic powder. The deagglomerated powder subsequently is vigorously stirred with a concentrated aqueous solution or dispersion of binder and rapidly and gently dried, preferably by freeze drying. Aluminum nitride powder prepared by this process can be further processed into shaped parts with a high thermal conductivity.
    Type: Grant
    Filed: September 8, 1993
    Date of Patent: March 28, 1995
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Hans-Michael Guether, Katharina Seitz, Friedrich Hessel, Frank Schroeder, Christine Koestler, Andreas Roosen
  • Patent number: 5395606
    Abstract: A metal nitride powder can be made by heating a reactant powder that includes an oxide or hydroxide of Al, Ti, or Zr to a reaction temperature in a nonreactive atmosphere. The heated reactant powder is contacted with a gaseous reactant mixture comprising a nitrogen source and a carbon source. The molar ratio of nitrogen to carbon in the gaseous reactant mixture is at least about 15. The reactant powder is maintained at the reaction temperature for a sufficient time to convert a portion of it to metal nitride powder.
    Type: Grant
    Filed: November 3, 1993
    Date of Patent: March 7, 1995
    Assignee: United Technologies Corporation
    Inventors: Youming Xiao, Benj J. Tan, Steven L. Suib, Francis S. Galasso
  • Patent number: 5370854
    Abstract: Carbothermally reduce a metal oxide to its corresponding metal nitride or metal carbide powder in a vertical gravity flow reactor by adding precursor pellets containing the metal oxide, a thermally decomposed binder material and carbon or a source of carbon directly to a heated reaction zone within the reactor. The pellets form a pellet bed, the top of which must be maintained within the heated reaction zone. The binder material is a blend of wheat and corn starches, optionally in conjunction with another binder such as melamine. The binder material thermally decomposes to a carbonaceous residue which functions both as an additional source of carbon and as a binder for the precursor pellets. The reactor may be modified by adding an internal vent line to remove volatile materials from the heated reaction zone before they have an opportunity to condense on internal reactor surfaces.
    Type: Grant
    Filed: January 8, 1993
    Date of Patent: December 6, 1994
    Assignee: The Dow Chemical Company
    Inventors: John P. Henley, Gene A. Cochran, David A. Dunn, Glenn A. Eisman, Alan W. Weimer
  • Patent number: 5356608
    Abstract: A process and apparatus for making high purity aluminum nitride from organometallic aluminum, such as an alkylaluminum compound. A gaseous alkylaluminum compound and gaseous ammonia are introduced into a heated reaction zone where the gases are mixed and high purity aluminum nitride is produced. The high purity aluminum nitride is collected in the form of a powder or deposited as a thick, dense layer on an appropriate substrate mounted in the reaction chamber. A carrier gas such as hydrogen gas, may be used to conduct the alkylaluminum compound from a suitable reservoir containing liquid alkylaluminum compound to the reaction chamber. A preferred alkylaluminum compound is triethylaluminum.
    Type: Grant
    Filed: March 16, 1989
    Date of Patent: October 18, 1994
    Assignee: Martin Marietta Corporation
    Inventor: Joseph J. Gebhardt
  • Patent number: 5352424
    Abstract: An aluminum nitride powder that has substantially no ammonia odor after exposure to atmospheric moisture is obtained by admixing the powder with a gettering compound that sublimes or decomposes at a temperature below 500.degree. C. The gettering compound is a C.sub.1 -C.sub.11 aliphatic carboxylic mono- or polyfunctional acid, an anhydride or an ester of such an acid or an anhydride of an aromatic carboxylic acid.
    Type: Grant
    Filed: February 16, 1993
    Date of Patent: October 4, 1994
    Assignee: The Dow Chemical Company
    Inventors: Kevin E. Howard, John R. Moyer
  • Patent number: 5348720
    Abstract: Disclosed is a basic aluminum material having enhanced antiperspirant activity, the material having the empirical formula Al.sub.2 (OH).sub.6-a X.sub.a, where 0.5.ltoreq.a.ltoreq.5.0, and X is a univalent complex oxoanion of nitrogen, chlorine and other halogens, which forms salts with Al.sup.3+ in aqueous solution so that these salts are essentially completely dissociated, which is readily soluble in water with metallic ions in the solution, and which forms conjugate acids that are strong acids; and wherein the material is characterized by:(a) size exclusion high performance liquid chromatography peaks corresponding to peak 3 and peak 4 of size exclusion chromatograms formed by HPLC technique;(b) a peak 4 relative area of at least 25%, a peak 3 relative area of less than 60%, the sum of the relative peak 3 and peak 4 areas being at least 50%; and(c) less than 10% chromatographic peaks eluting at shorter retention times than peak 3, corresponding to peaks 1 and 2.
    Type: Grant
    Filed: February 23, 1993
    Date of Patent: September 20, 1994
    Assignee: The Mennen Company
    Inventors: Paul J. Vincenti, Morton L. Barr
  • Patent number: 5344635
    Abstract: A powder mixture of aluminium nitride in the form of sintered agglomerates with fractions of different particle size, which mixture comprises (1) 80 to 50% by weight of aluminium nitride in the form of sintered agglomerates having a mean particle diameter of 30 to 50 .mu.m, and (2) 20 to 50% by weight of aluminium nitride in the form of unsintered particles and having a mean particle diameter of 0.1 to 5 .mu.m. The mixture is suitable for use as filler for polymer materials, especially for casting resins, from which moulded parts of high thermal conductivity can be fabricated, for example potted electronic components.
    Type: Grant
    Filed: February 1, 1993
    Date of Patent: September 6, 1994
    Assignee: Ciba-Geigy Corporation
    Inventors: Patrice Bujard, Ileana Cojanu
  • Patent number: 5340896
    Abstract: Aluminum-nitrogen polymers comprising a backbone of alternating aluminum and nitrogen atoms both having pendant organic groups, wherein some of the pendant organic groups are unsaturated, are prepared by reacting an unsaturated organic nitrile with a dialkylaluminum hydride. The polymers are crosslinked by supplying energy to generate free radicals. The crosslinked polymers can be pyrolyzed to form an aluminum nitride ceramic.
    Type: Grant
    Filed: November 8, 1993
    Date of Patent: August 23, 1994
    Inventor: James A. Jensen
  • Patent number: 5279808
    Abstract: A metal nitride powder can be made by heating a reactant powder that includes an oxide or hydroxide of Al, Ti, or Zr to a reaction temperature in a nonreactive atmosphere. The heated reactant powder is contacted with a gaseous reactant mixture comprising a nitrogen source and a carbon source. The molar ratio of nitrogen to carbon in the gaseous reactant mixture is at least about 15. The reactant powder is maintained at the reaction temperature for a sufficient time to convert a portion of it to metal nitride powder.
    Type: Grant
    Filed: December 17, 1992
    Date of Patent: January 18, 1994
    Assignee: United Technologies Corporation
    Inventors: Youming Xiao, Beng J. Tan, Steven L. Suib, Francis S. Galasso
  • Patent number: 5260397
    Abstract: Aluminum-nitrogen polymers comprising a backbone of alternating aluminum and nitrogen atoms both having pendant organic groups, wherein some of the pendant organic groups are unsaturated, are prepared by reacting an unsaturated organic nitrile with a dialkylaluminum hydride. The polymers are crosslinked by supplying energy to generate free radicals. The crosslinked polymers can be pyrolyzed to form an aluminum nitride ceramic.
    Type: Grant
    Filed: February 3, 1992
    Date of Patent: November 9, 1993
    Inventor: James A. Jensen
  • Patent number: 5246683
    Abstract: A process for producing small particles of aluminum nitride suitable for sintering and the particles thus-produced. The process comprises reacting particles of gamma alumina, or a precursor thereof, of less than 1 micron in size with a stoichiometrical excess of finely divided carbon in the presence of nitrogen, or a precursor which provides nitrogen in the reaction conditions, first at a temperature in the range of 1550.degree. to 1700.degree. C. for a period of between 1 and 6 (preferably 1 to 4) hours and then at a temperature in the range of 1750.degree. to 1850.degree. C. for a period of 1 to 4 (preferably 1 to 2) hours, followed by cooling said reaction mixture and reheating to a temperature in the range of 500.degree. to 700.degree. C. in an oxygen-containing atmosphere, and maintaining the temperature until excess unreacted carbon is removed.
    Type: Grant
    Filed: October 2, 1992
    Date of Patent: September 21, 1993
    Assignee: Alcan Internatonal Limited
    Inventors: Luc Parent, Mukesh Jain
  • Patent number: 5234676
    Abstract: An aqueous composition containing aluminum nitride powder which exhibits a reduced tendency for hydrolysis of the aluminum nitride contained therein. The aqueous composition comprises (a) a liquid medium containing water, (b) aluminum nitride powder, and (c) a combination of buffering agents which controls the pH of water from about 5.5 to about 7.5, wherein the combination of buffering agents is employed at a lower weight percent concentration than that of the aluminum nitride powder. In another embodiment of the invention, a method of processing aluminum nitride powder in water which exhibits a reduced tendency for hydrolysis of the aluminum nitride is disclosed, which method involves mixing the above-described aqueous composition.
    Type: Grant
    Filed: April 16, 1992
    Date of Patent: August 10, 1993
    Assignee: The Dow Chemical Company
    Inventor: Kevin E. Howard
  • Patent number: 5229468
    Abstract: A block copolymer is prepared by reacting an aluminum-nitrogen polymer and a silazane polymer at a temperature not greater than 400.degree. C. Block copolymers containing alkenyl or alkynyl groups can be crosslinked by supplying energy to generate free radicals. An AlN/SiC containing ceramic is formed by pyrolyzing the crosslinked block copolymer in a nonoxidizing atmosphere.
    Type: Grant
    Filed: February 13, 1992
    Date of Patent: July 20, 1993
    Assignee: Hercules Incorporated
    Inventor: James A. Jensen
  • Patent number: 5226952
    Abstract: A process for refining calcium containing aluminum as an impurity in the form CaAl.sub.2. The calcium is nitrided to form Ca.sub.3 N.sub.2, and that Ca.sub.3 N.sub.2 is made to react with CaAl.sub.2 initially present and with the particulate aluminum in such a manner as to form calcium, which is isolatable in the form of high-purity calcium containing less than 0.1% by weight of aluminum, and aluminum nitride.
    Type: Grant
    Filed: May 15, 1992
    Date of Patent: July 13, 1993
    Assignee: Pechiney Electrometallurgie
    Inventors: Alain Paret, Francois Peyron
  • Patent number: 5221527
    Abstract: For producing finely disperse aluminum nitride by reacting hydroxides of aluminum with carbon in a molar ratio of (1:1.5) to (1:2.5), the hydroxides of aluminum are intensively ground together with carbon, in particular carbon black, using a non-aqueous grinding fluid. After the non-aqueous grinding fluid has been separated off from the suspension, the ground material obtained is calcined at 400.degree. to 1000.degree. C., while passing nitrogen through. The material obtained is then treated under intensive contact with nitrogen for 1 to 100 hours at 1400.degree. to 1700.degree. C., before the excess carbon contained in the reaction product is removed by heating to 500.degree. to 900.degree. C. in contact with oxygen-containing gases.The hydroxides of aluminum and the carbon can also be intensively ground separately from one another, using a non-aqueous grinding fluid, and the suspensions obtained can be mixed.
    Type: Grant
    Filed: June 14, 1991
    Date of Patent: June 22, 1993
    Assignee: Hoechst Aktiengesellschaft
    Inventors: Friedrich-Wilhelm Dorn, Heinz Zschach
  • Patent number: 5219804
    Abstract: Rapidly heat powdered aluminum, an admixture of powdered aluminum and a compatible solid material, a powdered admixture of alumina and carbon, or aluminum nitride powder having a surface area lower than desired in the presence of a source of nitrogen at a temperature of 2473 to 3073K to produce aluminum nitride, then promptly quench the aluminum nitride product. The product has a surface area of greater than 10 m.sup.2 /g, preferably greater than 15 m.sup.2 /g.
    Type: Grant
    Filed: January 10, 1992
    Date of Patent: June 15, 1993
    Assignee: The Dow Chemical Company
    Inventors: Alan W. Weimer, Gene A. Cochran, John P. Henley, Glenn A. Eisman
  • Patent number: 5219539
    Abstract: A process for preparing fine aluminium nitride (AlN) powder is described using an inorganic flocculant based on polyaluminium chloride (PAC) having the following structural formula:Al.sub.n (OH).sub.m Cl.sub.3n-mwhere n and m are positive whole numbers and n is greater than m/3.
    Type: Grant
    Filed: October 15, 1991
    Date of Patent: June 15, 1993
    Assignee: Temav S.p.A.
    Inventors: Luigi Contursi, Giovanni Bezzi, Giordano Beghelli
  • Patent number: 5212125
    Abstract: A process for producing a sintered AlN ceramic body by mixing an organic solution comprising a hydrocarbon solvent and an organometallic compound with AlN powder to produce a slurry, removing the solvent from the slurry to form a mixture of organometallic compound and AlN, forming the mixture into a shape, and heating the shape in a non-oxidizing atmosphere to sintering temperature to obtain densification.
    Type: Grant
    Filed: November 20, 1990
    Date of Patent: May 18, 1993
    Assignee: The Carborundum Company
    Inventors: David D. Marchant, Joseph R. Fox, Timothy W. Brauneck
  • Patent number: 5204080
    Abstract: An aluminum nitride structure is prepared by placing an oxygen-trapping substance at at least one position on an aluminum nitride substrate having a first concentration of solution oxygen, and heating the resultant structure in a non-oxidizing atmosphere to locally reduce the first concentration of solution oxygen in said aluminum nitride substrate under said oxygen-trapping substance to a second concentration of solution oxygen by trapping the solution oxygen in the oxygen-trapping substance, thereby forming an aluminum nitride structure in which at least one region of the aluminum nitride structure corresponding to the position of said oxygen-trapping substance, which position has said second oxygen concentration, is integrally formed with aluminum nitride regions having said first concentration of solution oxygen. The aluminum nitride structure of the present invention exhibits anisotropic physical properties.
    Type: Grant
    Filed: June 29, 1990
    Date of Patent: April 20, 1993
    Assignee: Kabushiki Kaisha Toshiba
    Inventors: Mitsuo Kasori, Akihiro Horiguchi, Yoshiko Goto, Fumio Ueno
  • Patent number: 5190738
    Abstract: A process for producing unagglomerated single crystals of aluminum nitride of low oxygen content having a size of at least 10 microns suitable for the reinforcement of metal, ceramic and polymeric matrix composite materials, and especially metal matrix materials. The process involves producing a reaction mixture of alumina (or a precursor), carbon (or a precursor), and an alkali metal oxide (or precursor such as a carbonate) as a crystal growth promoter or catalyst. The alkali metal oxide is present in an amount required for the formation of crystals of the required size, preferably in the range of 10-60 microns. The reaction mixture is subjected to a preheating step under nitrogen at a temperature in the range of 1600.degree.-1700.degree. and is then subjected to a heating step under nitrogen at a temperature in the range of 1800.degree.-1950.degree. C. This two-stage heating process ensures that the resulting crystals are of low oxygen content and thus good thermal conductivity.
    Type: Grant
    Filed: June 17, 1991
    Date of Patent: March 2, 1993
    Assignee: Alcan International Limited
    Inventor: Luc Parent
  • Patent number: 5178844
    Abstract: A method and apparatus are provided for producing a product comprising a nitride compound, such as for example silicon nitride. A reactor is provided which has a chamber defined therein which is divided into a combustion zone and a reaction zone. A combustible mixture is injected into the combustion zone in a direction generally toward the reaction zone, and is accordingly combusted in the combustion zone. At least one reactant is injected at the boundary between the zones into the reactor chamber in a direction generally parallel to the longitudinal axis of the chamber so as to react to from raw product comprising the nitride compound. According to another aspect, a raw product powder as produced by the reactor comprises silicon nitride as the nitride compound and further comprises elemental silicon.
    Type: Grant
    Filed: April 3, 1990
    Date of Patent: January 12, 1993
    Assignee: Phillips Petroleum Company
    Inventors: Michael C. Carter, Bruce W. Gerhold
  • Patent number: 5174975
    Abstract: A process is provided for the preparation of metals, metal carbides, nitrides, borides, silicides, sulfides and phosphides by low temperature pyrolysis of a selected organometallic precursor. The precursor, in addition to containing organic ligands, contains the metal M, which is a transition metal or tin, and the element X (C, N, B, Si, S, or P), which may be bound directly to M, contained within the ligands, or both. The process enables one to provide surface coatings or shaped articles of metals, metal carbides, nitrides, and the like.
    Type: Grant
    Filed: November 13, 1989
    Date of Patent: December 29, 1992
    Assignee: SRI International
    Inventor: Richard M. Laine
  • Patent number: 5167944
    Abstract: An aluminum nitride-based sintered product can be produced at a relatively low heating temperature by mixing at least 20% by weight of ultrafine aluminum powder having an average size of not exceeding 0.5 .mu.m with other powdery raw material, compression molding the resultant powdery mixture, and heating the molded article under a nitrogen atmosphere at a heating temperature ranging from 600.degree. to 800.degree. C. to nitride the ultrafine aluminum powder, whereupon the heat of nitridation is utilized to sinter the molded article.
    Type: Grant
    Filed: October 17, 1991
    Date of Patent: December 1, 1992
    Assignee: Nisshin Steel Co., Ltd.
    Inventors: Masahiro Uda, Katsuhisa Ohsaki, Yoshikazu Morita
  • Patent number: 5164263
    Abstract: Methods are described for preparing aluminum nitride of controllable morphology for ceramic and heat conduction applications. The methods comprise forming spherical particles or flakes of an intermediate, RAlNH, followed by heating the spheres or flakes of RAlNH at elevated temperatures to produce high purity aluminum nitride of corresponding morphology. Spheres of RAlNH are formed by (i) freezing a suspension of RAlNH in a liquid medium and thawing, by (ii) aging the suspension, or by (iii) dissolving RAlNH in a liquid medium and precipitating it. Flakes are formed by freezing a suspension of RAlNH in a liquid medium and removing frozen medium from the frozen suspension.
    Type: Grant
    Filed: December 21, 1989
    Date of Patent: November 17, 1992
    Assignee: E. I. Du Pont de Nemours & Co.
    Inventors: John D. Bolt, Walter Mahler, Frederick N. Tebbe, Robert J. Young, Jr.
  • Patent number: 5154907
    Abstract: A process for the manufacture of high purity, ultra-fine aluminum nitride powder by the carbo-nitridization of alumina. Agglomerates uniform in both size, chemical composition and porosity are formed containing a stoichiometric mixture of alumina and carbon with the addition of a small amount of catalyst. The agglomerates are furnaced in a controlled manner in a well-mixed reaction vessel to achieve a uniform and consistent level of conversion. Milling of the as-reacted agglomerates under a controlled atmosphere will produce high purity, micron sized aluminum nitride powder.
    Type: Grant
    Filed: April 25, 1990
    Date of Patent: October 13, 1992
    Assignee: The Carborundum Company
    Inventors: Jonathan J. Kim, Viswanathan Venkateswaran, Joel D. Katz, Carl H. McMurtry, Ajit Y. Sane
  • Patent number: 5151260
    Abstract: Disclosed is a process for preparing fine powders of aluminum nitride, by starting from an aqueous solution of an inorganic aluminum salt, characterized in that said process comprises the following steps:(a) the anion of the inorganic salt of aluminum is at least partially removed by heating, with a colloidal solution of an aluminum compound being obtained;(b) carbon powder is dispersed in said colloidal solution, with a suspension of an aluminum compound and carbon being obtained;(c) said suspension is mixed with a carbohydrate, with a suspension being obtained of an aluminum compound and carbon in a solution which contains the carbohydrate;(d) the suspension obtained from the (c) step is sprayed onto, or dropwise added to, an alkaline solution, with spherical bodies being obtained, which contain aluminum hydroxide and carbon;(e) said spherical bodies are carbothermally reduced and nitrided at a temperature comprised within the range of from 1350.degree. to 1650.degree. C.
    Type: Grant
    Filed: December 19, 1990
    Date of Patent: September 29, 1992
    Assignee: Temay S.p.A.
    Inventors: Luigi Contursi, Leandro Beaulardi
  • Patent number: 5149514
    Abstract: A low temperature process is described for forming a coating or powder comprising one or more metals or metal compounds by first reacting one or more metal reactants with a halide-containing reactant to form one or more reactive intermediates capable of reacting, disproportionating, or decomposing to form a coating or powder comprising the one or more metal reactants. When one or more metal compounds are formed, either as powders or as coatings, a third reactant may be injected into a second reaction zone in the reactor to contact the one or more reactive intermediates formed in the first reaction zone to thereby form one or more metal compounds such as metal nitrides, carbides, oxides, borides, or mixtures of same.
    Type: Grant
    Filed: February 8, 1991
    Date of Patent: September 22, 1992
    Assignee: SRI International
    Inventor: Angel Sanjurjo
  • Patent number: 5149678
    Abstract: The present invention relates to a novel method of manufacturing a composite body, such as a ZrB.sub.2 -ZrC-Zr composite body, by utilizing a post-treatment technique which may improve the oxidation resistance of the composite body. Moreover, the invention relates to novel products made according to the process. The novel process modifies at least a portion of a composite body by exposing said body to a source of second metal.
    Type: Grant
    Filed: July 12, 1990
    Date of Patent: September 22, 1992
    Assignee: Lanxide Technology Company, LP
    Inventors: Terry D. Claar, William B. Johnson, Robert A. Rapp
  • Patent number: 5134102
    Abstract: Production of composite ceramic articles by infiltration of a particulate, permeable bed or permeable preform with a polycrystalline matrix produced as a metal-oxidant reaction product, wherein the bed or preform is comprised of dross.
    Type: Grant
    Filed: November 26, 1990
    Date of Patent: July 28, 1992
    Assignee: Lanxide Technology Company, LP
    Inventors: S. K. Nadkarni, Narasimha S. Raghavan
  • Patent number: 5126168
    Abstract: Lewis base-borane complexes such as (CH.sub.3).sub.2 S.BHBr.sub.2 are utilized as molecular precursors for the formation of both bulk powders, films and coatings of boron nitride. The complexes are subjected to slow heating under an ammonia atmosphere to displace the base and pyrolyze the resulting complex to BN. Analogous processes may be used to prepare Group IIIA-VA compounds of the formula MM' where M is selected from the group consisting of B, Al, Ga, In, and Tl, and M' is selected from the group consisting of N, P, As, Sb and Bi.
    Type: Grant
    Filed: February 1, 1989
    Date of Patent: June 30, 1992
    Assignee: The Trustees of the University of Pennsylvania
    Inventors: Larry G. Sneddon, Jeffrey Beck
  • Patent number: 5126121
    Abstract: Rapidly heat powdered aluminum in the presence of a source of nitrogen at a temperature of 1873 to 2373 K. to produce aluminum nitride, then promptly quench the aluminum nitride product. The product has a surface area between 2 and 8 square meters per gram and an oxygen content of less than 1.2 weight percent.
    Type: Grant
    Filed: May 3, 1991
    Date of Patent: June 30, 1992
    Assignee: The Dow Chemical Company
    Inventors: Alan W. Weimer, John P. Henley, Gene A. Cochran, Glenn A. Eisman, William G. Moore
  • Patent number: 5114695
    Abstract: A process of producing nitrides of aluminum and titanium. The process involves producing a uniform dispersion of microfine particles of the corresponding metal oxide in an infusible polymer, carbonizing the resulting dispersion in a non-oxidizing atmosphere and heating the carbonized product in a nitrogen atmosphere at high temperature to cause the oxide to react with the carbon and nitrogen to form the nitride. Before carbonization, however, the dispersion is formed into shapes in which none of the oxide particles is more than about 2.5 mm (0.098 inch) from an external surface and the shapes are loosely packed in a reactor. The process can achieve a good conversion of the oxide to the nitride to yield a product of high purity and small particle size.
    Type: Grant
    Filed: April 7, 1988
    Date of Patent: May 19, 1992
    Assignee: Alcon International Limited
    Inventors: Mukesh K. Jain, Sadashiv K. Nadkarni, Adam Gesing
  • Patent number: 5110575
    Abstract: Sinterable crystalline aluminum nitride powder is produced by reacting alkyl aluminum with ammonia in a gas phase to produce an amorphous aluminum nitride presursor powder, and subjecting the precursor powder to a primary calcination in a reducing gas containing at least 20% (vol.) ammonia at 600.degree. C. to 1300.degree. C., and then subjecting the calcined aluminum nitride to a secondary calination in an inert gas or a reducing gas at 1400.degree.-1750.degree. C.
    Type: Grant
    Filed: May 31, 1991
    Date of Patent: May 5, 1992
    Assignee: Mitsui Toatsu Chemicals, Inc.
    Inventors: Kazuo Wakimura, Masao Tanaka, Atsuhiko Hiai
  • Patent number: 5100846
    Abstract: A method is disclosed for purifying aluminum nitride produced by carbothermal reaction of aluminum oxide, carbon and nitrogen. Precursor pellets including aluminum oxide and carbon are exposed to nitrogen under conditions sufficient to carbothermally produce aluminum oxide, thereby producing aluminum nitride pellets having surface portions relatively rich in thermal conductivity-lowering and color-causing impurities compared to core portions of the aluminum nitride pellets. Significant amounts of the surface portions are thereafter removed to thereby significantly increase the purity of the aluminum nitride pellets.
    Type: Grant
    Filed: September 13, 1990
    Date of Patent: March 31, 1992
    Assignee: The Dow Chemical Company
    Inventors: David A. Dunn, James A. Hughes, Joyce A. Broka, Michael S. Paquette
  • Patent number: 5098870
    Abstract: This invention relates generally to a novel method of preparing self-supporting bodies and to the novel products made thereby. In its more specific aspects, this invention relates to a method of producing self-supporting bodies having controlled porosity and graded properties and comprising one or more boron-containing compounds, e.g., a boride or a boride and a carbide. The method comprises, in one embodiment, reacting a powdered parent metal, in molten form, with a bed or mass comprising a boron carbide material and, optionally, one or more inert fillers, to form the body. In another embodiment, both of a powdered parent metal and a body or pool of molten parent metal are induced to react with a bed or mass comprising a boron carbide material and, optionally, one or more inert fillers. in addition, combustible additives (e.g., gelatin, corn starch, wax, etc.) can be mixed with the bed or mass comprising a boron carbide material to aid in the porisity producing process.
    Type: Grant
    Filed: July 23, 1990
    Date of Patent: March 24, 1992
    Assignee: Lanxide Technology Company, LP
    Inventors: Terry D. Claar, William B. Johnson