Binary Compound (e.g., Silicide, Etc.) Patents (Class 423/344)
  • Patent number: 4399115
    Abstract: A process for synthesizing silicon nitride by reacting a silicon halide and ammonia at a high temperature, which is characterized in that at least while the reaction product is amorphous, hydrogen and chlorine are burned in the reaction zone where a halogen containing inorganic silicon compound and ammonia are reacting, and the reaction of said reactants is effected by the heat of combustion thus obtained.
    Type: Grant
    Filed: March 29, 1982
    Date of Patent: August 16, 1983
    Assignee: Asahi Glass Company Ltd.
    Inventors: Kimihiko Sato, Kunihiko Terase, Hitoshi Kijimuta
  • Patent number: 4397828
    Abstract: Stable, viscous polymers of silicon, nitrogen and hydrogen are formed by reacting a halosilane with ammonia in the presence of a solvent comprising an aliphatic ether, a chloromethane or mixtures thereof. After the solvent has been removed from the reaction product, the polymer can be poured into a container of desired shape and then can be sintered to form a uniform silicon nitride product.
    Type: Grant
    Filed: November 16, 1981
    Date of Patent: August 9, 1983
    Assignee: Massachusetts Institute of Technology
    Inventors: Dietmar Seyferth, Christian C. Prud'Homme, Gary H. Wiseman
  • Patent number: 4396587
    Abstract: Silicon nitride of improved quality is obtained by using a liquid silicic acid or modified liquid silicic acid as a silicic substance and carbon in a powdered form, a precursor of carbon in a powdered form, or a precursor of carbon in the form of a solution as a carbonaceous substance, and thermally treating these raw materials in a non-oxidative atmosphere containing nitrogen. By this method, .alpha.-type silicon nitride can be easily obtained. Particularly, finely divided .alpha.-type silicon nitride suitable for use as the raw material for the production of high-strength sintered articles is also produced. .alpha.-type silicon nitride whiskers useful as a reinforcing material for ceramic and metallic articles is also obtained.
    Type: Grant
    Filed: August 18, 1981
    Date of Patent: August 2, 1983
    Assignee: Asahi-Dow Limited
    Inventors: Masami Yamaguchi, Yoshirou Tajitsu, Yoshiharu Kitahama, Isamu Iwami
  • Patent number: 4387079
    Abstract: A method of manufacturing highly purified silicon nitride including the steps of preparing a nitrogen-containing silane selected from the group consisting of tetra-amide-monosilane and silicon imide, and heat-treating the prepared nitrogen-containing silane in the presence of ammonia in an inner atmosphere at a temperature above 400.degree. C. for a period of at least two hours to obtain silicon nitride, and cooling and collecting the silicon nitride thus formed. The step of preparing the nitrogen-containing silane comprises continuously reacting gaseous silicon tetra-chloride with gaseous ammonia in an inner atmosphere at a temperature of from -30.degree. to 70.degree. C. to produce the nitrogen-containing silane as a product and collecting the product. The resultant silicon nitride so produced has a chlorine content of less than 0.05 weight percent and a nitrogen content of over 38 weight percent.
    Type: Grant
    Filed: September 8, 1981
    Date of Patent: June 7, 1983
    Assignee: Toyo Soda Manufacturing Co., Ltd.
    Inventors: Kiyoshi Kasai, Kohji Tsukuma, Takaaki Tsukidate
  • Patent number: 4384909
    Abstract: Compositions are disclosed for securing Si.sub.3 N.sub.4 parts together, these compositions being in the .beta.'-Y.sub.2 Si.sub.2 O.sub.7 --Y.sub.3 Al.sub.5 O.sub.12 tetrahedron, e.g. compositions in mole % comprising (1) 15% Si.sub.3 N.sub.4, 79.1% Y.sub.2 Si.sub.2 O.sub.7 and 6.9% Y.sub.3 Al.sub.5 O.sub.12 or (2) 25% Si.sub.2 AlON.sub.3 and 75% Y.sub.3 Al.sub.5 O.sub.12 Y. A method of securing Si.sub.3 N.sub.4 parts together comprises placing the composition between the parts to be bonded and heating to brazing temperature (about 1600.degree. C.) in nitrogen.
    Type: Grant
    Filed: November 16, 1981
    Date of Patent: May 24, 1983
    Assignee: United Technologies Corporation
    Inventor: George K. Layden
  • Patent number: 4368180
    Abstract: A method for producing powder of a .alpha.-silicon nitride which comprises the steps of adding 0.1 to 2 parts by weight of carbon and 0.005 to 1 part by weight of at least one silicon compound selected from the group consisting of Si.sub.3 N.sub.4, SiC and Si.sub.2 ON.sub.2 to one part by weight, when converted to SiO.sub.2, of a liquid alkylchlorosilane that forms a precipitate and HCl by hydrolysis which precipitate is convertible to SiO.sub.2 at a baking temperature of 1300.degree. to 1550.degree. C., hydrolyzing the resultant mixture, washing the mixture to separate a solid component, and baking the solid component at a temperature of 1300.degree. to 1550.degree. C. in an atmosphere mainly consisting of a nitrogen gas or a gas of a nitrogen compound to effect formation of .alpha.-silicon nitride.
    Type: Grant
    Filed: August 17, 1981
    Date of Patent: January 11, 1983
    Assignee: Tokyo Shibaura Denki Kabushiki Kaisha
    Inventors: Hiroshi Inoue, Katsutoshi Komeya, Akihiko Tsuge
  • Patent number: 4352713
    Abstract: A vapor growth method of forming deposition film on a plurality of substrates disposed within a cylindrical reaction vessel by causing flow of reaction gas under a reduced pressure through the reaction vessel, in which the treated surfaces of substrates are inclined to the upstream side of the reaction gas flow with respect to the axis of the reaction vessel and the individual substrates but the most upstream side one are each shifted in position with respect to the preceding one in a direction perpendicular to the axis of the reaction vessel.
    Type: Grant
    Filed: November 7, 1980
    Date of Patent: October 5, 1982
    Assignee: Tokyo Shibaura Denki Kabushiki Kaisha
    Inventor: Shigeru Morita
  • Patent number: 4349636
    Abstract: A method for imparting ductility and very high electrical conductivity to very brittle refractory single crystals by subjecting said crystals to a hydrostatic deformation technique at room temperature and at pressures of from about 5 to 25 kilobars.
    Type: Grant
    Filed: May 14, 1981
    Date of Patent: September 14, 1982
    Inventor: Fred W. Vahldiek
  • Patent number: 4346068
    Abstract: High-purity .alpha.-type silicon nitride comprised of a granular crystal having an .alpha.-phase content of at least 95%, a nitrogen content of at least 38% by weight and an average particle size of not larger than 3 .mu.m is provided. This high-purity .alpha.-type silicon nitride is prepared by heating a nitrogen-containing silane compound at a temperature of at least about 1,300.degree. C. in a heating furnace comprised of a material containing a metal having a melting point exceeding 1,600.degree. C. and capable of being bonded with oxygen at the heating temperature.
    Type: Grant
    Filed: January 5, 1981
    Date of Patent: August 24, 1982
    Assignee: Toyo Soda Manufacturing Co., Ltd.
    Inventors: Kiyoshi Kasai, Yoshitaka Kubota, Takaaki Tsukidate
  • Patent number: 4331772
    Abstract: A method of manufacturing nitrided silicon parts by sintering a silicon powder containing aluminium under an atmosphere rich in nitrogen. A small quantity of carbon monoxide is added to the nitrogen atmosphere and the nitrogen and carbon monoxide partial pressures and the aluminium content of the silicon powder are chosen so that the oxidation reaction by the carbon monoxide on the nitrided silicon formed in the surfaces layers of the parts maintains therein an open porosity which is sufficient to allow the nitrogen to penetrate to the cores of the parts until the parts are homogeneously nitrided. Application to the manufacture of parts which must retain good mechanical strength at high temperature.
    Type: Grant
    Filed: October 17, 1980
    Date of Patent: May 25, 1982
    Assignee: Association pour la Recherche
    Inventors: Jean-Paul Torre, Joel Demit
  • Patent number: 4314956
    Abstract: Pre-polymers which are aminated methylpolysilanes are useful for the preparation of fine grained silicon carbide ceramic materials and silicon carbide-containing ceramics. The pre-polymers exhibit ease of handling and their use to obtain silicon carbide ceramic materials results in high yields.
    Type: Grant
    Filed: July 23, 1980
    Date of Patent: February 9, 1982
    Assignee: Dow Corning Corporation
    Inventors: Ronald H. Baney, John H. Gaul, Jr.
  • Patent number: 4310482
    Abstract: Novel, high yielding prepolymers are prepared by reducing chloropolysilanes with lithium aluminum hydride. These prepolymers exhibit good handling properties and are useful for preparing ceramics, silicon carbide ceramic materials and articles containing silicon carbide.
    Type: Grant
    Filed: July 23, 1980
    Date of Patent: January 12, 1982
    Assignee: Dow Corning Corporation
    Inventor: Ronald H. Baney
  • Patent number: 4298558
    Abstract: Pre-polymers which are alkoxylated or phenoxylated methylpolysilanes are useful for the preparation of fine grained silicon carbide ceramic materials and silicon carbide-containing ceramics. The pre-polymers exhibit ease of handling and their use to obtain silicon carbide ceramic materials results in high yields.
    Type: Grant
    Filed: July 23, 1980
    Date of Patent: November 3, 1981
    Assignee: Dow Corning Corporation
    Inventors: Ronald H. Baney, John H. Gaul, Jr.
  • Patent number: 4298559
    Abstract: Pre-polymers which are alkylated or arylated methylpolysilanes are useful for the preparation of silicon carbide ceramic materials. The pre-polymers exhibit ease of handling and their use to obtain silicon carbide ceramic materials results in high yields.
    Type: Grant
    Filed: July 23, 1980
    Date of Patent: November 3, 1981
    Assignee: Dow Corning Corporation
    Inventors: Ronald H. Baney, John H. Gaul, Jr.
  • Patent number: 4289801
    Abstract: Novel fine grained pyrolytic silicon nitride is produced by adding a substantial amount of methane to the normal reactant gases. Silicon tetrafluoride and ammonia in ratios of 60:40 to 10:90 may be employed with additions of methane in amounts equal to from 50 to 500% of the sum of silicon tetrafluoride and ammonia. When these reactant gases are passed over a heated substrate at a low pressure pyrolytic silicon nitride with a grain size of less than about 10 microns results.
    Type: Grant
    Filed: May 21, 1980
    Date of Patent: September 15, 1981
    Assignee: United Technologies Corporation
    Inventors: Francis S. Galasso, Malcolm Basche, deceased
  • Patent number: 4289952
    Abstract: Metal or ceramic powders having a narrow size distribution are produced by passing a gas entrained powder through an intense light beam which couples preferentially with the larger particles to heat and selectively vaporize a portion of the larger particles until their diameter approximates the desired size.
    Type: Grant
    Filed: December 12, 1979
    Date of Patent: September 15, 1981
    Assignee: Massachusetts Institute of Technology
    Inventor: John S. Haggerty
  • Patent number: 4284432
    Abstract: Ceramic powder material mainly consists of silicon nitride wherein the content of oxygen combined with generally unavoidable impurities as measured by activation analysis accounts for less than 2% by weight. The above-mentioned ceramic powder material can also be prepared preferably by the method which comprises the step of heating raw ceramic powder material mainly consisting of silicon nitride to 1,400.degree. C. to 1,900.degree. C. in the presence of a separately prepared nonsintered molding of ceramic material or sintered molding of ceramic material having a porosity of at least 10%.
    Type: Grant
    Filed: September 21, 1979
    Date of Patent: August 18, 1981
    Assignee: Tokyo Shibaura Electric Co. Ltd.
    Inventors: Katsutoshi Nishida, Michiyasu Komatsu, Tadashi Miyano
  • Patent number: 4280989
    Abstract: A method of producing silicon nitride which comprises heating silica in a gas atmosphere comprising hydrocarbon gas, ammonia gas and hydrogen gas.
    Type: Grant
    Filed: June 12, 1980
    Date of Patent: July 28, 1981
    Assignee: Tokyo Shibaura Denki Kabushiki Kaisha
    Inventors: Motoo Seimiya, Katsutoshi Nishida
  • Patent number: 4277320
    Abstract: A process for the direct thermal nitridation of silicon semiconductor devices in which the semiconductor body is placed in an atmosphere of N.sub.2, at a temperature of less than 1000.degree. C. The N.sub.2 is activated by an RF electrical field which ionizes the nitrogen, which then combines with the silicon surface.
    Type: Grant
    Filed: October 1, 1979
    Date of Patent: July 7, 1981
    Assignee: Rockwell International Corporation
    Inventors: Moiz M. E. Beguwala, Francis M. Erdmann
  • Patent number: 4264565
    Abstract: A method for producing powder of .alpha.-silicon nitride which comprises the steps of:adding 0.3 to 2 parts by weight of powder of carbon and 0.005 to 1 paret by weight of at least one silicon compound selected from the group consisting of Si.sub.3 N.sub.4, SiC and silicon oxide nitride series compounds to one part by weight (as converted to SiO.sub.2) to a liquid silane derivative which produces a precipitate and HCl by hydrolysis and further causes SiO.sub.2 to be grown by the baking of said precipitate, or the precipitate produced by hydrolysis of the liquid silane derivatives;hydrolyzing the resultant mixture, if necessary;washing the mixture to separate a solid component, if necessary; andbaking the solid component for reduction and nitrogenization at a temperature of 1300.degree. to 1500.degree. C. in an atmosphere mainly consisting of a nitrogen gas or a gas of a nitrogen compound.
    Type: Grant
    Filed: February 13, 1980
    Date of Patent: April 28, 1981
    Assignee: Tokyo Shibaura Denki Kabushiki Kaisha
    Inventors: Hiroshi Inoue, Katsutoshi Komeya, Akihiko Tsuge
  • Patent number: 4235857
    Abstract: A method of manufacturing silicon nitride particles, either in an aglomerated or unaglomerated form, is disclosed. Basically, the particles to be nitrided are placed in an enclosed furnace and heated to a suitable temperature at which the enclosed furnace is filled with an initial gaseous mixture of nitrogen and hydrogen, the mixture containing not more than about 6% by volume hydrogen. Thereafter, the material is heated in the enclosed furnace to a temperature of about 900.degree. C. to about 1000.degree. C. at which time the nitrogen starts to react with the silicon in the furnace. Thereafter, the enclosed furnace is demand filled with a nitriding gas mixture consisting essentially of 1 to 10% by volume helium and about 99 to 90% by volume nitrogen. The furnace is heated to a suitable nitriding temperature and the demand filling of the chamber with the nitriding gas helium/nitrogen combination is continued until the nitriding operation is terminated.
    Type: Grant
    Filed: July 2, 1979
    Date of Patent: November 25, 1980
    Assignee: Ford Motor Company
    Inventor: John A. Mangels
  • Patent number: 4224296
    Abstract: A super hard-highly pure silicon nitride includes a preferentially oriented crystalline silicon nitride having a grain size of 1-50 .mu.m and a micro Vickers hardness of 3,000 kg/mm.sup.2 under a load of 100 g, a finely grained crystalline silicon nitride having an average grain size of less than 1 .mu.m and a micro Vickers hardness of 3,500 kg/mm.sup.2 under a load of 100 g, and an amorphous silicon nitride having a micro Vickers hardness of 2,200 kg/mm.sup.2 under a load of 100 g, and is produced by blowing a nitrogen depositing source and a silicon depositing source on a substrate heated at 500.degree.-1,900.degree. C. with a blowpipe composed of a pipe assembly wherein a first pipe for the nitrogen depositing source is surrounded with a second pipe for the silicon depositing source and the distance from an opening end of the first pipe to the substrate is shorter than the distance from an opening end of the second pipe to the substrate.
    Type: Grant
    Filed: July 21, 1978
    Date of Patent: September 23, 1980
    Assignee: The Research Institute for Iron, Steel and Other Metals of the Tohoku University
    Inventors: Toshio Hirai, Koichi Niihara
  • Patent number: 4217470
    Abstract: To provide for better distributor radio interference noise suppression and to localize resistance elements used in connection therewith as close to the spark gap of the distributor, the rotor electrode and/or the stationary electrodes in the distributor are made of a resistance material which has a sufficiently high resistance to provide for effective interference suppression; the material may be a high-melting oxynitride, particularly of a metal of the III or IV-B to VI-B groups of the periodic table; or a ceramic substrate, on which a coating is applied, for example of high melting point titanium, zirconium or aluminum oxide which are rendered conductive by being present in less than stoichiometric proportions; or silicon compounds such as chromium-silicon compounds, molybdenum-silicon compounds, with or without a matrix of silicon or ceramic-metal mixture in which the metal is both a binder and a conductive component, particularly Al.sub.2 O.sub.3 -Mo, Cr.sub.2 O.sub.3 -Si, SiC-Cr-Ni and B.sub.4 C.sub.
    Type: Grant
    Filed: June 15, 1978
    Date of Patent: August 12, 1980
    Assignee: Robert Bosch GmbH
    Inventor: Kuno Kirner
  • Patent number: 4208215
    Abstract: High purity, fine Si.sub.3 N.sub.4 powder produced by the vapor phase reaction of SiCl.sub.4 with NH.sub.3 is amorphous. The crystallization rate of the amorphous powder is enhanced by heating the powder while in intimate contact with a titanium containing material, for example, TiN codeposited with the Si.sub.3 N.sub.4 by the simultaneous reaction of TiCl.sub.4 with NH.sub.3.
    Type: Grant
    Filed: September 18, 1978
    Date of Patent: June 17, 1980
    Assignee: GTE Service Corporation
    Inventors: Richard N. Kleiner, Emil J. Mehalchick
  • Patent number: 4206190
    Abstract: This is a method of producing silicon nitride in a plasma arc furnace utilizing silicon metal or silicon dioxide as a starting material. When silicon metal is used it is reacted directly with a nitrogen bearing gas to produce silicon nitride. When silicon dioxide is used a two-step process is performed wherein the silicon dioxide is first reacted with hydrogen to produce silicon monoxide gas and water and thereafter the silicon monoxide gas is reacted with hydrogen and nitrogen to produce silicon nitride and water.
    Type: Grant
    Filed: March 11, 1974
    Date of Patent: June 3, 1980
    Assignee: Westinghouse Electric Corp.
    Inventors: Francis J. Harvey, II, Raymond J. Bratton
  • Patent number: 4196178
    Abstract: Fine metallic nitride powders having a high purity are prepared, without causing any plugging or other problems in the reaction apparatus and with easy heat control of the reaction, by reacting a metallic halide with liquid ammonia in the presence of an organic solvent which has a specific gravity higher than that of liquid ammonia, and also is not miscible or is only slightly miscible with liquid ammonia at a reaction temperature. The process according to the present invention is effected by introducing the metallic halide into the lower organic solvent layer of the reaction system.
    Type: Grant
    Filed: April 6, 1979
    Date of Patent: April 1, 1980
    Assignee: Ube Industries, Ltd.
    Inventors: Tadashi Iwai, Takashi Kawahito, Tetsuo Yamada
  • Patent number: 4181751
    Abstract: Low temperature photonitride (LTPN) films of excellent quality have been prepared at temperatures ranging from 300.degree. C. downward to 100.degree. C. by a photochemical vapor deposition process, wherein a mixture of silane, ammonia, and hydrazine is caused to react to form Si.sub.3 N.sub.4 films at the substrate interface. These films are suitable for the preparation of silicon nitride passivation layers on solid-state devices, such as metal-oxide semiconductors (MOS) and charge coupled devices to impart enhanced reliability.
    Type: Grant
    Filed: May 24, 1978
    Date of Patent: January 1, 1980
    Assignee: Hughes Aircraft Company
    Inventors: Thomas C. Hall, John W. Peters
  • Patent number: 4177230
    Abstract: Porous reaction sintered silicon nitride body is infiltrated with an organosilicon compound after which the body is heated at a temperature sufficient to decompose the infiltrated material, resulting in a silicon nitride body having an increased density and significantly improved room temperature strength.
    Type: Grant
    Filed: June 2, 1978
    Date of Patent: December 4, 1979
    Assignee: The United States of America as represented by the Secretary of the Air Force
    Inventor: Khodabakhsh S. Mazdiyasni
  • Patent number: 4164553
    Abstract: A plasma-arc process is disclosed for the production of powders of various chemical products, according to endothermic reactions, such as TiC and the like. The process consists essentially in carrying out, in a furnace with an anodic function without dissipative cooling, a series of steps comprising:(a) forming a chemically reactive fluidodynamic mass having a high thermal content and a high concentration of the desired reactive species, by injecting into the electronic column of a plasma-arc of a noble gas at least one reactant selected from the class consisting of metal and metalloid halides, the injection taking place, with mixing through a choker-injector-mixer nozzle which is electrically insulated;(b) causing the electronic condensation of said mass inside a main nozzle anode without dissipative cooling; and(c) injecting into said electronically condensed mass the residual part of said reactants necessary to the desired main chemical reaction for producing the chemical powder.
    Type: Grant
    Filed: February 14, 1977
    Date of Patent: August 14, 1979
    Assignee: Montedison S.p.A.
    Inventors: Giancarlo Perugini, Enzo Marcaccioli
  • Patent number: 4156051
    Abstract: Composite ceramic articles formed by integrally assembling a plurality of previously molded constituent members without applying an adhesive to their joints and designed to have a density than higher 98% of the theoretical value, and a flexural strength greater than 50 kg/cm.sup.2 at 1200.degree. C., and a method of producing ceramic articles of particularly complicated shape which comprises the steps of previously molding a plurality of constituent members of complicated shape and later integrally assembling said constituent members without applying an adhesive to their joints.
    Type: Grant
    Filed: September 5, 1978
    Date of Patent: May 22, 1979
    Assignee: Tokyo Shibaura Electric Co., Ltd.
    Inventors: Kiyoshi Nakamura, Takashi Ishii, Michiyasu Komatsu, Tadashi Miyano, Masae Nakanishi
  • Patent number: 4150999
    Abstract: Method for the manufacture of ferrosilicon nitride is disclosed. The method produces ferrosilicon nitride with a silicon nitride content of 65% to 85% by weight by oxidizing the metallic iron which is present in the ferrosilicon nitride in an aqueous medium in the presence of selected oxidizing agents while forcing a mixture of air and steam through the aqueous medium.
    Type: Grant
    Filed: June 1, 1978
    Date of Patent: April 24, 1979
    Assignee: Denki Kagaku Kogyo Kabushiki Kaisha
    Inventor: Sadayuki Iwamoto
  • Patent number: 4145224
    Abstract: High purity, fine Si.sub.3 N.sub.4 powder produced by the vapor phase reaction of SiCl.sub.4 with NH.sub.3 is amorphous. The crystallization rate of the amorphous powder is enhanced by heating the powder while in intimate contact with a titanium containing material, for example, TiN codeposited with the Si.sub.3 N.sub.4 by the simultaneous reaction of TiCl.sub.4 with NH.sub.3.
    Type: Grant
    Filed: November 22, 1974
    Date of Patent: March 20, 1979
    Assignee: GTE Sylvania Incorporated
    Inventors: Emil J. Mehalchick, Richard N. Kleiner
  • Patent number: 4125592
    Abstract: A method for forming a silicon nitride article is set forth. An article having silicon particles therein is formed in a manner which provides a degree of porosity for the article. The silicon particles of the article are reactable with nitrogen to form silicon nitride. The article is heated to a temperature below a significant reaction temperature at which nitrogen gas reacts with the silicon particles at a measurable rate. The article is surrounded with an atmosphere containing nitrogen gas. A reaction zone is established on at least a portion of the surface area of the article. The reaction zone has a temperature above the significant reaction temperature whereby the silicon particles in the reaction zone are reacted at a measurable rate with the nitrogen gas to form silicon nitride. The reaction zone is moved in a controlled manner from the surface of the article into the interior of the article whereby the article is progressively nitrided inwardly into its bulk from the surface thereof.
    Type: Grant
    Filed: December 9, 1977
    Date of Patent: November 14, 1978
    Assignee: Ford Motor Company
    Inventors: Andre Ezis, John J. Schuldies
  • Patent number: 4122155
    Abstract: A gas mixture of silane and ammonia is heated at temperatures between about 600.degree. C and 1000.degree. C producing an amorphous powdery reaction product which, when heated at a calcination temperature of at least 1100.degree. C yields ultrafine Si.sub.3 N.sub.4 powder of high purity.
    Type: Grant
    Filed: January 3, 1977
    Date of Patent: October 24, 1978
    Assignee: General Electric Company
    Inventors: Svante Prochazka, Charles D. Greskovich
  • Patent number: 4122152
    Abstract: A process for preparing silicon nitride powder having a high .alpha.-phase content which comprises the steps of (a) providing a blended powder material composed of silica powder and amorphous carbon powder having an oil absorption of not less than 100 ml/100g, the weight ratio of the carbon powder to the silica powder being not less than 0.5, and then (b) nitriding and burning the blended powder material by heating in at a temperature of from 1300.degree. to 1700.degree. C while feeding a nitrogen-containing, non-oxidizing gas. The product obtained by this process is suitable as a raw material for the manufacture of high-density and high-strength sintered articles of silicon nitride.
    Type: Grant
    Filed: January 27, 1977
    Date of Patent: October 24, 1978
    Assignee: Toshiba Ceramics Co., Ltd.
    Inventors: Masaaki Mori, Norihira Takai
  • Patent number: 4122220
    Abstract: Silicon nitride bodies are improved by being impregnated with a silicon halide which is then converted to silicon imide in the pores of the body, which, in turn, is converted into silicon nitride.
    Type: Grant
    Filed: September 6, 1977
    Date of Patent: October 24, 1978
    Assignee: Rosenthal Aktiengesellschaft
    Inventor: Godehard Sussmuth
  • Patent number: 4117095
    Abstract: .alpha.-Silicon nitride powder which is used as a raw material for the preparation of high strength silicon nitride with additives such as magnesia and yttrium oxide, and other sintered materials suitable for high temperature gas turbine engine components and the like, is prepared by heating a powdered mixture of silica, carbon and metallic silicon in a nitrogen containing atmosphere and then subjecting the material to a heat treatment in an oxidizing atmosphere for decarbonization of said material.
    Type: Grant
    Filed: September 22, 1976
    Date of Patent: September 26, 1978
    Assignee: Tokyo Shibaura Electric Co., Ltd.
    Inventors: Katsutoshi Komeya, Hiroshi Inoue, Takao Ohta
  • Patent number: 4101616
    Abstract: Si.sub.3 N.sub.4 fibrous articles are produced by forming a low density compact of amorphous Si.sub.3 N.sub.4 powder and heat treating the compact to promote in-situ formation of fibrous crystalline alpha Si.sub.3 N.sub.4. Such articles are useful as thermal insulants, packing materials, resilient seals, etc.
    Type: Grant
    Filed: March 23, 1977
    Date of Patent: July 18, 1978
    Assignee: GTE Sylvania Incorporated
    Inventor: Sergei-Tomislav Buljan
  • Patent number: 4073845
    Abstract: Si.sub.3 N.sub.4 ceramics exhibiting densities and modulus of rupture values heretofore obtainable only by hot pressing are produced by pressureless sintering of powder compacts of partly amorphours, partly crystalline Si.sub.3 N.sub.4 powder containing between 5 and 60 percent by weight of crystalline material.
    Type: Grant
    Filed: January 29, 1976
    Date of Patent: February 14, 1978
    Assignee: GTE Sylvania Incorporated
    Inventors: Sergej T. Buljan, Philip E. Stermer
  • Patent number: 4040848
    Abstract: A polycrystalline silicon body is produced by forming a particulate mixture of silicon powder having an average particle size less than 3 microns and boron in an amount ranging from 0.1% to 5% by weight of the silicon powder, shaping the particulate mixture into a green body and sintering the body to a density of at least 60% of the theoretical density of silicon.
    Type: Grant
    Filed: January 6, 1976
    Date of Patent: August 9, 1977
    Assignee: General Electric Company
    Inventors: Charles D. Greskovich, Joseph H. Rosolowski
  • Patent number: 4036653
    Abstract: An amorphous silicon nitride composition consisting essentially of from 95.0% to 99.9% by weight of amorphous silicon nitride and from 0.1% to 5.0% of carbon prepared by the vapor phase reaction of silicon tetrachloride, ammonia, and a gaseous hydrocarbon at temperatures from 1000.degree.C. to 1500.degree.C. This composition is particularly useful in the preparation of fully dense ceramics requiring high strength at elevated temperatures.
    Type: Grant
    Filed: May 28, 1975
    Date of Patent: July 19, 1977
    Assignee: E. I. Du Pont de Nemours and Company
    Inventor: Howard Wayne Jacobson
  • Patent number: 4022872
    Abstract: Helical flow of hot plasma gas, e.g., hydrogen gas, produced by a gas vortex stabilized plasma arc is cancelled by introducing attenuating gas, e.g., hydrogen gas, into the hot plasma gas in a manner such that the attenuating gas assumes a vortical direction opposite to the helical flow of the hot plasma gas. The resulting gas stream is well-collimated. The well-collimated plasma gas stream is used in the preparation of finely-divided refractory metal and metalloid carbides, borides, nitrides, silicides and sulfides. Reactants for the preparation of the aforementioned refractory powders are introduced into the collimated plasma gas stream. The reaction is conducted in the gas phase within a reactor and solid, finely-divided refractory powder removed from the reactor.
    Type: Grant
    Filed: November 12, 1975
    Date of Patent: May 10, 1977
    Assignee: PPG Industries, Inc.
    Inventors: Donald R. Carson, Calvin B. Holden
  • Patent number: 3983198
    Abstract: A method of increasing the oxidation resistance of silicon nitride is disclosed. A furnace is preheated to a temperature in the range of 2500.degree.F to 2750.degree.F. The silicon nitride body to be treated is inserted into the preheated furnace. The silicon nitride article is maintained in the furance for a period of time sufficient to develop an oxidation resistant surface on the article. The period of time is generally in the range from one-half hour to five hours.
    Type: Grant
    Filed: February 12, 1975
    Date of Patent: September 28, 1976
    Assignee: Ford Motor Company
    Inventor: John A. Mangels
  • Patent number: 3979500
    Abstract: The preparation of metal and metalloid carbides, borides, nitrides silicides and sulfides by reaction in the vapor phase of the corresponding vaporous metal halide, e.g., metal chloride, with a source of carbon, boron, nitrogen, silicon or sulfur respectively in a reactor is described. Reactants can be introduced into the reactor through a reactant inlet nozzle assembly. Inhibition and often substantial elimination of product growth on exposed surfaces of such assembly is accomplished by introducing the corresponding substantially anhydrous hydrogen halide, e.g., hydrogen chloride, into the principal reactant mixing zone.
    Type: Grant
    Filed: May 12, 1975
    Date of Patent: September 7, 1976
    Assignee: PPG Industries, Inc.
    Inventors: Robert S. Sheppard, Franklin E. Groening
  • Patent number: 3966885
    Abstract: This invention is concerned with methods and materials for producing unitary silicon nitride structures by means of joining together at least two silicon based bodies with an intervening mixture of silicon powder and a heat removable liquid binder therefor between the joining faces, mantaining said faces in juxtaposition and slowly heating the assembly in a nitriding atmosphere to remove the liquid binder and to convert the material of said bodies and the intervening silicon powder into a unitary structure.
    Type: Grant
    Filed: March 3, 1975
    Date of Patent: June 29, 1976
    Assignee: National Research Development Corporation
    Inventor: Edwin Richard Wells May
  • Patent number: 3959446
    Abstract: A method is provided for preparing alpha silicon nitride powder in which very high purity, liquid silicon tetrachloride is reacted with an excess of ammonia gas in dry deoxygenated benzene or normal hexane at about 0.degree.C, yielding a precipitate of silicon diimide and ammonium chloride. After removal of the benzene or n-hexane from the precipitate, the mixture of silicon diimide and ammonium chloride powder is heated under a vacuum from room temperature to a temperature in the range of 1200.degree. to 1350.degree.C and maintained at the latter temperature for a period of about 2 to 8 hours. The product obtained is a high purity, submicron, alpha phase silicon nitride powder which is eminently suitable for the fabrication of dense, high strength, creep resistant and thermal shock resistant bodies for use in high performance gas turbine engines and in radome applications.
    Type: Grant
    Filed: March 1, 1974
    Date of Patent: May 25, 1976
    Assignee: The United States of America as represented by the Secretary of the Air Force
    Inventors: Khodabakhsh S. Mazdiyasni, Charles M. Cooke
  • Patent number: 3953579
    Abstract: A method is provided for making reactive metal silicide, particularly for use in adding lanthanum or other reactive metals to metal melts, by reacting reactive metal oxide with a metal silicide or silicon in an ESR furnace.
    Type: Grant
    Filed: July 2, 1974
    Date of Patent: April 27, 1976
    Assignee: Cabot Corporation
    Inventor: Robert B. Herchenroeder
  • Patent number: 3937792
    Abstract: A method of manufacturing a silicon nitride powder comprises heating a bed of silicon powder in a furnace having an atmosphere containing nitrogen so that the silicon reacts with the nitrogen to produce silicon nitride. The exothermic reaction between the silicon and the nitrogen is monitored, either by comparing the temperature in the reaction bed with the temperature at another point in the furnace, or by allowing the nitrogen containing atmosphere to flow through the furnace and measuring the rates of flow of the atmosphere into and out of the furnace. The partial pressure of the nitrogen in the furnace atmosphere is then controlled in accordance with the exothermic reaction so as to ensure that the temperature in the bed does not exceed a predetermined value above which .beta.-phase silicon nitride is formed, the partial pressure of the nitrogen in the furnace being controlled by effecting at least one of the steps of:A. diluting the nitrogen in the furnace atmosphere and,B. evacuating the furnace.
    Type: Grant
    Filed: March 14, 1972
    Date of Patent: February 10, 1976
    Assignee: Joseph Lucas (Industries) Limited
    Inventor: Roland John Lumby