From Inorganic Salt Precursors (e.g., Nitrates) Patents (Class 505/737)
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Patent number: 5077267Abstract: A process for forming a composite high temperature superconductor copper wire, said process comprising the steps of (1) directing a submicron sized powder of a superconducting ceramic material through a length of copper tubing to coat the interior surface of said tubing with a uniform compact film of said powder, and (2) sintering said powder while passing oxygen through said tube and while maintaining the outside of said tube in an inert atmosphere. In a preferred embodiment an aerosol process is used to generate the submicron sized powder of the superconductor.Type: GrantFiled: July 12, 1988Date of Patent: December 31, 1991Assignee: International Business Machines CorporationInventors: Edward M. Engler, Toivo T. Kodas, Victor Y. Lee
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Patent number: 5071827Abstract: Finely divided, homogeneous and easily sintered superconducting powders of at least one rare earth element, e.g., yttrium and/or lanthanum, at least one alkaline earth metal, e.g., barium, calcium and/or strontium, and at least one transition metal, e.g., copper, nickel, manganese, cobalt and/or iron, and oxygen, are produced by (a) intimately admixing a sol of a rare earth element and an aqueous solution of at least one alkaline earth metal nitrate and of at least one nitrate of a transition metal, with the pH of the resulting mixture being adjusted to a value such that said nitrates remain solubilized therein; (b) drying the resulting mixture; (c) calcining the dried product; and, optionally; (d) grinding the calcined material.Type: GrantFiled: September 19, 1988Date of Patent: December 10, 1991Assignee: Rhone-Poulenc ChimieInventors: Marie-Odile Lafon, Claude Magnier
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Patent number: 5071829Abstract: This invention describes the way to prepare high purity Bi-based superconducting powders with the zero resistance temperature at 110K. The technique employs the dissolution of corresponding metal nitrates in deionized water, plus oxalic acid to chelate the metal cations. The amount of oxalic acid equals to about half of the total nitrate anion in molar ratio. After pH adjustment and gelation, optimal calcination results in 110K superconducting powders in high purity.Type: GrantFiled: June 27, 1990Date of Patent: December 10, 1991Assignee: Industrial Technology Research InstituteInventors: Chung K. Chiang, Cheng Y. Shei, Yao T. Huang
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Patent number: 5066636Abstract: A citrate/ethylenediamine gel method for forming oxide superconductors of the Y-Ba-Cu-O, Bi-Ca-Sr-Cu-O, Tl-Ca-Ba-Cu-O system by employing the nitrates of the individual metals and citric acid. Ethylenediamine is then added to form gels. These materials then undergo calcination and sintering processes. The respective superconductors obtained possess a superconducting zero resistance temperature at 93K, 78K and 118K respectively.Type: GrantFiled: August 15, 1990Date of Patent: November 19, 1991Assignee: Industrial Technology Research InstituteInventors: Ru-Shi Liu, Wang-Nang Wang, Chan-Ting Chang
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Patent number: 5064808Abstract: The invention relates to production of superconductors, more particularly, LnM.sub.2.sup.II M.sub.3.sup.I O.sub.y compounds where y=6-8; Ln=Y, Sc or lanthanide; M.sup.II =Ba, Ca or Sr; M.sup.I =Cu, Cu+Ag or LnM.sub.2.sup.II M.sup.I O.sub.y-x F where x=1-2. It comprises local initiation of an exothermic reaction in a stoichiometric mixutre of source constituents chosen to provide for production of the afore-mentioned compounds. An exothermic mixture of corresponding constituents includes a non-combustible component and a combustible component comprising at least one metal from the group composed of a rare-earth metal of the periodic system chosen from scandium, yttrium and lanthanide, a metal of group II of the periodic system, a metal of group I of the periodic system or hydride of at least one of said metals.Type: GrantFiled: November 22, 1989Date of Patent: November 12, 1991Assignee: Institut Strukturnoi Makrokinetiki an SSSRInventors: Alexandr G. Merzhanov, Inna P. Borovinskaya, Mikael D. Nersesian, Andrei G. Peresada
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Patent number: 5063199Abstract: This invention provides a method for depositiing a superconducting thin film comprising at least one high temperature Bi-Sr-Ca-Cu-O-based superconductor phase onto a substrate such as, for example, a ceramic oxide or a metal. High temperature Bi-Sr-Ca-Cu-O-based superconductor phases include Bi.sub.2 Sr.sub.2 CaCu.sub.2 O.sub.8, Bi.sub.4 Sr.sub.3 Ca.sub.3 Cu.sub.4 O.sub.16, and Bi.sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.10.Type: GrantFiled: June 15, 1990Date of Patent: November 5, 1991Assignee: Minnesota Mining and Manufacturing CompanyInventor: Kenton D. Budd
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Patent number: 5061683Abstract: There is disclosed an improved process for preparing a superconducting composition having the formula M.sub.w A.sub.z Cu.sub.v O.sub.x wherein M is selected from the group consisting if Bi, Tl, Y, Nd, Sm, Eu, Gd, Dy, Ho, Er, Tm Yb and Lu; A is at least one alkaline earth metal selected from the group consisting of Ba, Ca and Sr; x is at least 6; w is at least 1; z is at least 2 and v is at least 1; said composition having a superconducting transition temperature of above 77 K, preferably above about 90 K; said process consisting essentially of (a) forming a suspension having an M:A:Cu atomic ratio of w:z:v by mixing A(OH).sub.2, AO or AO.sub.2 and M.sub.2 O.sub.3 with an aqueous solution of cupric carboxylate or cupric nitrate at a temperature from about 50.degree. C. to about 100.degree. C., or mixing A(OH).sub.2 with an aqueous solution of Cu carboxylate, nitrate or a mixture thereof and M carboxylate, nitrate or a mixture thereof at a temperature from about 50.degree. C. to about 100.degree. C.Type: GrantFiled: May 31, 1988Date of Patent: October 29, 1991Assignee: E. I. Du Pont de Nemours and CompanyInventor: Harold S. Horowitz
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Patent number: 5061682Abstract: Ceramic precursor mixtures containing a metal cation, a carbohydrate, and an anion capable of participating in an anionic oxidation-reduction reaction with the carbohydrate for continuous or batchwise drying and pyrolyzing to provide ceramic powders.Type: GrantFiled: January 17, 1990Date of Patent: October 29, 1991Assignee: The Washington Technology CenterInventors: Ilhan A. Aksay, Chan Han, Gary D. Maupin, Corrie B. Martin, Randal P. Kurosky, Gregory C. Stangle
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Patent number: 5055436Abstract: An improved process for preparing superconducting ceramic powder includes calcining superconducting precursor compounds in an atmosphere having a controlled amount of oxygen, generally not more than that found in air, the remainder of the atmosphere composed of a gas or mixture of gases inert with respect to the ceramic. A preferred process includes forming the precursor compounds into a slurry, granulating the slurry, drying the granules (a binder can be added to the slurry to promote green strength), and calcining in the controlled atmosphere to provide the desired HTSC (high temperature superconductor) composition.Type: GrantFiled: August 19, 1988Date of Patent: October 8, 1991Assignee: CPS Superconductor Corp.Inventors: Lori J. Klemptner, James D. Hodge, John W. Halloran
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Patent number: 5034372Abstract: An improved method for producing superconductive oxide substance, wherein a solution containing therein a plurality of elements to constitute the superconductive oxide substance is atomized into mists, then the thus atomized mists are transported on a carrier gas into a chemical reaction device, and, after the chemical reaction in this chemical reaction device, the superconductive oxide substance is deposited on a substrate in a desired shape, with further heat-treatment of the thus deposited superconductive oxide substance in an oxygen-containing atmosphere at a temperature ranging from 200.degree. C. to 1,200.degree. C.Type: GrantFiled: December 7, 1988Date of Patent: July 23, 1991Assignee: Mitsubishi Denki Kabushiki KaishaInventors: Shigeru Matsuno, Yoshio Kubo, Kiyoshi Yoshizaki, Mitsunobu Wakata, Syouji Miyashita, Fumio Fujiwara
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Patent number: 5032568Abstract: A method is provided to apply a coating of a superconducting ceramic oxide to a substrate comprising introducing an atomized aqueous solution comprising at least three metal salts into inductively coupled plasma so as to deposit a superconductive ceramic oxide on the substrate, or alternatively, to deposit a mixed metal oxide on the substrate, which is converted into a superconductive ceramic oxide by post-annealing.Type: GrantFiled: September 1, 1989Date of Patent: July 16, 1991Assignee: Regents of the University of MinnesotaInventors: Yuk-Chiu Lau, Emil Pfender
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Patent number: 5021399Abstract: An improved method for preparing high temperature Bi-Sr-Ca-Cu-O superconductive films utilizing spray pyrolysis. The method can further include an additional annealing step to improve the electrical transport properties.Type: GrantFiled: March 10, 1989Date of Patent: June 4, 1991Assignee: Microelectronics & Computer Technology Corp.Inventors: Hsyh-Min Hsu, Ian Y. K. Yee
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Patent number: 5021395Abstract: A process for preparing the superconductive material MBa.sub.2 Cu.sub.3 O.sub.x, M being, inter alia, yttrium and x being from about 6.5-7 and a precursor material MBa.sub.2 Cu.sub.3 O.sub.y, y being from about 6-6.5, by controlled heating and cooling in a controlled atmosphere.Type: GrantFiled: June 28, 1989Date of Patent: June 4, 1991Assignee: E. I. Du Pont de Nemours and CompanyInventors: Joe D. Druliner, Harold S. Horowitz, Stephan J. McLain, Arthur W. Sleight
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Patent number: 5021400Abstract: Improved process for making Tl-Ca-Ba-CuO superconductors. A solution of the monocarboxylates (e.g., acetates) of Ca, Ba, and Cu is dried, calcined, mixed with Tl.sub.2 O.sub.3, and the mixture is heated to make a superconductor. The method minimizes introduction of contaminants. Novel compositions result.Type: GrantFiled: October 17, 1989Date of Patent: June 4, 1991Assignee: W. R. Grace & Co.-Conn.Inventors: Jacob Block, Leonard E. Dolhert
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Patent number: 5002928Abstract: A thin film of a superconductor comprising composite metal oxides is formed by atomizing and spraying a homogeneous solution or solutions containing as solutes one or more of metal compounds capable of forming the superconductor, with an ultrasonic wave sprayer, onto a hot substrate to form the thin film, and the ultrasonic wave sprayer for forming the thin film of the superconductor comprises an ultrasonic wave-generating vibrator, feedstock supplier, atomized solution-escaping inhibitor, substrate supporter and heater, the ultrasonic wave-generating vibrator being connected through an axis to a solution-atomizing nozzle.Type: GrantFiled: November 9, 1989Date of Patent: March 26, 1991Assignee: TOA Nenryo Kogyo Kabushiki KaishaInventors: Keitaro Fukui, Osamu Nakamura, Yasushi Okayama, Atsushi Tsunoda
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Patent number: 5001107Abstract: This invention provides improved methods for the preparation of precursor powders that are used in the preparation of superconducting ceramic materials that contain thallium. A first solution that contains the hydrogen peroxide and metal cations, other than thallium, that will be part of the ceramic is quickly mixed with a second solution that contains precipitating anions and thallium (I) to form a precipitate which is dried to yield precursor powders. The precursor powders are calcined an sintered to produce superconducting materials that contain thallium.Type: GrantFiled: August 2, 1989Date of Patent: March 19, 1991Assignee: The United States Department of EnergyInventors: Bruce C. Bunker, Diana L. Lamppa, James A. Voigt
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Patent number: 4997809Abstract: A method for producing a patterned layer of high T.sub.c oxide superconductor is provided in which patterning is accomplished prior to the attainment of a superconducting state in the layer. A solution containing precursor components of the desired oxide superconductor is sprayed onto a substrate and dried to provide a layer thereon. This layer is then irradiated in selected areas to convert the irradiated layers to an intermediate oxide state, the nonirradiated areas being unchanged. The nonirradiated areas are then dissolved away, leaving a pattern of oxide material. This oxide material is then converted to a high T.sub.c superconducting state, as by annealing in an oxygen atmosphere. This provides the patterned layer of high T.sub.c oxide superconductor. An example of a such a superconductor is a mixed copper oxide, such as Y.sub.1 Ba.sub.2 Cu.sub.3 O.sub.7-x.Type: GrantFiled: November 18, 1987Date of Patent: March 5, 1991Assignee: International Business Machines CorporationInventor: Arunava Gupta
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Patent number: 4996189Abstract: A novel method of producing mixed metal oxide powder (e.g., ferrite powder, or high temperature superconductor powder such as YBa.sub.2 Cu.sub.3 O.sub.x powder) is disclosed. The method comprises forming an intimate mixture of appropriate metal salts (e.g., nitrates and acetates), at least one of which is an oxidizing agent with respect to at least one of the others, and heating the mixture to a reaction temperature such that an exothermic redox reaction occurs. Appropriate choice of oxidizing and reducing agents permits control of heat of reaction and reaction temperature. The product of the reaction typically is a precursor of the desired mixed oxide, the precursor typically consisting essentially of the metal constituents of the mixed oxide and oxygen. Heat treatment in an O.sub.2 -containing atmosphere transforms the precursor into the desired mixed oxide powder. The thus produced powder can then be used in conventional fashion, e.g., to produce bodies therefrom by pressing and/or sintering.Type: GrantFiled: October 24, 1988Date of Patent: February 26, 1991Assignee: AT&T Bell LaboratoriesInventors: Kostantinos Kourtakis, Murray Robbins
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Patent number: 4994420Abstract: The specification discloses forming ceramic films, and especially high temperature superconductor films, by dissolving ceramic precursor metal iodides in organic solvents, applying them to a substrate, evaporating the solvent and pyrolyzing and annealing the resulting ceramic precursor metal iodide films.Type: GrantFiled: October 12, 1989Date of Patent: February 19, 1991Assignee: Dow Corning CorporationInventors: Ronald H. Baney, Debora F. Bergstrom, Bruce H. Justice
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Patent number: 4994433Abstract: Cations such as La, Sr, Cu, or Y, Ba, Cu are dissolved in an organic solvent such as ethylene glycol and citric acid. The solution is formed into either a free-standing or supported film which is dried to produce a solid organic polymer. The polymer is then fired in an oxidizing atmosphere (pyrolysis) to obtain the superconducting oxide. It is preferred that the film be spin coated on a substrate to produce uniform coatings of thicknesses less than one micrometer. The resulting superconducting oxide film is fully dense, of controlled microstructure, very monogeneous in composition and suitable for demanding electronic device purposes or as coatings to form superconducting wires or other current carrying components.Type: GrantFiled: May 22, 1987Date of Patent: February 19, 1991Assignee: Massachusetts Institute of TechnologyInventor: Yet-Ming Chiang
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Patent number: 4983573Abstract: There is disclosed an improved process for preparing a superconducting composition having the formula MBa.sub.2 Cu.sub.3 O.sub.x wherein M is selected from the group consisting of Y, Nd, Sm, Eu, Gd, Dy, Ho, Er, Tn, Yb and Lu; x is from about 6.5 to about 7.0; said composition having a superconducting transition temperature of about 90.degree. K.; said process consisting essentially of preparing a precursor solution, drying the solution to obtain a solid material, and heating and cooling the solid material under specified conditions to obtain the desired product. In another embodiment, a shaped superconducting MBa.sub.2 Cu.sub.3 O.sub.x article is prepared by impregnating an article of cellulose material with the precursor solution, drying the impregnated article, and heating and cooling the impregnated article under prescribed conditions to obtain the desired product.Type: GrantFiled: March 13, 1989Date of Patent: January 8, 1991Assignee: E. I. Du Pont de Nemours and CompanyInventors: John D. Bolt, Munirpallam A. Subramanian
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Patent number: 4975415Abstract: The present invention pertains to a method of preparing particles of superconducting ceramic powders, which method comprises:(a) dissolving the soluble salts of the cations in aqueous medium;(b) obtaining a solution having pH of between about 4 and 7 by optionally treating the aqueous medium with ammonia, or ammonium hydroxide;(c) atomizing the solution of step (b) onto liquid nitrogen at about -196.degree. C.;(d) removing the liquid nitrogen by evaporation;(e) removing the water by sublimation at reduced pressure;(f) heating the solid residue of step (e) at 40-60.degree. C. at reduced pressure;(g) calcining the solid residue in flowing oxygen or air at temperature of between about 200.degree. to 895.degree. C.; and(h) cooling the solid at a temperature of between about 900.degree. C. and ambient temperature in sufficient air or oxygen and recovering the superconducting powder having an average diameter of between about 0.1 and 10 microns.Type: GrantFiled: July 10, 1987Date of Patent: December 4, 1990Assignee: SRI - InternationalInventors: Michael I. Gusman, Sylvia M. Johnson
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Patent number: 4956338Abstract: A complex oxidation reaction product of two or more metals in an oxidized state is formed by positioning a suitable precursor metal adjacent to a permeable mass of a metal-containing compound in an oxidizing atmosphere and heating the assembly to form a body of molten precursor metal. The molten metal infiltrates the permeable mass and reacts therewith and with the oxidizing atmosphere to form a complex oxidation reaction product. Methods for determining the shape of the resulting article are described. The disclosed methods can be used to form superconducting perovskites.Type: GrantFiled: July 6, 1988Date of Patent: September 11, 1990Assignee: Lanxide Technology Company, LPInventors: Robert A. Rapp, Andrew W. Urquhart, Alan S. Nagelberg, Marc S. Newkirk
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Patent number: 4956340Abstract: A process for preparing compound metal oxides, superconductive compound oxides, is disclosed. The process comprises preparing an aqueous solution containing a predetermined content ratio of chloride, nitrate or acetate of a rare earth metal, an alkaline earth metal and copper, said content ration corresponding to the composition of the object compound metal oxide, adjusting the pH of the solution to 1.5-2.0, adding oxalic acid in an amount such that the concentration of the residual oxalic acid becomes 0.05 M/l-0.1 M/l, collecting the thus formed precipitate and firing it.Type: GrantFiled: November 3, 1989Date of Patent: September 11, 1990Assignee: Mitsubishi Kinzoku Kabsuhiki KaishaInventors: Etsuji Kimura, Nozomu Hasegawa, Yutaka Nishiyama
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Patent number: 4952557Abstract: A method for depositing superconducting ceramic materials on an article by electrodeposition including the steps of obtaining a dispersion of the components of a superconducting ceramic material in a non-aqueous medium and creating an electrical field within the medium such that the material will migrate to and deposit on an electrode placed within the medium. After deposition, the article is sintered and then reoxygenated to achieve the composition required for the superconducting ceramic material.Type: GrantFiled: July 6, 1988Date of Patent: August 28, 1990Assignee: Ametek, Inc.Inventor: Ferenc Schmidt
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Patent number: 4895832Abstract: A homogenous coprecipitation method by which superconducting oxides having perovskite-like structure, such as YBa2Cu307-x, can be produced in mass, in which urea is used as solvent to adjust and control the PH value of an aqueous nitrate solution. The coprecipitation method of this invention comprises following steps: (a) preparing an aqueous mixture containing Y, Ba and Cu salts with molar ratio of 1:2:3 wherein Y being 0.068M; (b) adding 5-10 moles of oxalic acid per one mole of Y and 20-250 moles of urea per moles of Y into the aqueous mixture; (c) heating the aqueous mixture to a temperature range of 80.degree. to 100.degree. C. to proceed a hydrolysis of the urea such that PH value of the aqueous mixture will be gradually elevated by NH.sub.3 gas evoluted from the urea hydrolysis; and (d) cooling the temperature of the aqueous mixture to room temperature at which time a desired uniform PH value is reached. After cooling, pale blue homogeneous coprecipitates of the superconducting oxides can be obtained.Type: GrantFiled: November 3, 1988Date of Patent: January 23, 1990Assignee: Industrial Technology Research InstituteInventors: Chau-Ting Chang, Ru-Shi Liu