Settling Of Powder In Molten Metal Or Salt Bath Patents (Class 75/368)
  • Patent number: 10245642
    Abstract: A method for producing a metal powder includes maintaining molten reducing metal in a sealed reaction vessel that is substantially free of oxygen and water, establishing a vortex in the molten reducing metal, introducing a metal halide into the vortex so that the molten reducing metal is in a stoichiometric excess to the metal halide, thereby producing metal particles and salt, removing unreacted reducing metal, removing the salt, and recovering the metal powder. The molten reducing metal can be a Group I metal, a Group II metal, or aluminum.
    Type: Grant
    Filed: February 23, 2016
    Date of Patent: April 2, 2019
    Assignee: Nanoscale Powders LLC
    Inventors: David Henderson, Andrew Matheson, Richard Van Lieshout, Donald Finnerty, John W. Koenitzer
  • Patent number: 9878919
    Abstract: The invention provides a Potassium Fluotitanate (K2TIF6) manufacture process. The Potassium Fluotitanate (K2TIF6) manufacture process includes steps: A. providing titanium ferrum powder to a reaction furnace and adding HF and peroxide solution to react with the titanium ferrum powder sufficiently to manufacture H2TiF6, B. filtrating the sufficiently mixed solution of step A and adding it to another reaction furnace, and then after the H2TiF6 cools off, adding Potassium Chloride (KCl) solution to react with the mixed solution to manufacture Potassium Fluotitanate (K2TiF6); C. adding K2CO3 solution to the remaining solution of step B and react with the remaining solution and controlling the pH value, the element Fe is recycled by a form of Fe(OH)3 flocculent precipitate and the Potassium Chloride (KCl) and KF solution are recycled.
    Type: Grant
    Filed: July 29, 2010
    Date of Patent: January 30, 2018
    Assignee: SHENZHEN SUNXING LIGHT ALLOYS MATERIALS CO., LTD.
    Inventors: Xuemin Chen, Qingdong Ye, Jianguo Li, Chaowen Liu, Yueming Yu
  • Patent number: 8790441
    Abstract: The invention provides a crystalline Ti powder produced in a molten salt medium, said powder comprising predominantly particles of single ?-Ti crystals that are directly applicable in powder metallurgy.
    Type: Grant
    Filed: December 23, 2011
    Date of Patent: July 29, 2014
    Assignee: CSIR
    Inventors: David Steyn Van Vuuren, Salomon Johannes Oosthuizen
  • Patent number: 8430944
    Abstract: A process and system for producing tantalum or other valve metal particles is provided comprising forming tantalum particles in a reduction process carried out in a reactor vessel, and using a siphon to transfer fine tantalum particles out of the reaction mixture to a recovery vessel. This particle transfer can occur while the reaction mixture is agitated. The tantalum particles can be automatically withdrawn when the reaction mixture has a depth level greater than the fluid level of the tantalum fine particle recovery vessel, and outflow automatically stops when the fluid levels of the reactor and particle recovery vessel equilibrate. Tantalum or other valve metal powders made by the processes, and capacitors made with valve metal powders are also provided.
    Type: Grant
    Filed: November 20, 2009
    Date of Patent: April 30, 2013
    Assignee: Global Advanced Metals, USA, Inc.
    Inventor: Hitoshi Iijima
  • Patent number: 8066861
    Abstract: A method for producing metal powder is provided the comprising supplying a molten bath containing a reducing agent, contacting a metal oxide with the molten bath for a time and at a temperature sufficient to reduce the metal in the metal oxide to elemental metal and produce free oxygen; and isolating the elemental metal from the molten bath.
    Type: Grant
    Filed: February 14, 2008
    Date of Patent: November 29, 2011
    Assignee: The United States of America as represented by the Department of Energy
    Inventor: Jong-Hee Park
  • Patent number: 8012273
    Abstract: A metallic article is produced by furnishing one or more nonmetallic precursor compound comprising the metallic constituent element(s), and chemically reducing the nonmetallic precursor compound(s) to produce an initial metallic particle, preferably having a size of no greater than about 0.070 inch, without melting the initial metallic particle. The initial metallic particle is thereafter melted and solidified to produce the metallic article. By this approach, the incidence of chemical defects in the metal article is minimized. The melted-and-solidified metal may be used in the as-cast form, or it may be converted to billet and further worked to the final form.
    Type: Grant
    Filed: June 28, 2010
    Date of Patent: September 6, 2011
    Assignee: General Electric Company
    Inventors: Andrew P. Woodfield, Clifford E. Shamblen, Eric A. Ott
  • Patent number: 7914600
    Abstract: A method for production of titanium particles or other metal of interest by a metallothermic reduction reaction of TiCl4 or other metal chloride in a reaction zone which comprises conducting the reaction in a fluidized bed reaction zone, and recycling particles to the reaction zone to build up particle size.
    Type: Grant
    Filed: January 11, 2008
    Date of Patent: March 29, 2011
    Assignee: Materials & Electrochemical Research Corp.
    Inventors: James C. Withers, Raouf Loutfy
  • Patent number: 7419528
    Abstract: A metallic article made of metallic constituent elements is fabricated from a mixture of nonmetallic precursor compounds of the metallic constituent elements. The mixture of nonmetallic precursor compounds contains more of a base-metal element, such as nickel, cobalt, iron, iron-nickel, and iron-nickel-cobalt than any other metallic element. The mixture of nonmetallic precursor compounds is chemically reduced to produce a metallic superalloy material, without melting the metallic superalloy material. The metallic superalloy material is consolidated to produce a consolidated metallic article, without melting the metallic superalloy material and without melting the consolidated metallic article.
    Type: Grant
    Filed: February 19, 2003
    Date of Patent: September 2, 2008
    Assignee: General Electric Company
    Inventors: Clifford Earl Shamblen, Andrew Philip Woodfield, Eric Allen Ott, Michael Francis Xavier Gigliotti
  • Patent number: 6942715
    Abstract: A process for producing metallic titanium includes forming metallic titanium fine particles by supplying liquid or mist titanium tetrachloride from above the surface of a reaction bath liquid containing fused magnesium and fused magnesium chloride in a reaction vessel to effect a reaction, wherein a circulating flow perpendicular to the bath surface of the reaction bath liquid is generated or extended just under the bath surface by imparting a stirring force to the reaction bath liquid so as to generate or increase an upward flow rate of the reaction bath liquid in at least part of the region at a depth of more than 100 mm below the bath surface.
    Type: Grant
    Filed: April 4, 2003
    Date of Patent: September 13, 2005
    Assignee: Toho Titanium Co., Ltd.
    Inventors: Nobuaki Ito, Masanori Yamaguchi, Kenichi Kato, Shigeo Ampo
  • Patent number: 6855185
    Abstract: A method of manufacturing niobium and/or tantalum powder consisting of: a first-stage reduction process of reducing niobium and/or tantalum oxides with alkali metals and/or alkaline-earth metals to obtain low-grade oxide powder represented by (NbTa) Ox, where x=0.06 to 0.35, a process of removing the oxide of alkali metals and/or alkaline-earth metals generated in the first-stage reduction process, and a second-stage reduction process of reducing the low-grade oxide powder obtained in the first-stage reduction process, with a melt solution of alkali metals and alkaline-earth metals to obtain niobium and/or tantalum powder.
    Type: Grant
    Filed: October 10, 2002
    Date of Patent: February 15, 2005
    Assignee: Sumitomo Metal Mining Co., Ltd.
    Inventors: Toshiyuki Osako, Tetsufumi Komukai
  • Patent number: 6814777
    Abstract: The invention provides platinum or platinum alloy powders for use in fuel cells and for chemical reactions. The powders are characterized by a high surface area and, at the same time, low chlorine contents. The powders are prepared by forming a melt which contains, as starting substances, a low melting mixture of alkali metal nitrates, a chlorine-free platinum compound and optionally chlorine-free compounds of alloying elements, the melt is then heated to a reaction temperature at which the platinum compound and the compounds of alloying elements thermally decompose to give oxides, the melt is then cooled and dissolved in water and the oxides or mixed oxides formed are converted into platinum or platinum alloy powders by subsequent reduction. Binary or ternary eutectic mixtures from the LiNO3—KNO3—NaNO3 system are suitable as a low melting mixture of nitrates of the alkali metals. Hexahydroxoplatinic-(IV)-acid is preferably used as a chlorine-free platinum compound.
    Type: Grant
    Filed: July 31, 2002
    Date of Patent: November 9, 2004
    Assignee: Umicore AG & Co. KG
    Inventor: Peter Biberbach
  • Patent number: 6749663
    Abstract: A process is described for the preparation of tungsten and/or molybdenum metal powder or carbide by reducing and optionally carburizing treatment of tungsten and/or molybdenum oxide powder in the presence of alkali metal compounds, wherein at least two alkali metal compounds are used in a ratio so that mixed alkali tungstate or molybdate potentially formed in an intermediate step ((Li, Na, K)2 WOZ, (Li, Na, K)2MoOZ) has a melting point of less than 550° C., wherein z is from 3 to 4.
    Type: Grant
    Filed: August 30, 2001
    Date of Patent: June 15, 2004
    Assignee: H.C. Starck GmbH
    Inventors: Jörg Bredthauer, Benno Gries, Bernhard Szesny
  • Publication number: 20020084006
    Abstract: A novel product composed of a ceramic phase particle dispersoid in metal, including uniformly distributed, finely sized carbide phase particles formed in situ in a molten metal and a novel method for producing such a ceramic phase particle dispersoid in metal are disclosed. A salt-based liquid state reaction involving a liquid metal/alloy containing a liquid Ti, B, Si, Sc, Hf, Nb, Ta, Zr, Mo, Al (when the molten metal matrix is not aluminum), or V and a halide salt containing carbon particles forms a uniform distribution of finely sized ceramic phase particles formed and dispersed in-situ in the metal matrix. The ceramic dispersoid in metal product of the present invention includes at least about 50 volume percent of a matrix metal of aluminum; and up to about 50 volume percent of a uniform distribution of finely sized ceramic phase particles formed and dispersed in-situ in the aluminum metal matrix, wherein the finely sized ceramic phase particles have an average particle diameter of less than about 2.
    Type: Application
    Filed: February 7, 2002
    Publication date: July 4, 2002
    Inventors: Men Glenn Chu, Siba P. Ray
  • Patent number: 6210461
    Abstract: This invention provides improved production, continuous or batch, especially of metals which have been produced by versions of the Kroll and Ames processses. This list includes titanium, zirconium, hafnium, vanadium, niobium, tantalum, rhenium, molybdenum, tungsten, and uranium. It also offers a process for growing particular shapes of metallic crystals, e.g., needlelike. This invention is intended to be less expensive to operate and to provide a superior product than from Kroll batch processing, as often used: For the continuous metal production, circulating molten salt supports two principal reaction stages, which together allow continuous metal production: Titanium powder production with one possible set of reactants may be used as an example for the group of metals listed: In Stage 1 a pumped solution of titanium ions (Ti++) dissolved in molten salt (e.g., MgCl2—KCl) flows onto, then down beside, molten magnesium that floats on molten salt below.
    Type: Grant
    Filed: August 10, 1998
    Date of Patent: April 3, 2001
    Inventor: Guy R. B. Elliott
  • Patent number: 6139658
    Abstract: The invention provides a method of making a titanium carbide metal matrix alloy, by firing a particulate reaction mixture comprising carbon, titanium and matrix material, under conditions such that the titanium and carbon react exothermically to form a dispersion of fine particles comprising titanium carbide (preferably less than 10 microns) in a predominantly metal matrix. The titanium and matrix are preferably added as a titanium alloy such as ferrotitanium, e.g. eutectic ferrotitanium. The reaction conditions are preferably selected so that during the reaction a molten zone moves through the body of the reaction mixture; the resulting hard particles are of globular form; and their average size is uniform throughout the resulting dispersion.
    Type: Grant
    Filed: September 23, 1997
    Date of Patent: October 31, 2000
    Assignee: London & Scandinavian Metallurgical Co., Ltd.
    Inventors: Peter Davies, James Leslie Frederick Kellie, Richard Nigel McKay, John Vivian Wood
  • Patent number: 6136062
    Abstract: The process comprises the reduction of niobium and/or tantalum oxides by means of alkaline earth metals and/or rare earth metals, wherein the first reduction stage is carried out as far as an average composition corresponding to (Nb, Ta)O.sub.x where x=0.5 to 1.5 and before the second stage the reduction product from the first stage is freed from alkaline earth oxides and/or rare earth metal oxides which are formed (and optionally from excess alkaline earth metal and/or rare earth metal) by washing with mineral acids.
    Type: Grant
    Filed: September 21, 1999
    Date of Patent: October 24, 2000
    Assignee: H. C. Starck GmbH & Co. KG
    Inventors: Josua Loffelholz, Frank Behrens
  • Patent number: 6036792
    Abstract: A novel product composed of a ceramic phase particle dispersoid in metal, including uniformly distributed, finely sized carbide phase particles formed in situ in a molten metal and a novel method for producing such a ceramic phase particle dispersoid in metal are disclosed. A salt-based liquid state reaction involving a liquid metal/alloy containing a liquid Ti, B, Si, Sc, Hf, Nb, Ta, Zr, Mo, Al (when the molten metal matrix is not aluminum), or V and a halide salt containing carbon particles forms a uniform distribution of finely sized ceramic phase particles formed and dispersed in-situ in the metal matrix. The ceramic dispersoid in metal product of the present invention includes at least about 50 volume percent of a matrix metal of aluminum; and up to about 50 volume percent of a uniform distribution of finely sized ceramic phase particles formed and dispersed in-situ in the aluminum metal matrix, wherein the finely sized ceramic phase particles have an average particle diameter of less than about 2.
    Type: Grant
    Filed: April 1, 1998
    Date of Patent: March 14, 2000
    Assignee: Aluminum Company of America
    Inventors: Men Glenn Chu, Siba P. Ray
  • Patent number: 5964918
    Abstract: A process for preparing a metal powder, comprising the steps of: bringing a solution comprising at least one metal salt to fine droplets; and heating the droplets to a temperature above the decomposition temperature of the metal salt, wherein at least one compound which is heat-decomposable to produce a metal, a semimetal or an oxide of the metal or semimetal capable of remaining unmelted upon heating at the heat temperature is added to the solution and at least one selected from the group consisting of the metal, semimetal and oxide is heat-segregated in the vicinity of the surface of the metal powder. The resultant metal powder has a uniform particle size and good dispersibility without fusing or aggregation and is useful for the preparation of thick film pastes used in electronic circuits or components.
    Type: Grant
    Filed: September 23, 1997
    Date of Patent: October 12, 1999
    Assignee: Shoei Chemical Inc.
    Inventors: Eiichi Asada, Yuji Akimoto, Kazuro Nagashima, Mineto Iwasaki
  • Patent number: 5795366
    Abstract: To essentially eliminate aluminum and silicon as contaminants in a doped tungsten wire, the tungsten wire is obtained by mechanical working of reduced tungsten blue oxide which contains as a primary or major constituent a special hexagonal ammonium tungsten bronze of the general formula (NH.sub.4).sub.X (NH.sub.3).sub.y WO.sub.3. A liquid doping step is carried out by adding a solution containing potassium nitrate, the special doped ammonium tungsten bronze forming preferably more than 70% by weight of the overall tungsten blue oxide. The special hexagonal ammonium tungsten bronze is made by decomposing ammonium paratungstate in an ammonium atmosphere, preferably at a temperature between about 400.degree. and 550.degree. C.
    Type: Grant
    Filed: February 28, 1996
    Date of Patent: August 18, 1998
    Assignee: Patent-Treuhand-Gesellschaft fuer elektrische Gluehlampen mbH
    Inventors: Michael Salmen, Hans-Joachim Lunk, Alfred-Georg Gahn, Bernhard Altmann, Martin Fait
  • Patent number: 5785731
    Abstract: To dope ammonium paratungstate with potassium, essentially devoid of silicon and ammonium, an aqueous potassium containing solution, preferably potassium hydroxide is added to an aqueous solution of ammonium paratungstate (APW), in a mol relationship of potassium to ammonium of between 0.1 and 10. A doped ammonium potassium paratungstate (AKPW) is obtained. This ammonium potassium paratungstate is then converted to tungsten blue oxide, which is reduced, preferably in a hydrogen containing atmosphere and a tungsten powder is then obtained which will be doped with 40 to 120 ppm, preferably about 90 ppm of potassium. Lamps equipped with tungsten wire filaments drawn from so doped tungsten have lifetimes at least 10% more than lamps with conventional tungsten filaments.
    Type: Grant
    Filed: February 28, 1996
    Date of Patent: July 28, 1998
    Assignee: Patent-Treuhand-Gesellschaft fur elektrische Gluhlampen mbH
    Inventors: Martin Fait, Joachim Fuchs, Alfred-Georg Gahn, Hans-Joachim Lunk, Michael Salmen, Burkhard Ziemer
  • Patent number: 5735976
    Abstract: A novel method for producing a ceramic phase particle dispersoid in metal and a novel product composed thereof are disclosed, including finely sized carbide phase particles formed in situ in a molten metal by salt-based liquid state reaction with Ti, B, Si, Sc, Hf, Nb, Ta, Zr, Mo, Al (when the molten metal matrix is not aluminum), or V and a halide salt containing carbon particles to form a uniform distribution of finely sized ceramic phase particles formed and dispersed in-situ in the metal matrix. The step of reacting includes vigorously stirring to form a reaction mixture at an elevated temperature for a residence time less than one hour to form a uniform distribution of particles sized less than 2.5 microns uniformly dispersed in-situ in the metal matrix.
    Type: Grant
    Filed: January 31, 1996
    Date of Patent: April 7, 1998
    Assignee: Aluminum Company of America
    Inventors: Men Glenn Chu, Siba P. Ray
  • Patent number: 5707420
    Abstract: The copper powder contains at least one substance, which is not soluble in copper, e.g. Al.sub.2 O.sub.3, TiO.sub.2, SiO.sub.2 or B.sub.2 O.sub.3. For the production of this copper powder, a surplus of copper metal granulate is mixed with an ammonium salt and/or ammonium hydroxide, together with a saline solution in an aqueous solution, while a gas containing oxygen is added, and at a pH-value of at least 4. A copper-containing precipitate is produced, which is separated and treated at a temperature in the range from 150.degree. to 500.degree. C. in a reducing atmosphere. During this process, Cu(OH).sub.2 and Cu-oxide are transformed into metallic copper powder, which contains the dispersoid. The dispersoid content of the copper powder is preferably in the range from 0.1 to 5% by weight.
    Type: Grant
    Filed: September 26, 1995
    Date of Patent: January 13, 1998
    Assignee: Norddeutsche Affinerie Aktiengesellschaft
    Inventors: Bernd E. Langner, Peter Stantke, Rene-Holger Wilde
  • Patent number: 5626645
    Abstract: A process for making silver metal particles from silver salt particles having the same morphology. Precursor silver salt particles selected from the group consisting of silver acetate and silver sulfide having a selected morphology are contained in a reactor vessel having means for supporting the particles in an air suspension to prevent the agglomeration of the particles. Air is flowed through the reactor vessel at a flow rate sufficient to suspend the particles in the reactor vessel. The suspended precursor silver salt particles are heated to a processing temperature and at a heating rate below which the physical deterioration of the suspended precursor silver salt particles takes place. The suspended precursor silver salt particles are maintained at the processing temperature for a period of time sufficient to convert the particles into silver metal particles having the same morphology as the precursor silver salt particles.
    Type: Grant
    Filed: September 27, 1995
    Date of Patent: May 6, 1997
    Assignee: The United States of America as represented by the Department of Energy
    Inventor: Carlos E. Bamberger
  • Patent number: 5482691
    Abstract: The invention relates to a process for the production of metallic titanium, characterized in that the process comprises reducing a titanium-fluorine compound selected from titanium tetrafluoride and any hexafluorotitanate soluble in a molten fluoroaluminate, with metallic aluminum in a molten fluoroaluminate. A process for the production of intermediates useful in the processing ilmenite and related minerals is also described.
    Type: Grant
    Filed: January 23, 1995
    Date of Patent: January 9, 1996
    Assignee: The University of Melbourne
    Inventors: Thomas A. O'Donnell, John Besida, Teresa K. H. Pong, David G. Wood
  • Patent number: 5439502
    Abstract: A method for the manufacture of finely divided silver particles comprising the sequential steps:A. Forming an unsaturated solution of thermally decomposable silver-containing compound in a volatilizable solvent;B. Forming an aerosol from the unsaturated solution and a carrier gas;C. Heating the aerosol to a temperature above the decomposition temperature of the silver compound, but below the melting point of silver metal by which the silver compound is decomposed to form finely divided particles of pure densified silver; andD. Separating the precipitated silver particles from the carrier gas, reaction by-products and solvent voltilization products.
    Type: Grant
    Filed: April 8, 1994
    Date of Patent: August 8, 1995
    Assignees: E. I. Du Pont de Nemours and Company, University of New Mexico
    Inventors: Toivo T. Kodas, Timothy L. Ward, Howard D. Glicksman
  • Patent number: 5397375
    Abstract: The invention relates to a process for the production of metallic titanium, characterized in that the process comprises reducing a titanium-fluorine compound selected from titanium tetrafluoride and any hexafluorotitanate soluble in a molten fluoroaluminate, with metallic aluminum in a molten fluoroaluminate. A process for the production of intermediates useful in the processing ilmenite and related minerals is also described.
    Type: Grant
    Filed: October 22, 1993
    Date of Patent: March 14, 1995
    Assignee: The University of Melbourne
    Inventors: Thomas A. O'Donnell, John Besida, Tersesa K. H. Pong, David G. Wood
  • Patent number: 5259862
    Abstract: A continuous process for producing a granular metal selected from the group consisting of Ti, Zr or Hf under conditions that provide orderly growth of the metal free of halide inclusions comprising:a) dissolving a reducing metal selected from the group consisting of Na, Mg, Li or K in their respective halide salts to produce a reducing molten salt stream;b) preparing a second molten salt stream containing the halide salt of Ti, Zr or Hf;c) mixing and reacting the two molten streams of steps a) and b) in a continuous stirred tank reactor;d) wherein steps a) through c) are conducted at a temperature range of from about 800.degree. C. to about 1100.degree. C. so that a weight percent of equilibrium solubility of the reducing metal in its respective halide salt varies from about 1.6 weight percent at about 900.degree. C. to about 14.4 weight percent at about 1062.degree. C.
    Type: Grant
    Filed: October 5, 1992
    Date of Patent: November 9, 1993
    Assignee: The United States of America as represented by the Secretary of the Interior
    Inventors: Jack C. White, Laurance L. Oden
  • Patent number: 4921531
    Abstract: The present invention relates to a process for the production of fine powder materials and the products of that process. The process involves the in-situ precipitation of second phase particles, such as ceramic or intermetalics, within a metal matrix, followed by separation of the particles from the matrix to yield a powder comprising the second phase particles. Particles formed by this process are typically in the size range of 0.01 to 10 microns and have controlled morphology, narrow size distribution, well defined stoichiometery and relatively high purity. Exemplary of second phase particles formed by this process are metal borides, carbides, nitrides, oxides, silicides and beryllides, including TiB.sub.2, ZrB.sub.2, VB.sub.2, MoB.sub.2, TiC, WC, VC, TiN, ZrSi.sub.2, MoSi.sub.2, Ti.sub.5 Si.sub.3, and TiBe.sub.12.
    Type: Grant
    Filed: August 30, 1989
    Date of Patent: May 1, 1990
    Assignee: Martin Marietta Corporation
    Inventors: Dennis C. Nagle, John M. Brupbacher, Leontios Christodoulou