Titanium, Zirconium, Or Hafnium (ti, Zr, Or Hf) Patents (Class 205/397)
  • Patent number: 11142841
    Abstract: Methods for electropolishing and coating aluminum on a surface of an air and/or moisture sensitive substrate, including: in a vessel, submerging the substrate in a first molten salt bath and applying an anodizing current to the substrate at a first temperature to electropolish the surface of the substrate; wherein the first molten salt bath includes one of a first organic salt bath and first inorganic salt bath; wherein, when used, the first organic salt bath includes one of (a) aluminum halide and ionic liquid, (b) a combination of an aluminum halide and halogenatedmethylphenylsulfone (C6(H5?y,Xy)SO2CX3, where y is a number from 0-5), (c) a combination of an aluminum halide, an ionic liquid, and halogenatedmethylphenylsulfone (C6(H5?y,Xy)SO2CX3), and (d) AlF3-organofluoride-hydrofluoric acid adduct; wherein, when used, the first inorganic salt bath includes aluminum halide and alkali metal halide; and wherein the anodizing current is 10-30 mA/cm2.
    Type: Grant
    Filed: September 17, 2019
    Date of Patent: October 12, 2021
    Assignee: Consolidated Nuclear Security, LLC
    Inventors: John W. Freiderich, Tasha L. Boyd
  • Patent number: 10106902
    Abstract: This invention provides an electrolyte salt for use in an electrodeposition process for depositing Zirconium metal on a thin foil substrate. The prior art electrochemical process causes a reaction between a uranium substrate and ZrF4 species in the electrolyte that causes the formation of UFx at the substrate surface that prevents the formation of a dense uniform zirconium coating. This problem is solved by using an electrolyte salt in an electrodeposition process consisting of lithium fluoride (LiF) in a concentration ranging between about 11.5 molar percent and about 61 molar percent and one or more salts selected from the group consisting of sodium fluoride (NaF), potassium fluoride (KF), cesium fluoride (CsF), or cesium chloride (CsCL). Zirconium is added to the electrolyte salt through an addition of zirconium fluoride (ZrF4) in the range of about 1 to about 5 mass percent (w/w %). The Zr coating is of at least 98% pure Zr with a density of at least 98%.
    Type: Grant
    Filed: March 21, 2017
    Date of Patent: October 23, 2018
    Assignee: Plasma Processes, LLC
    Inventors: Alexander Smirnov, Scott O'Dell, Anatoliy Shchetkovskiy
  • Patent number: 9150943
    Abstract: A method for producing a pure metal M or metal alloy MxNy, of interest, which comprises electrolyzing a molten salt electrolyte of an alkali-metal or alkaline-earth metal halide AX or AX2, with an anode formed of graphite or made of a composite of a metal oxide of the metal of interest and carbon, to discharge the alkali or alkaline-earth metal A, at the cathode, and to discharge nascent chlorine gas at the anode, whereby to produce a halide of the metal of interest MXn and/or NXn, and metallothermically reducing the metal halide MXn and/or NXn either separately or combined, with the alkali or alkaline-earth metal A, obtained cathodically to produce the metal M or the metal alloy MxNy of interest in particulate form.
    Type: Grant
    Filed: January 18, 2008
    Date of Patent: October 6, 2015
    Assignee: MATERIALS & ELECTROCHEMICAL RESEARCH CORP.
    Inventors: James C. Withers, Raouf O. Loutfy
  • Patent number: 9017541
    Abstract: The present invention relates to the electrodeposition of elemental zirconium at a temperature of less than 100° C. from a mixture of a Lewis acid, a zirconium salt and an ionic liquid.
    Type: Grant
    Filed: May 28, 2010
    Date of Patent: April 28, 2015
    Assignee: Astron Advanced Materials Limited
    Inventors: Kenneth Seddon, Geetha Srinivasen, Anthony Wilson
  • Publication number: 20140291161
    Abstract: Provided is a method for obtaining a particular metal at high purity, with safety, and at low cost, from a treatment object containing two or more metal elements. The present invention provides a method for producing a metal by molten salt electrolysis, the method including a step of dissolving, in a molten salt, a metal element contained in a treatment object containing two or more metal elements; and a step of depositing or alloying a particular metal present in the molten salt, on one of a pair of electrode members disposed in the molten salt containing the dissolved metal element, by controlling a potential of the electrode members to a predetermined value.
    Type: Application
    Filed: October 22, 2012
    Publication date: October 2, 2014
    Inventors: Tomoyuki Awazu, Masatoshi Majima
  • Publication number: 20140144786
    Abstract: The manufacturing method for high-purity Zirconium is characterized by self-propagating high temperature synthesis (SHS) of a raw material having zirconium raw ore containing ZrO2, ZrSiO4, KZr2(PO4)3, or a mixture thereof and a reducing agent that is metal powder, to prepare zirconium intermetallic compound or zirconium nitride, followed by the recovery of high-purity Zr by electrolytic refining the reaction product of the SHS.
    Type: Application
    Filed: July 29, 2011
    Publication date: May 29, 2014
    Applicant: The Industry & Academic Cooperation in Chungnam National University
    Inventors: Jong Hyeon Lee, Yoon Sang Lee, Han Soo Lee, Seon Jin Kim, Sun Kyo Chung, H. Nersisyan Hayk
  • Publication number: 20130277228
    Abstract: A method for stabilizing a nuclear material may include electrolytically reducing the nuclear material in a first molten salt electrolyte of an electroreducer to produce a reduced material. A reducer waste may accumulate in the first molten salt electrolyte as a byproduct of the electroreduction. After the electroreduction, the reduced material may be electrolytically dissolved in a second molten salt electrolyte of an electrorefiner to produce a purified metal product on a refiner cathode assembly of the electrorefiner. As a result of the electrorefining, a first refiner waste may accumulate in the second molten salt electrolyte and a second refiner waste may accumulate in a refiner anode assembly of the electrorefiner. The reducer waste from the electroreducer and the first refiner waste from the electrorefiner may be converted into a ceramic waste form, while the second refiner waste from the electrorefiner may be converted into a metallic waste form.
    Type: Application
    Filed: April 23, 2012
    Publication date: October 24, 2013
    Applicant: GE-HITACHI NUCLEAR ENERGY AMERICAS LLC
    Inventors: Eric P. Loewen, John F. Berger
  • 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
  • Publication number: 20110108434
    Abstract: An object of the present invention is to provide a method of producing metal zirconium, the method having a fewer steps and a smaller amount of secondary wastes generated, wherein the metal zirconium is obtained from a zirconium compound containing hafnium. A method of producing metal zirconium according to the present invention includes: a separation step of separating a hafnium oxychloride from a first substance containing a zirconium oxychloride and a hafnium oxychloride to obtain a second substance having a higher content of the zirconium oxychloride; a calcination step of calcining the second substance to obtain a third substance containing at least any of a zirconium oxychloride and a zirconium oxide; and a direct reduction step of holding the third substance in a molten salt with the third substance brought into contact with a cathode and applying a voltage between the cathode and an anode to directly reduce the third substance to obtain metal zirconium.
    Type: Application
    Filed: June 29, 2009
    Publication date: May 12, 2011
    Applicant: KABUSHIKI KAISHA TOSHIBA
    Inventors: Reiko Fujita, Koji Mizuguchi, Hitoshi Nakamura, Kouki Fuse, Mitsuru Kawamoto, Masaru Ito
  • Publication number: 20090152104
    Abstract: A molten salt electrolyzer for reducing metal comprises an electrolytic cell filled with a molten salt composed of a reducing metal chloride, an anode immersed in the molten salt of the electrolytic cell and surrounded by a first wall at the periphery thereof, and a cathode immersed in the molten salt of the electrolytic cell and surrounded by a second wall at the periphery thereof.
    Type: Application
    Filed: June 21, 2006
    Publication date: June 18, 2009
    Inventors: Yuichi Ono, Masanori Yamaguchi
  • Publication number: 20090000955
    Abstract: An electrolysis system for generating a metal and molecular oxygen includes a container for receiving a metal oxide containing a metallic species to be extracted, a cathode positioned to contact a metal oxide housed within the container; an oxygen-ion-conducting membrane positioned to contact a metal oxide housed within the container; an anode in contact with the oxygen-ion-conducting membrane and spaced apart from a metal oxide housed within the container, said anode selected from the group consisting of liquid metal silver, oxygen stable electronic oxides, oxygen stable crucible cermets, and stabilized zirconia composites with oxygen stable electronic oxides.
    Type: Application
    Filed: July 14, 2006
    Publication date: January 1, 2009
    Applicant: TRUSTEES OF BOSTON UNIVERSITY
    Inventor: Uday B. Pal
  • Patent number: 7470355
    Abstract: A process for electrochemically reducing a metal oxide, such as titania, in a solid state in an electrochemical cell that includes a bath of molten electrolyte, a cathode, and an anode, which process includes the steps of: a) applying a cell potential across the anode and the cathode that is capable of electrochemically reducing the metal oxide supplied to the molten electrolyte bath, b) continuously or semi-continuously feeding the metal oxide in powder and/or pellet form into the molten electrolyte bath, c) transporting the powders and/or pellets along a path within the molten electrolyte bath and reducing the metal oxide as the metal oxide powders and/or pellets move along the path, and d) continuously or semi-continuously removing metal from the molten electrolyte bath. Also disclosed and claims is an electrochemical cell for carrying out this process.
    Type: Grant
    Filed: December 12, 2003
    Date of Patent: December 30, 2008
    Assignee: BHP Billiton Innovation Pty Ltd
    Inventors: Steve Osborn, Ivan Ratchev, Les Strezov, Greg Rigby
  • Patent number: 7208075
    Abstract: A method of reducing a metal oxide in a solid state, in an electrolytic cell, is provided, as is an electrolytic cell suitable for performing the method. The cathode of the electrolytic cell is formed at least in part from the metal oxide to be reduced, and the electrolyte includes cations of a metal that is capable of chemically reducing the cathode metal oxide. The method includes operating the cell at a potential that is above the potential at which cations of the reducing metal will deposit as metal on the cathode.
    Type: Grant
    Filed: August 11, 2003
    Date of Patent: April 24, 2007
    Assignee: BHP Billiton Innovation Pty Ltd.
    Inventors: Lazar Strezov, Ivan Ratchev, Steve Osborn
  • Patent number: 7169285
    Abstract: A low temperature method for reducing and purifying refractory metals, metal compounds, and semi-metals using a catalyst. Using this invention, TiO2 can be reduced directly to Ti metal at room temperature. The catalyst is an ion in an electrolyte that catalyzes the rate of the reduction of a compound MX to M, wherein M is a metal or a semi-metal; MX is a metal compound, a semi-metal compound, or a metal or semi-metal dissolved as an impurity in M; and X is an element chemically combined with or dissolved in M.
    Type: Grant
    Filed: June 16, 2004
    Date of Patent: January 30, 2007
    Assignee: The United States of America as represented by the Secretary of the Navy
    Inventors: William E. O'Grady, Graham T. Cheek
  • Patent number: 6958115
    Abstract: This invention discloses and claims the low temperature reduction and purification of refractory metals, metal compounds, and semi-metals. The reduction is accomplished using non-aqueous ionic solvents in an electrochemical cell with the metal entity to be reduced. Using this invention, TiO2 is reduced directly to Ti metal at room temperature.
    Type: Grant
    Filed: June 24, 2003
    Date of Patent: October 25, 2005
    Assignee: The United States of America as represented by the Secretary of the Navy
    Inventors: William E. O'Gardy, Graham T. Cheeck
  • Patent number: 6921473
    Abstract: A method of removing oxygen from a solid metal, metal compound or semi-metal M1O by electrolysis in a fused salt of M2Y or a mixture of salts, which comprises conducting electrolysis under conditions such that reaction of oxygen rather than M2 deposition occurs at an electrode surface and that oxygen dissolves in the electrolyte M2Y and wherein, M1O is in the form of (sintered) granules or is in the form of a powder which is continuously fed into the fused salt. Also disclosed is a method of producing a metal foam comprising the steps of fabricating a foam-like metal oxide preform, removing oxygen from said foam structured metal oxide preform by electrolysis in a fused salt of M2Y or a mixture of salts, which comprises conducting electrolysis under conditions such that reaction of oxygen rather than M2 deposition occurs at an electrode surface. The method is advantageously applied for the production of titanium from Ti-dioxide.
    Type: Grant
    Filed: February 20, 2001
    Date of Patent: July 26, 2005
    Assignee: Qinetiq Limited
    Inventors: Charles M Ward-Close, Alistair B Godfrey
  • Patent number: 6146513
    Abstract: The present invention includes uranium-bearing ceramic phase electrodes and electrolysis apparatus and electrolysis methods featuring same, including methods of metal production and the like by the electrolytic reduction of oxides or salts of the respective metals. More particularly, the invention relates to an inert type electrode composition, and methods for fabricating electrode compositions, useful in the electrolytic production of such metals. The present invention also includes an inert-type electrode composition, and methods for fabricating electrode compositions, used in processes for generating energy from fossil fuels.
    Type: Grant
    Filed: December 31, 1998
    Date of Patent: November 14, 2000
    Assignee: The Ohio State University
    Inventors: Kenneth H. Sandhage, Robert L. Snyder
  • Patent number: 6086745
    Abstract: A method of obtaining a new allotropic modification of metal zirconium and hafnium with layered structure consisting of double layered disposition of metal atoms with decreased interatomic distances in the doubled layers and increased interatomic distances between doubled layers in comparison with usual hexagonal close packed .alpha.-form of metal zirconium or hafnium is presented. The metal zirconium and hafnium with such a crystal structure are obtained by an electrochemical reduction process of solid zirconium monochloride or hafnium monochloride which serves as a cathode at a temperature about 450.degree. C. (830.degree. F.) in molten inorganic electrolyte consisting of lithium chloride and chlorides of alkali and alkaline earth metals in the presence of an inert anode, or metal zirconium or hafnium anode. X-ray analysis results of an obtained polymorphic modification of metal zirconium and resulting density are presented.
    Type: Grant
    Filed: July 3, 1997
    Date of Patent: July 11, 2000
    Inventor: Viatcheslav I. Tsirelnikov