EP0253841A1 - Verfahren zur herstellung von übergangsmetallpulver durch schmelzflusselektrolyse. - Google Patents

Verfahren zur herstellung von übergangsmetallpulver durch schmelzflusselektrolyse.

Info

Publication number
EP0253841A1
EP0253841A1 EP87900658A EP87900658A EP0253841A1 EP 0253841 A1 EP0253841 A1 EP 0253841A1 EP 87900658 A EP87900658 A EP 87900658A EP 87900658 A EP87900658 A EP 87900658A EP 0253841 A1 EP0253841 A1 EP 0253841A1
Authority
EP
European Patent Office
Prior art keywords
metal
electrolysis
bath
transition metal
baths
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP87900658A
Other languages
English (en)
French (fr)
Other versions
EP0253841B1 (de
Inventor
Marcel Armand
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pechiney SA
Original Assignee
Pechiney SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Pechiney SA filed Critical Pechiney SA
Publication of EP0253841A1 publication Critical patent/EP0253841A1/de
Application granted granted Critical
Publication of EP0253841B1 publication Critical patent/EP0253841B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
    • C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
    • C25C5/04—Electrolytic production, recovery or refining of metal powders or porous metal masses from melts

Definitions

  • the present invention relates to the preparation of powders of transition metals by electrolysis of their halides in baths of molten salts.
  • transition metals means any metal belonging to columns IVb, Vb, VIb of the periodic table.
  • powder means a solid substance, finely divided and containing grains ranging in size from a few micron fractions to about 200 microns.
  • the process which is the subject of the present invention consists in an electrolysis of a halide of the metal, in particular of its chloride, dissolved in a bath of molten salts based on alkali and / or alkaline earth halides, carried out under conditions particular.
  • the electrolytic processes, known for these metals lead in fact to deposits of excellent quality from the point of view of purity which are in the form of more or less massive or dendrltic crystals directly usable for melting, but unsuitable for metallurgy powders.
  • the method is characterized in that the electrolysis is carried out so that the deposition voltage of the metal to be obtained in powder form is 0.1 to 0.4 volt lower than that of the easiest alkali or alkaline earth metal to reduce and preferably less than 0.2 to 0.3 volts.
  • E 0 is the normal potential
  • R the constant of ideal gases
  • T the temperature in ° K
  • n the number of electrons exchanged
  • F the number of FARADAY
  • a the activity of metal ions in the solution.
  • Example 1 illustrates the application of the method according to the two modes described above.
  • Example 1 illustrates the application of the method according to the two modes described above.
  • the anode device further comprises a diaphragm which separates the bath into two compartments, an anode compartment which contains only traces of Titanium in solution, and a cathode compartment in which the content of dissolved Titanium is kept constant by a continuous feeding device.
  • the bath consists of an equimolecular mixture of potassium chlorides and sodium molten at 750 ° C.
  • the halide introduced is titanium tetrachloride.
  • the content of titanium dissolved in the bath is 4%.
  • the deposition voltage of titanium measured by drawing the voltage / current curve is 2.15 V., that of the alkali the easiest to reduce, in this case, the sodium is 3.2 V.
  • the deposits collected on the cathode are in the form of well crystallized dendrites which can reach several centimeters and meet the following analysis in ppm
  • the electrical efficiency is greater than 90%.
  • This example relates to Hafnium.
  • the halide introduced this time being hafnium tetrachloride, at the content of 25%, under normal conditions.
  • electrolysis i.e. with a current density of 1.0A / cm2
  • the Hafnium deposition voltage is 2.2 V. and deposits are obtained in the form of relatively massive dendrites (aspect of cauliflower) with an electrical efficiency greater than 95%.
  • the ratio here is equal to 12 but that with other metals with values of this ratio between 3 and 20 can be used; preferably the best results are obtained in the range of values between 6 and 12.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)
EP87900658A 1986-01-06 1987-01-05 Verfahren zur herstellung von übergangsmetallpulver durch schmelzflusselektrolyse Expired - Lifetime EP0253841B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8600390 1986-01-06
FR8600390A FR2592664B1 (fr) 1986-01-06 1986-01-06 Procede d'elaboration de poudres de metaux de transition par electrolyse en bains de sels fondus

Publications (2)

Publication Number Publication Date
EP0253841A1 true EP0253841A1 (de) 1988-01-27
EP0253841B1 EP0253841B1 (de) 1990-05-23

Family

ID=9331054

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87900658A Expired - Lifetime EP0253841B1 (de) 1986-01-06 1987-01-05 Verfahren zur herstellung von übergangsmetallpulver durch schmelzflusselektrolyse

Country Status (7)

Country Link
US (1) US4770750A (de)
EP (1) EP0253841B1 (de)
JP (1) JPS63500187A (de)
CA (1) CA1287814C (de)
DE (1) DE3762890D1 (de)
FR (1) FR2592664B1 (de)
WO (1) WO1987004193A1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991001942A1 (en) * 1989-08-01 1991-02-21 Australian Copper Company Pty. Ltd. Production of copper compounds

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE60130322T2 (de) * 2000-02-22 2008-06-12 Metalysis Ltd., Wath-Upon-Dearne Verfahren zur herstellung von metallschaum durch elektrolytische reduktion poröser oxidischer vorformen
WO2005111272A1 (ja) * 2004-04-06 2005-11-24 Iox Co., Ltd. プラズマ誘起電解による微粒子の製造方法
PL377451A1 (pl) * 2005-10-05 2007-04-16 Instytut Wysokich Ciśnień PAN Sposób prowadzenia reakcji i reaktor chemiczny
WO2013096893A1 (en) 2011-12-22 2013-06-27 Universal Technical Resource Services, Inc. A system and method for extraction and refining of titanium
JP7096235B2 (ja) 2016-09-14 2022-07-05 ユニバーサル アケメタル タイタニウム リミテッド ライアビリティ カンパニー チタン－アルミニウム－バナジウム合金の製造方法
WO2018186922A2 (en) 2017-01-13 2018-10-11 Universal Technical Resource Services, Inc. Titanium master alloy for titanium-aluminum based alloys

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2951021A (en) * 1952-03-28 1960-08-30 Nat Res Corp Electrolytic production of titanium
GB736567A (en) * 1952-07-03 1955-09-07 Horizons Titanium Corp Improvements in production of metallic titanium
FR1265427A (fr) * 1960-06-03 1961-06-30 Ciba Geigy Procédé d'élaboration électrolytique des métaux niobium et tantale

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO8704193A1 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991001942A1 (en) * 1989-08-01 1991-02-21 Australian Copper Company Pty. Ltd. Production of copper compounds

Also Published As

Publication number Publication date
WO1987004193A1 (fr) 1987-07-16
US4770750A (en) 1988-09-13
JPH0312156B2 (de) 1991-02-19
FR2592664B1 (fr) 1990-03-30
JPS63500187A (ja) 1988-01-21
EP0253841B1 (de) 1990-05-23
FR2592664A1 (fr) 1987-07-10
DE3762890D1 (de) 1990-06-28
CA1287814C (fr) 1991-08-20

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