US2995439A - Preparation of high purity chromium and other metals - Google Patents

Preparation of high purity chromium and other metals Download PDF

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US2995439A
US2995439A US790390A US79039059A US2995439A US 2995439 A US2995439 A US 2995439A US 790390 A US790390 A US 790390A US 79039059 A US79039059 A US 79039059A US 2995439 A US2995439 A US 2995439A
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metal
chromium
monosulfide
vanadium
metals
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US790390A
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Lawrence M Litz
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Union Carbide Corp
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Union Carbide Corp
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents

Definitions

  • This invention relates .to the purification of certain metals, and more particularly relates to a process of purifying metals utilizing a novel scavenging compound, thereby decreasing the impurity content and subsequently improving the metallurgical properties of such metals.
  • the hardness and ductility of metals are generally dependent upon their impurity content in addition to the inherent properties of the metals themselves. It would be greatly advantageous to purify certain metals, such as chromium and vanadium, thereby rendering them softer and occasionally more ductile than they are as presently available. Such improved ductility and softness will facilitate drawing, extruding, machining, and molding of such metals into desired shapes.
  • the invention comprises either heating a metal chosen from the group consisting of chromium and vanadium to an elevated temperature in the presence of cerium monosulfide, or heating the metal in question to an elevated temperature a d then placing cerium monosulfide in its presence.
  • a metal chosen from the group consisting of chromium and vanadium
  • the process of this invention may be carried out by heating such metal to above its melting point in contact with this compound.
  • Constant agitation at this elevated temperature may be beneficial in order to allow all of the metal to come into contact with the compound, thereby providing an inter face where purification occurs.
  • the invention may be carried out by heating a metal from the above-disclosed group in a container made of cerium monosulfide to effect the escape of gaseous impurities from the metal without substantial reaction occurring between the metal and the container.
  • a related method of purification encompasses adding the cerium monosulfide directly to a pool of the metal to be purified in the molten state. The mixture is desirably agitated for a given length of time, depending upon the impurity content of the metal and the temperature involved, and the purified metal is then recovered. It is important in the practice of any of the above-noted methods that the purification be carried out in a nonoxidizing inert atmosphere.
  • Such an atmosphere may be provided by evacuating the system or by blanketing it with an inert gas such as helium or argon. Heating of the metal may be accomplished by induction heating through the compound if such is used as the container for the metal to be purified, or by any other convenient means which contamination of the metal by the heating element.
  • an inert gas such as helium or argon.
  • chromium has been purified by heating it in a cerium monosulfide crucible to various temperatures between 50 C. and 150 C. above its melting point for periods of from 5 to 32 minutes, under an argon atmosphere.
  • the results of these test runs appear in summary form in Table A below.
  • a process for purifying a material consisting of a metal selected from the group consisting of vanadium, chromium, vanadium base alloys and chromium base alloys which comprises heating said material in the presence of independently produced cerium monosulfide to a temperature above the melting point of said material, at such elevated temperature for a sufiicient' time to render said metal relatively ductile, and cooling said metal.
  • a process for purifying vanadium metal which comprises heating said material in the presence of independently produced cerium monosulfide to a temperature above the melting point of said metal, agitating said metal at such elevated temperature for a suflicient time to render said metal relatively ductile, and cooling said metal.
  • a process for purifying chromium metal which comprises heating said material in the presence of independently produced cerium monosulfide to a temperature above the melting point of said metal, agitating said metal at such elevated temperature for a sufiicient time to render said metal relatively ductile, and cooling said metal.
  • a process for purifying chromium base alloys which comprises heating said alloy in the presence of independently produced cerium monosulfide to a temperature above the melting point of said alloy, agitating said alloy at such elevated temperature for a sufiicient time to render said alloy relatively ductile, and cooling said alloy.
  • a process for purifying vanadium base alloys which comprises heating said alloy in the presence of independently produced cerium monosulfide to a temperature above the melting point of said alloy, agitating said alloy at such elevated temperature for a suflicient time to render said alloy relatively ductile, and cooling said alloy.
  • a process for purifying a material consisting of a metal selected from the group consisting of vanadium, chromium, vanadium base alloys and chromium base alloys which comprises melting said material in a cerium monosulfide crucible under an inert atmosphere, agitating said molten material, superheating such during said agitation and cooling said purified material.
  • a process for purifying vanadium metal which comprises melting said metal in a cerium monosulfide crucible under an inert atmosphere, agitating said molten metal, superheating such during said agitation, and cooling said metal.
  • a process for purifying chromium metal which comprises melting said metal in a cerium monosulfide crucible under an inert atmosphere, agitating said molten metal, superheating such during said agitation, and cooling said metal.
  • a process for purifying chromium base alloys which comprises melting said alloy in a cerium monosulfide crucible under an inert atmosphere, agitating said molten alloy, superheating such during said agitation, and cooling said alloy.
  • a process for purifying vanadium base alloys which comprises melting said alloy in a cerium monosulfide crucible under an inert atmosphere, agitating said molten alloy, superheating such during said agitation, and cooling said alloy.
  • a process for purifying chromium which comprises melting said chromium in a cerium monosulfide crucible under an inert atmosphere, agitating said molten chromium for from 5 to 32 minutes, superheating said molten chromium between 50 C. and C. above the melting point thereof during said agitation, and cooling said chromium.

Description

United States Patent Ofiice Patented Aug. 8, 1961 2995 '43s PREPARATION or their PURITY CHROMIUM AND ornnn METAIS Lawrence M. Litz, Lakewood, Ohio, assiguor to Union Carbide Corporation, a corporation of New York No Drawing. Filed Feb. 2, 1959, Ser. No. 790,390 11 Claims. (Cl. 75-434) This invention relates .to the purification of certain metals, and more particularly relates to a process of purifying metals utilizing a novel scavenging compound, thereby decreasing the impurity content and subsequently improving the metallurgical properties of such metals.
The hardness and ductility of metals are generally dependent upon their impurity content in addition to the inherent properties of the metals themselves. It would be greatly advantageous to purify certain metals, such as chromium and vanadium, thereby rendering them softer and occasionally more ductile than they are as presently available. Such improved ductility and softness will facilitate drawing, extruding, machining, and molding of such metals into desired shapes.
It is therefore the primary object of this invention to produce purer metals of the above-disclosed group than have been available in the past. It is another object of this invention to provide a novel process for the purification of such metals thereby rendering them softer and occasionally more ductile than has been formerly possible.
In accord with and fulfilling the above-mentioned objects, the invention comprises either heating a metal chosen from the group consisting of chromium and vanadium to an elevated temperature in the presence of cerium monosulfide, or heating the metal in question to an elevated temperature a d then placing cerium monosulfide in its presence. Broadly, the process of this invention may be carried out by heating such metal to above its melting point in contact with this compound.
Constant agitation at this elevated temperature may be beneficial in order to allow all of the metal to come into contact with the compound, thereby providing an inter face where purification occurs.
More particularly, the invention may be carried out by heating a metal from the above-disclosed group in a container made of cerium monosulfide to effect the escape of gaseous impurities from the metal without substantial reaction occurring between the metal and the container. A related method of purification encompasses adding the cerium monosulfide directly to a pool of the metal to be purified in the molten state. The mixture is desirably agitated for a given length of time, depending upon the impurity content of the metal and the temperature involved, and the purified metal is then recovered. It is important in the practice of any of the above-noted methods that the purification be carried out in a nonoxidizing inert atmosphere. Such an atmosphere may be provided by evacuating the system or by blanketing it with an inert gas such as helium or argon. Heating of the metal may be accomplished by induction heating through the compound if such is used as the container for the metal to be purified, or by any other convenient means which contamination of the metal by the heating element.
It is to be understood that the above discussion of chromium and vanadium applies equally as well to chromium and vanadium base alloys.
As specific examples of the practice of this invention, chromium has been purified by heating it in a cerium monosulfide crucible to various temperatures between 50 C. and 150 C. above its melting point for periods of from 5 to 32 minutes, under an argon atmosphere. The results of these test runs appear in summary form in Table A below.
TABLE A Chromium melted in CeS 5 Run I Run 11 Run III Superheat, O., above melt- 50 75 140.
tng p0 Duration, Minutes 30 32 5. Helium Pressure, mm. Hg 380 380 100. Surface Appearance. Sllvery Silver-Yellow.-. Gold.
Chemical Analysis Run I Run II Run III Before Impurity Purificatlon nil 0. 079 0.04 0. 017 0.004 0.007 0.039 nil 0.012 0.047 N.T. 0.76 0.013 N.T. 0.05 Hardness: Diamond Pyrami 637 174 N.T. 205
1 N.T.Not tested.
TABLE B 35 Hardness 0. Pressure, Metal Superheat mm. Hg Standard Purified DPH DPH Vanadium 60 1x10 259 190 Dlamond Pyramid hardness.
Metallographic examination of vanadium showed a very significant reduction in impurity occlusions.
What is claimed is:
.1. A process for purifying a material consisting of a metal selected from the group consisting of vanadium, chromium, vanadium base alloys and chromium base alloys which comprises heating said material in the presence of independently produced cerium monosulfide to a temperature above the melting point of said material, at such elevated temperature for a sufiicient' time to render said metal relatively ductile, and cooling said metal.
2. A process for purifying vanadium metal which comprises heating said material in the presence of independently produced cerium monosulfide to a temperature above the melting point of said metal, agitating said metal at such elevated temperature for a suflicient time to render said metal relatively ductile, and cooling said metal.
3. A process for purifying chromium metal which comprises heating said material in the presence of independently produced cerium monosulfide to a temperature above the melting point of said metal, agitating said metal at such elevated temperature for a sufiicient time to render said metal relatively ductile, and cooling said metal.
4. A process for purifying chromium base alloys which comprises heating said alloy in the presence of independently produced cerium monosulfide to a temperature above the melting point of said alloy, agitating said alloy at such elevated temperature for a sufiicient time to render said alloy relatively ductile, and cooling said alloy.
5. A process for purifying vanadium base alloys which comprises heating said alloy in the presence of independently produced cerium monosulfide to a temperature above the melting point of said alloy, agitating said alloy at such elevated temperature for a suflicient time to render said alloy relatively ductile, and cooling said alloy.
6. A process for purifying a material consisting of a metal selected from the group consisting of vanadium, chromium, vanadium base alloys and chromium base alloys which comprises melting said material in a cerium monosulfide crucible under an inert atmosphere, agitating said molten material, superheating such during said agitation and cooling said purified material.
7. A process for purifying vanadium metal which comprises melting said metal in a cerium monosulfide crucible under an inert atmosphere, agitating said molten metal, superheating such during said agitation, and cooling said metal.
8. A process for purifying chromium metal which comprises melting said metal in a cerium monosulfide crucible under an inert atmosphere, agitating said molten metal, superheating such during said agitation, and cooling said metal.
9. A process for purifying chromium base alloys which comprises melting said alloy in a cerium monosulfide crucible under an inert atmosphere, agitating said molten alloy, superheating such during said agitation, and cooling said alloy.
10. A process for purifying vanadium base alloys which comprises melting said alloy in a cerium monosulfide crucible under an inert atmosphere, agitating said molten alloy, superheating such during said agitation, and cooling said alloy.
11. A process for purifying chromium which comprises melting said chromium in a cerium monosulfide crucible under an inert atmosphere, agitating said molten chromium for from 5 to 32 minutes, superheating said molten chromium between 50 C. and C. above the melting point thereof during said agitation, and cooling said chromium.
References Cited in the file of this patent UNITED STATES PATENTS 1,869,496 Osborg Aug. 2, 1932 1,869,979 Osborg Aug. 2, 1932 2,101,919 Schichtel Dec. 14, 1937 2,509,189 Jordan May 23, 1950 2,624,667 Tour Jan. 6, 1953 2,670,284 Zvanut Feb. 23, 1954 2,759,723v Crespi Aug. 21, 1956 2,766,110 Meister Oct. 9, 1956 2,801,099 Larson Ian. 30, 1957 FOREIGN PATENTS 1312/36 Australia Nov. 30, 1936

Claims (1)

1. A PROCESS FOR PURIFYING A MATERIAL CONSISTING OF A METAL SELECTED FROM THE GROUP CONSISTING OF VANADIUM, CHROMIUM, VANADIUM BASE ALLOYS AND CHROMIUM BASE ALLOYS WHICH COMPRISES HEATING SAID MATERIAL IN THE PRESENCE OF INDEPENDENTLY PRODUCED CERIUM MONOSULFIDE TO A TEMPERATURE ABOVE THE MELTING POINT OF SAID MATERIAL, AT SUCH ELEVATED TEMPERATURE FOR A SUFFICIENT TIME TO RENDER SAID METAL RELATIVELY DUCTILE, AND COOLING SAID METAL.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3146092A (en) * 1960-05-04 1964-08-25 Nat Distillers Chem Corp Process for purifying hafnium
US3386817A (en) * 1965-09-10 1968-06-04 Dow Chemical Co Process for the reduction of metal oxides
US5259866A (en) * 1990-10-23 1993-11-09 Japan Metals & Chemicals Co., Ltd. Method for producing high-purity metallic chromium

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1869979A (en) * 1930-09-06 1932-08-02 Osborg Hans Art of treating metals
US1869496A (en) * 1930-09-06 1932-08-02 Osborg Hans Art of treating metals
AU131236A (en) * 1936-04-01 1936-12-10 The Mono Nickel Company Limited Improvements inthe manufacture of alloys
US2101919A (en) * 1933-03-30 1937-12-14 American Magnesium Metals Corp Production of refined magnesium and magnesium alloys
US2509189A (en) * 1948-09-08 1950-05-23 Jordan James Fernando Process for the removal of sulfur from ferrous metals
US2624667A (en) * 1950-06-29 1953-01-06 Julius S W Bates Cartridge for below-surface treatment of molten metals
US2670284A (en) * 1950-06-28 1954-02-23 Olin Ind Inc Production of nonferrous alloys
US2759723A (en) * 1953-02-03 1956-08-21 Crespi Giovanni Compress laminated refractory block for metallurgical furnaces
US2766110A (en) * 1944-03-08 1956-10-09 Meister George Method of refining uranium
US2801099A (en) * 1954-04-14 1957-07-30 United States Steel Corp Monolithic liner and method of construction

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1869979A (en) * 1930-09-06 1932-08-02 Osborg Hans Art of treating metals
US1869496A (en) * 1930-09-06 1932-08-02 Osborg Hans Art of treating metals
US2101919A (en) * 1933-03-30 1937-12-14 American Magnesium Metals Corp Production of refined magnesium and magnesium alloys
AU131236A (en) * 1936-04-01 1936-12-10 The Mono Nickel Company Limited Improvements inthe manufacture of alloys
US2766110A (en) * 1944-03-08 1956-10-09 Meister George Method of refining uranium
US2509189A (en) * 1948-09-08 1950-05-23 Jordan James Fernando Process for the removal of sulfur from ferrous metals
US2670284A (en) * 1950-06-28 1954-02-23 Olin Ind Inc Production of nonferrous alloys
US2624667A (en) * 1950-06-29 1953-01-06 Julius S W Bates Cartridge for below-surface treatment of molten metals
US2759723A (en) * 1953-02-03 1956-08-21 Crespi Giovanni Compress laminated refractory block for metallurgical furnaces
US2801099A (en) * 1954-04-14 1957-07-30 United States Steel Corp Monolithic liner and method of construction

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3146092A (en) * 1960-05-04 1964-08-25 Nat Distillers Chem Corp Process for purifying hafnium
US3386817A (en) * 1965-09-10 1968-06-04 Dow Chemical Co Process for the reduction of metal oxides
US5259866A (en) * 1990-10-23 1993-11-09 Japan Metals & Chemicals Co., Ltd. Method for producing high-purity metallic chromium

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