US2803596A - Electro-cleaning of vanadium - Google Patents
Electro-cleaning of vanadium Download PDFInfo
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- US2803596A US2803596A US416585A US41658554A US2803596A US 2803596 A US2803596 A US 2803596A US 416585 A US416585 A US 416585A US 41658554 A US41658554 A US 41658554A US 2803596 A US2803596 A US 2803596A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/02—Etching
- C25F3/08—Etching of refractory metals
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- This invention pertains to vanadium, and more specifically relates to a method of electro-cleaning this metal in preparation for its cold working and to apparatus for doing the same.
- vanadium Because of its high afiinity for oxygen, vanadium acquires a hard and brittle skin surface when. itis, hot worked. Since oxygen dissolves in the vanadium to a high weight content during this process, no protective oxide coating forms on the metallic surface, but rather thereis formed a brittle layer beneath the oxide surface of the metal. When vanadium is cold worked in this condition, or if an attempt is made to straighten distorted bars of this metal, the oxygen-bearing surface metal cracks.
- vanadium metal bars and rods having a diameter greater than /2 inch have been finished by machining from hot rolled stock. Similar sizes were prepared by cold swaging /2 inch diameter machined parts. Machining the hard surface of vanadium is, however, a difficult as well as a wasteful practice since special rests and set-ups are necessary in the machining of long lengths of hot rolled bars, and sincethe ductile vanadium rising along the irregular metallic surface is thereby lost.
- the primary object of this invention to electrically clean vanadium metal so as to enable it to be cold worked without surface cracking, and simultaneously obtain a maximum recovery of ductile vanadium by eliminating the necessity of surface machining of the hot worked metal.
- Fig. 1 represents a convenient embodiment of this invention
- t Fig. 2 represents a further refinement of the invention.
- Sodium carbonate is the preferred electrolyte for this process, for in addition to being inexpensive, safe and easy to handle, it effectively electro-cleans vanadium with out pitting. With many other electrolytes, if current density is not properly adjusted, metal is removed, but the metallic surface is adversely affected. With sodium carbonate, current density is not critical in this respect.
- aqueous sodium carbonate solution ranging from 10% to 15% by weight is preferred, but concentrated solutions having as much as 35% sodium carbonate, the solubility limit of this compound in hot water, or as little as 5%, are also suitable in the practice of this invention.
- electrolytes having carbonate ions such as potas- "ice sium carbonate, ammonium carbonate and the like may also be used in this method in equivalent concentrations up to their saturation points as may also sodium bicarbonate, potassium bicarbonate and other similar electrolytes capable of providing bicarbonate ions.
- Current density values may vary between 0.26 and 1.2 amperes per square inch. In particular cases, current densities as high as 6 amperes per square inch may be used. The lower values indicated, however, are preferred, as they permit the exercise of better control over the cleaning operation, and'avoid possible excessive loss of sound metal.
- Quality control of the 'electro-cleaned vanadium metal is accomplished by hardness tests taken periodically during the electrolytic process.
- the electrolysis is preferably continued to a point at which the vanadium plate has a maximum of Rockwell B to B85 since this figure is sufiiciently low to allow its cold working.
- a vanadium plate measuring inch x 3 /2 inches x 13 inches was formed by hot rolling at 1150 C.
- This plate was prepared for electro-cleaning by sand blasting its surface to remove the heavy oxide film which covered it.
- the plate 10 then served as the anode and a stain less steel strip 112 as the cathode of an electrolytic cell 14 consisting of a hard rubber vat 16 filled with a 10% solution of sodium carbonate.
- a current of 20 amperes was applied for 22 hours, during which time periodic hardness tests were made on the vanadium plate. It was found after the complete treatment that the smooth and polished surface of the plate was completely free of its hard surface layer. During this process the plate thickness was reduced from 0.365 inch to 0.280 inch. It was subsequently cold rolled without any difliculty to 0.030 inch.
- a hot worked vanadium rod, 20, 0.550 inch in diameter by 36 inches in length was immersed in a steel pipe 22, which in addition to being the cell cathode, also served as the electrolytic cell as shown in Fig. 2..
- a 20% solution of sodium carbonate was supplied to this pipe, and a direct current of 15 amperes was applied for 4 /2 hours.
- the original diameter of the bar, 0.550 inch, was reduced to 0.440 inch.
- the brittle surface of the bar was cleaned equally on all sides. The electro-cleaned bar was then easily conventionally swaged to inch in ditools as is the case where the hard surface is not removed.”
- the present invention makes possible the removal of the contaminated outside layer of vanadium of high oxygen content resulting from the hot working process, by electro-cleaning, using carbonate or bicarbonate solutions as the electrolyte, thereby eliminating the machining step for rods to be cold swaged to sizes smaller than V2 inch, or for cold rolling vanadium plates to thin sheets.
- the method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having anaqueous electrolyte consisting of ions selected from the group consisting of the alkali metal carbonates and alkali metal bicarbonates, applying a direct current of pre-determined voltage and continuing electrolytic action until the brittle layer of the vanadium metal has been removed.
- the method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell, using an aqueous electrolyte consisting of alkali metal carbonate ions at a concentration range between 5% and 35%, and continuing electrolysis until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
- the method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having an aqueous electrolyte consisting of alkali metal carbonate ions, applying a direct current having a density between 0.2 and 6.0 ameres per square inch and continuing electrolytic action until the brittle layer of the vanadium metal has been removed.
- the method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell using an aqueous sodium carbonate electrolyte having a concentration range between 5% and 35%, and continuing electrolysis until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
- the method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell, using an aqueous sodium carbonate electrolyte having a concentration of about 10%, and continuing electrolysis under a current density ranging between 0.2 and 1.2 amperes per square inch until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
- the method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having an aqueous potassium carbonate electrolyte, and continuing electrolysis until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
- the method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having an ammonium carbonate electrolyte at a concentration range between 5% and saturation, and continuing electrolysis until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
- the method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell using a potassium carbonate electrolyte at a concentration range between 5% and saturation, and continuing electrolysis under a current density ranging between 0.2 and 6.0 amperes per square inch until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
- the method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell using an ammonium carbonate electrolyte at a concentration range between 5% and saturation, and continuing electrolysis under a current density rangingbetween 0.2 and 6.0 amperes per square inch until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
- the method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having an aqueous electrolyte consisting of bicarbonate ions, applying a direct current of predetermined voltage, and continuing electo lytic action until the brittle layer of the vanadium metal has been removed.
- the method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having an aqueous sodi um bicarbonate electrolyte at a concentration range between 5% and saturation, and continuing electrolysis until the vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform thickness is obtained.
- the method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having an aqueous potassium bicarbonate electrolyte at a concentration range between 5% and saturation, and continuing electrolysis until the vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform thickness is obtained.
Description
Aug. 2%; 1957 c. M. BROWN ELECTRO-CLEANING OF VANADIUM Sfainiess $feefl H (Cathode) Filed March 16, 1954 Vanadium (Anode) Vanadium INVENTOR CHARLES M. BROWN v ATTORNEY G d o n. A
United States Patent ELECTRO-CLEANING or VANADIUM Charles M. Brown, Lewiston, N. Y., assignor toUriion Carbide Corporation, a corporation of New York Application March 16, 1954, Serial No.'416,585
' 12 Claims. 01. 204-141 v This invention pertains to vanadium, and more specifically relates to a method of electro-cleaning this metal in preparation for its cold working and to apparatus for doing the same.
Because of its high afiinity for oxygen, vanadium acquires a hard and brittle skin surface when. itis, hot worked. Since oxygen dissolves in the vanadium to a high weight content during this process, no protective oxide coating forms on the metallic surface, but rather thereis formed a brittle layer beneath the oxide surface of the metal. When vanadium is cold worked in this condition, or if an attempt is made to straighten distorted bars of this metal, the oxygen-bearing surface metal cracks.
In the past, vanadium metal bars and rods having a diameter greater than /2 inch have been finished by machining from hot rolled stock. Similar sizes were prepared by cold swaging /2 inch diameter machined parts. Machining the hard surface of vanadium is, however, a difficult as well as a wasteful practice since special rests and set-ups are necessary in the machining of long lengths of hot rolled bars, and sincethe ductile vanadium rising along the irregular metallic surface is thereby lost.
It is, therefore, the primary object of this invention to electrically clean vanadium metal so as to enable it to be cold worked without surface cracking, and simultaneously obtain a maximum recovery of ductile vanadium by eliminating the necessity of surface machining of the hot worked metal.
It is another object of this invention to provide an inexpensive and safe electrolyte which will electro-clean vanadium without pitting its surface, and which does not require critical current densities.
These objects are attained in the practice of this invention, which comprises using vanadium metal as the anode of an electrolytic cell having a suitable cathode, an aqueous alkali metal carbonate or bicarbonate electrolyte, applying direct current of a predetermined voltage and suitable current density, and allowing electrolytic action to proceed until the hard, brittle metallic layer on the vanadium metal is removed.
In the drawings:
Fig. 1 represents a convenient embodiment of this invention; and t Fig. 2 represents a further refinement of the invention.
Sodium carbonate is the preferred electrolyte for this process, for in addition to being inexpensive, safe and easy to handle, it effectively electro-cleans vanadium with out pitting. With many other electrolytes, if current density is not properly adjusted, metal is removed, but the metallic surface is adversely affected. With sodium carbonate, current density is not critical in this respect.
An aqueous sodium carbonate solution ranging from 10% to 15% by weight is preferred, but concentrated solutions having as much as 35% sodium carbonate, the solubility limit of this compound in hot water, or as little as 5%, are also suitable in the practice of this invention.
Other electrolytes having carbonate ions such as potas- "ice sium carbonate, ammonium carbonate and the like may also be used in this method in equivalent concentrations up to their saturation points as may also sodium bicarbonate, potassium bicarbonate and other similar electrolytes capable of providing bicarbonate ions.
Current density values may vary between 0.26 and 1.2 amperes per square inch. In particular cases, current densities as high as 6 amperes per square inch may be used. The lower values indicated, however, are preferred, as they permit the exercise of better control over the cleaning operation, and'avoid possible excessive loss of sound metal.
Quality control of the 'electro-cleaned vanadium metal is accomplished by hardness tests taken periodically during the electrolytic process. The electrolysis is preferably continued to a point at which the vanadium plate has a maximum of Rockwell B to B85 since this figure is sufiiciently low to allow its cold working. These figures are not in any way critical, however. What is important is that excessively hard and contaminated outer layers of metal should be removed until a uniform base metal hardness is reached.
As an example of the practice of this invention, a vanadium plate measuring inch x 3 /2 inches x 13 inches was formed by hot rolling at 1150 C. This plate was prepared for electro-cleaning by sand blasting its surface to remove the heavy oxide film which covered it. The plate 10 then served as the anode and a stain less steel strip 112 as the cathode of an electrolytic cell 14 consisting of a hard rubber vat 16 filled with a 10% solution of sodium carbonate. A current of 20 amperes was applied for 22 hours, during which time periodic hardness tests were made on the vanadium plate. It was found after the complete treatment that the smooth and polished surface of the plate was completely free of its hard surface layer. During this process the plate thickness was reduced from 0.365 inch to 0.280 inch. It was subsequently cold rolled without any difliculty to 0.030 inch.
As a further example of the practice of this invention,
a hot worked vanadium rod, 20, 0.550 inch in diameter by 36 inches in length was immersed in a steel pipe 22, which in addition to being the cell cathode, also served as the electrolytic cell as shown in Fig. 2.. A 20% solution of sodium carbonate was supplied to this pipe, and a direct current of 15 amperes was applied for 4 /2 hours. The original diameter of the bar, 0.550 inch, was reduced to 0.440 inch. By the use of this modification of the invention, the brittle surface of the bar was cleaned equally on all sides. The electro-cleaned bar was then easily conventionally swaged to inch in ditools as is the case where the hard surface is not removed."
It is thus seen that the shape and size of the electro lytic cells employed in the practice of this: invention are not at all critical, butmay be varied within wide limits in order to accommodate anodes of various shapes and sizes.
In both examples given above, the recovery of vanadium in cold rolled bars or sheets after the electrolytic step is above as opposed to below 50% as occurs when the hot worked vanadium is machined prior to cold rolling.
The present invention makes possible the removal of the contaminated outside layer of vanadium of high oxygen content resulting from the hot working process, by electro-cleaning, using carbonate or bicarbonate solutions as the electrolyte, thereby eliminating the machining step for rods to be cold swaged to sizes smaller than V2 inch, or for cold rolling vanadium plates to thin sheets.
What is claimed is:
l. The method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having anaqueous electrolyte consisting of ions selected from the group consisting of the alkali metal carbonates and alkali metal bicarbonates, applying a direct current of pre-determined voltage and continuing electrolytic action until the brittle layer of the vanadium metal has been removed.
2. The method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell, using an aqueous electrolyte consisting of alkali metal carbonate ions at a concentration range between 5% and 35%, and continuing electrolysis until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
3. The method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having an aqueous electrolyte consisting of alkali metal carbonate ions, applying a direct current having a density between 0.2 and 6.0 ameres per square inch and continuing electrolytic action until the brittle layer of the vanadium metal has been removed.
4. The method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell using an aqueous sodium carbonate electrolyte having a concentration range between 5% and 35%, and continuing electrolysis until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
5. The method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell, using an aqueous sodium carbonate electrolyte having a concentration of about 10%, and continuing electrolysis under a current density ranging between 0.2 and 1.2 amperes per square inch until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
6. The method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having an aqueous potassium carbonate electrolyte, and continuing electrolysis until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
7. The method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having an ammonium carbonate electrolyte at a concentration range between 5% and saturation, and continuing electrolysis until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
8. The method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell using a potassium carbonate electrolyte at a concentration range between 5% and saturation, and continuing electrolysis under a current density ranging between 0.2 and 6.0 amperes per square inch until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
9. The method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell using an ammonium carbonate electrolyte at a concentration range between 5% and saturation, and continuing electrolysis under a current density rangingbetween 0.2 and 6.0 amperes per square inch until the said vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform hardness is obtained.
it). The method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having an aqueous electrolyte consisting of bicarbonate ions, applying a direct current of predetermined voltage, and continuing electo lytic action until the brittle layer of the vanadium metal has been removed.
11. The method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having an aqueous sodi um bicarbonate electrolyte at a concentration range between 5% and saturation, and continuing electrolysis until the vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform thickness is obtained.
12. The method of electrically removing the contaminated, high oxygen-containing surface layer of vanadium metal which comprises making the metal to be treated the anode of an electrolytic cell having an aqueous potassium bicarbonate electrolyte at a concentration range between 5% and saturation, and continuing electrolysis until the vanadium metal has been freed from the hard contaminated outer layers, and base metal of uniform thickness is obtained.
References Cited in the file of this patent UNITED STATES PATENTS 1,077,696 Fuller Nov. 4, 1913 1,347,897 'Coulson July 27, 1920 1,663,564 Rich Mar. 27, 1928 1,731,269 Rich Oct. 15, 1929 2,410,213 Herro et al. Oct. 29, 1946 FOREIGN PATENTS 514,365 Germany Dec. 11, 1930 OTHER REFERENCES Industrial and Engineering Chemistry, vol. 19 (1927), pages 786-788, article by Marden et al.
Claims (1)
1. THE METHOD OF ELECTRICALLY REMOVING THE CONTAMIUATED, HIGH OXYGEN-CONTAINING SURFACE LAYER OF VANADIUM METAL WHICH COMPRISES MAKING THE METAL TO BE TREATED THE ANODE OF AN ELECTROLYTIC CELL HAVING AN AQUEOUS ELECTROLYTE CONSISTING OF IONS SELECTED FROM THE GROUP CONSISTING OF THE ALKALI METAL CARBONATES AND ALKALI METAL BICARBONATES, APPLYING A DIRECT CURRENT OF PRE-DETERMINED VOLTAGE AND CONTINUING ELECTROLYTIC ACTION UNTIL THE BRITTLE LAYER OF THE VANADIUM METAL HAS BEEN REMOVED.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US416585A US2803596A (en) | 1954-03-16 | 1954-03-16 | Electro-cleaning of vanadium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US416585A US2803596A (en) | 1954-03-16 | 1954-03-16 | Electro-cleaning of vanadium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2803596A true US2803596A (en) | 1957-08-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| US416585A Expired - Lifetime US2803596A (en) | 1954-03-16 | 1954-03-16 | Electro-cleaning of vanadium |
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| US (1) | US2803596A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4060467A (en) * | 1971-01-15 | 1977-11-29 | Mitsubishi Denki Kabushiki Kaisha | Electrolytic machining system |
| US5160589A (en) * | 1991-06-13 | 1992-11-03 | Michelangelo Gionfriddo | Procedure for the reduction of the cross-section of a wire |
| US20090200173A1 (en) * | 2008-02-07 | 2009-08-13 | Shmuel Altman | Cleaning, pickling and electroplating apparatus |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1077696A (en) * | 1912-03-29 | 1913-11-04 | Gen Electric | Working tungsten. |
| US1347897A (en) * | 1917-11-03 | 1920-07-27 | Westinghouse Electric & Mfg Co | Electrolytic pickling process |
| US1663564A (en) * | 1925-10-30 | 1928-03-27 | Westinghouse Lamp Co | Refractory metal filament |
| US1731269A (en) * | 1925-01-23 | 1929-10-15 | Westinghouse Lamp Co | Pliable tungsten and method of producing the same |
| DE514365C (en) * | 1928-09-11 | 1930-12-11 | Hellmuth Hartmann Dr Ing | Process for the electrolytic extraction of metals, in particular tungsten |
| US2410213A (en) * | 1939-11-06 | 1946-10-29 | Carnation Co | Electrolytic can cleaner |
-
1954
- 1954-03-16 US US416585A patent/US2803596A/en not_active Expired - Lifetime
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US1077696A (en) * | 1912-03-29 | 1913-11-04 | Gen Electric | Working tungsten. |
| US1347897A (en) * | 1917-11-03 | 1920-07-27 | Westinghouse Electric & Mfg Co | Electrolytic pickling process |
| US1731269A (en) * | 1925-01-23 | 1929-10-15 | Westinghouse Lamp Co | Pliable tungsten and method of producing the same |
| US1663564A (en) * | 1925-10-30 | 1928-03-27 | Westinghouse Lamp Co | Refractory metal filament |
| DE514365C (en) * | 1928-09-11 | 1930-12-11 | Hellmuth Hartmann Dr Ing | Process for the electrolytic extraction of metals, in particular tungsten |
| US2410213A (en) * | 1939-11-06 | 1946-10-29 | Carnation Co | Electrolytic can cleaner |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4060467A (en) * | 1971-01-15 | 1977-11-29 | Mitsubishi Denki Kabushiki Kaisha | Electrolytic machining system |
| US5160589A (en) * | 1991-06-13 | 1992-11-03 | Michelangelo Gionfriddo | Procedure for the reduction of the cross-section of a wire |
| US20090200173A1 (en) * | 2008-02-07 | 2009-08-13 | Shmuel Altman | Cleaning, pickling and electroplating apparatus |
| US8241472B2 (en) | 2008-02-07 | 2012-08-14 | Shmuel Altman | Cleaning, pickling and electroplating apparatus |
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