US2492204A - Electrodeposition of gold on tantalum - Google Patents

Electrodeposition of gold on tantalum Download PDF

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Publication number
US2492204A
US2492204A US595381A US59538145A US2492204A US 2492204 A US2492204 A US 2492204A US 595381 A US595381 A US 595381A US 59538145 A US59538145 A US 59538145A US 2492204 A US2492204 A US 2492204A
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Prior art keywords
tantalum
gold
grid
electrodeposition
temperature
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Expired - Lifetime
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US595381A
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Russell D Van Gilder
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48—After-treatment of electroplated surfaces
    • C25D5/50—After-treatment of electroplated surfaces by heat-treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34—Pretreatment of metallic surfaces to be electroplated
    • C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/922—Static electricity metal bleed-off metallic stock
    • Y10S428/9265—Special properties
    • Y10S428/929—Electrical contact feature
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00—Stock material or miscellaneous articles
    • Y10S428/922—Static electricity metal bleed-off metallic stock
    • Y10S428/9335—Product by special process
    • Y10S428/934—Electrical process
    • Y10S428/935—Electroplating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12806—Refractory [Group IVB, VB, or VIB] metal-base component
    • Y10T428/12819—Group VB metal-base component
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
    • Y10T428/12771—Transition metal-base component
    • Y10T428/12861—Group VIII or IB metal-base component
    • Y10T428/12889—Au-base component

Definitions

  • My invention relates to the art of electroplating and more particularly, to a method of electrodepositing a strongly adherent, durable and wear-resistant film of gold on tantalum grids for electronic tubes.
  • My invention consists in first heating the tantalum metal preferably with an induction heating coil in a vacuum of the order of millimeters of mercury to a temperature of approximately 1900 C. After reaching this temperature the metal is allowed to cool before placing in an electroplating bath.
  • the electroplating bath used comprises gold chlorides and a cyanide salt.
  • Said bath may be prepared by dissolving 2.0 oz. of sodium cyanide in a quantity of lukewarm distilled water, a few ounces less than one U. S. gallon, then adding 0.5 oz. of gold chloride and making up to one gallon of solution.
  • a predetermined portion of said electroplating bath is used, depending upon the size of the tantalum metal to be electroplated.
  • the pretreated grid of tantalum metal, acting as the cathode, and an anode of gold or graphite are placed in an appropriate amount of said electroplating bath and maintained at a temperature of 70 C., while passing an electric current through said bath.
  • a very low current density is used, such as .01 ampere per square centimeter and a time limit of the order of 8 minutes.
  • the plated grid is then washed clean of said electroplating bath solution with distilled water and again placed in a vacuum of approximately 10- millimeters of mercury and heated with an induction heating coil to a temperature of approximately 1100 C. After cooling the plated tantalum grid is ready for use.
  • the weight of gold plated on will be of the order of .3560 gram, when the initial weight of said tantalum grid is of the order of 4.0228 grams. This will give a thickness of plated gold of 1 mil on a 5 mil tantalum wire.
  • the method of electrodepositing a strongly adherent gold film on tantalum grids of electronic tubes comprising heating said tantalum grid in a vacuum to a temperature of approximately 1900" C., allowing said tantalum grid to cool after it had reached said temperature, electrodepositing a, gold film on said tantalum grid from an electroplating bath solution consisting essentially of gold chloride, sodium cyanide and water, rinsing the plated metal from said electroplating bath solution and heating said plated grid in a vacuum to a temperature of approximately 1100 C.
  • the method of electrodepositing a strongly adherent gold film on tantalum grids of electronic tubes comprising heating said tantalum grid with an induction heating coil in a vacuum of approximately 10" millimeter of mercury to a temperature of approximately 1900 C., allowing said tantalum to cool after it had reached said temperature, electrodepositing a gold film on said tantalum grid from an electroplating bath solution consisting essentially of gold chloride, sodium cyanide and water, rinsing the plated metal from said electroplating bath solution and heating said plated grid in a vacuum to a temperature of approximately 1100 C.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electroplating And Plating Baths Therefor (AREA)

Description

Patented Dec. 27, 1949 ANTALU Russell D. Van Gilder, Avalon, Pa.--,Tassignor to the United States of America as represented by the Secretary of War No Drawing. Application May 23, 1945, Serial No. 595,381
(Granted under the act of March 3, 1883, as amended April 30, 1928; 370 0. G. 757) 2 Claims.
The invention described herein may be manufactured and used by or for the Government for governmental purposes, without the payment to me of any royalty thereon.
My invention relates to the art of electroplating and more particularly, to a method of electrodepositing a strongly adherent, durable and wear-resistant film of gold on tantalum grids for electronic tubes.
The difiiculties encountered in electroplating tantalum with precious metals are well known to the art. Such electrodepositions do not bond to the tantalum and can be stripped with ease.
It is the object of my invention to provide a method by which tantalum grids for electronic tubes may be electroplated with a very thin but strongly adherent gold film which will withstand all stresses and strains which the grid has to undergo while the tube is in operation.
Other objects and advantages of my invention will become apparent from the following description.
My invention consists in first heating the tantalum metal preferably with an induction heating coil in a vacuum of the order of millimeters of mercury to a temperature of approximately 1900 C. After reaching this temperature the metal is allowed to cool before placing in an electroplating bath.
In my method of the electrodeposition of gold on tantalum metal the electroplating bath used comprises gold chlorides and a cyanide salt. Said bath may be prepared by dissolving 2.0 oz. of sodium cyanide in a quantity of lukewarm distilled water, a few ounces less than one U. S. gallon, then adding 0.5 oz. of gold chloride and making up to one gallon of solution. A predetermined portion of said electroplating bath is used, depending upon the size of the tantalum metal to be electroplated.
The pretreated grid of tantalum metal, acting as the cathode, and an anode of gold or graphite are placed in an appropriate amount of said electroplating bath and maintained at a temperature of 70 C., while passing an electric current through said bath. A very low current density is used, such as .01 ampere per square centimeter and a time limit of the order of 8 minutes. The plated grid is then washed clean of said electroplating bath solution with distilled water and again placed in a vacuum of approximately 10- millimeters of mercury and heated with an induction heating coil to a temperature of approximately 1100 C. After cooling the plated tantalum grid is ready for use. In following the above described method of electrodeposition of gold on said tantalum grid the weight of gold plated on will be of the order of .3560 gram, when the initial weight of said tantalum grid is of the order of 4.0228 grams. This will give a thickness of plated gold of 1 mil on a 5 mil tantalum wire.
It is to be understood that variations and modifications may be made within the scope of my invention as those skilled in the art will readily understand.
Having thus described my invention I desire to secure by Letters Patent and claim:
1. The method of electrodepositing a strongly adherent gold film on tantalum grids of electronic tubes comprising heating said tantalum grid in a vacuum to a temperature of approximately 1900" C., allowing said tantalum grid to cool after it had reached said temperature, electrodepositing a, gold film on said tantalum grid from an electroplating bath solution consisting essentially of gold chloride, sodium cyanide and water, rinsing the plated metal from said electroplating bath solution and heating said plated grid in a vacuum to a temperature of approximately 1100 C.
2. The method of electrodepositing a strongly adherent gold film on tantalum grids of electronic tubes comprising heating said tantalum grid with an induction heating coil in a vacuum of approximately 10" millimeter of mercury to a temperature of approximately 1900 C., allowing said tantalum to cool after it had reached said temperature, electrodepositing a gold film on said tantalum grid from an electroplating bath solution consisting essentially of gold chloride, sodium cyanide and water, rinsing the plated metal from said electroplating bath solution and heating said plated grid in a vacuum to a temperature of approximately 1100 C.
RUSSELL D. VAN GILDER.
(References on following page) REFERENCES CITED OTHER REFERENCES The following references are of record in the Electrodeposition of Metals, by G. Langbein. file of this patent: 1924, pages 510, 511, 512.
Transactions of the American Electrochemical UNHED STATES PATENTS Society, vol. 23 (1913), pages 32-34. Number Name Date The Metal Tantalum, published by Fansteel 6 71 Aylsworth Ju y 1 1904 Metallurgical 00., N. Chicago, 111., 1939, pages 1,803,691 Brockway May 5, 19 1 4, 9, 2,093,845 c a p 1937 Industrial and Engineering Chemistry, 27 2,107,277 Austin Feb. 1 (1935), pages 1166, 1167. 2,116,927 Germer May 10, 1938 2,133,995 Lukens Oct. 25, 1938 FOREIGN PATENTS Number Country Date 1 5 797,485 France Feb. 17, 1936
US595381A 1945-05-23 1945-05-23 Electrodeposition of gold on tantalum Expired - Lifetime US2492204A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2719797A (en) * 1950-05-23 1955-10-04 Baker & Co Inc Platinizing tantalum
US2928169A (en) * 1957-01-07 1960-03-15 John G Beach Electroplated articles having molybdenum base metal
US3071522A (en) * 1958-10-30 1963-01-01 Bell Telephone Labor Inc Low resistance contact for semiconductors
US4655884A (en) * 1985-08-19 1987-04-07 General Electric Company Nickel plating of refractory metals
US11753736B2 (en) 2020-11-16 2023-09-12 Raytheon Company Indium electroplating on physical vapor deposition tantalum

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US765371A (en) * 1903-09-15 1904-07-19 Edison Storage Battery Co Process of nickel-plating.
US1803691A (en) * 1928-11-28 1931-05-05 World Bestos Corp Process and apparatus for plating wire
FR797485A (en) * 1935-01-28 1936-04-27 Sani Chrome Bath for electroplating metals on any conductive surfaces
US2093845A (en) * 1935-09-06 1937-09-21 Philip M Mckenna Method of producing hard compositions of matter
US2107277A (en) * 1932-04-14 1938-02-08 Fansteel Metallurgical Corp Tantalum recovery
US2116927A (en) * 1935-04-20 1938-05-10 Germer Edmund Electrical discharge device
US2133995A (en) * 1937-12-16 1938-10-25 Howard Hunt Pen Company C Process for gold plating chromium alloy steels

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US765371A (en) * 1903-09-15 1904-07-19 Edison Storage Battery Co Process of nickel-plating.
US1803691A (en) * 1928-11-28 1931-05-05 World Bestos Corp Process and apparatus for plating wire
US2107277A (en) * 1932-04-14 1938-02-08 Fansteel Metallurgical Corp Tantalum recovery
FR797485A (en) * 1935-01-28 1936-04-27 Sani Chrome Bath for electroplating metals on any conductive surfaces
US2116927A (en) * 1935-04-20 1938-05-10 Germer Edmund Electrical discharge device
US2093845A (en) * 1935-09-06 1937-09-21 Philip M Mckenna Method of producing hard compositions of matter
US2133995A (en) * 1937-12-16 1938-10-25 Howard Hunt Pen Company C Process for gold plating chromium alloy steels

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2719797A (en) * 1950-05-23 1955-10-04 Baker & Co Inc Platinizing tantalum
US2928169A (en) * 1957-01-07 1960-03-15 John G Beach Electroplated articles having molybdenum base metal
US3071522A (en) * 1958-10-30 1963-01-01 Bell Telephone Labor Inc Low resistance contact for semiconductors
US4655884A (en) * 1985-08-19 1987-04-07 General Electric Company Nickel plating of refractory metals
US11753736B2 (en) 2020-11-16 2023-09-12 Raytheon Company Indium electroplating on physical vapor deposition tantalum

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