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US3634207A - Nickel etching and plating bath - Google Patents

Nickel etching and plating bath Download PDF

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Publication number
US3634207A
US3634207A US855420A US3634207DA US3634207A US 3634207 A US3634207 A US 3634207A US 855420 A US855420 A US 855420A US 3634207D A US3634207D A US 3634207DA US 3634207 A US3634207 A US 3634207A
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Prior art keywords
nickel
bath
plating
plating bath
sulfate
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US855420A
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Emil Toledo
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US Department of Navy
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US Department of Navy
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Classifications

    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/12Electroplating: Baths therefor from solutions of nickel or cobalt
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34Pretreatment of metallic surfaces to be electroplated
    • C25D5/38Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
    • C25D5/40Nickel; Chromium

Definitions

  • Collettid ABSTRACT A process for plating nickel onto a nickel surface comprising first etching said nickel surface by anodic treatment in a bath, and then electroplating in the same bath.
  • the bath is comprised of nickel chloride, nickel sulfate and boric acid to which are added small amounts of a brightener and a wetting agent.
  • the present invention relates to a process for electroplating nickel onto a nickel surface and has particular utility in applying a nickel coating onto a nickel coated printed circuit board.
  • baths and processes for electroplating nickel are described in Principles of Electroplating and Electroforming, by Blum and Hogaboom, pages 362-381, revised third addition, 1949, McGraw-Hill Book Co., Inc., New York; and in Modern Electroplating," edited by A. G. Gray, the Electrochemical Society, 1953, pages 299-355.
  • baths for electroplating nickel contain nickel sulfate, a chloride, such as nickel chloride, a buffering agent, such as boric acid, and a wetting agent such as sodium lauryl sulfate, sodium lauryl ether sulfate or sodium 7-ethyl-2-methyl-4-undecanol sulfate.
  • Such baths include the well-known Watts bath and other baths containing, as the source of the nickel, a combination of nickel fluoborate with nickel sulfate and nickel chloride, or a combination of nickel fluoborate with nickel chloride.
  • the present invention provides an improved process for plating nickel onto a nickel surface by providing a bath which serves as both a cleaning bath and a plating bath.
  • the article is first reverse plated, that is, the article is immersed as anode in the bath and, after about 1 minute of current application, the
  • the bath is a nickel sulfate-nickel chloride bath to which a buffering agent, a brightener, and a wetting agent are added.
  • EXAMPLE I A nickel coated printed circuit board having an area of 1.7 square inches was prepared for plating by first cleaning. The article was degreased in a methanol rinse and then dipped in an acid bath (50 percent I-ICI dip at about F The plating bath was comprised as follows:
  • Nickel chloride 10 ozJgal. Nickel sulfate 30 oz./gal. Boric acid 5 oz./gal. Saccharine 0.1 oz./gal. Sodium lauryl sulfate 0.0] oz./gal. Temperature I60 F.
  • a nickel coated printed circuit board was reverse plated for 1 minute at 500 ma. in the plating bath and then plated at 500 ma. for 1 hour without removing the circuit board from the plating bath after reverse plating.
  • a process for electroplating nickel onto a thin nickelcoated surface on a printed circuit board comprising first removing oxide coating from said nickel-coated surface by reverse plating in a bath with said nickel-coated surface being connected as anode and then plating in the same bath with said nickel-coated surface being connected as cathode, said bath consisting of about 10 oz./gal. of nickel chloride, about 30 oz./gal. of nickel sulfate, about 5 oz./gal. of boric acid, about 0.1 oz./gal. of saccharine, about 0.0l oz./gal. of sodium lauryl sulfate and the balance of water.

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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 Methods And Accessories (AREA)

Abstract

A process for plating nickel onto a nickel surface comprising first etching said nickel surface by anodic treatment in a bath, and then electroplating in the same bath. The bath is comprised of nickel chloride, nickel sulfate and boric acid to which are added small amounts of a brightener and a wetting agent.

Description

United States Patent Emil Toledo Natick, Mass.
Sept. 4, 1969 Jan. 11, 1972 The United States of America as represented by the Secretary of the Navy Inventor Appl. No. Filed Patented Assignee NICKEL ETCHING AND PLATING BATH 2 Claims, No Drawings US. Cl 204/32 R, 204/49 Int. Cl C23b 3/02 Field of Search 204/32 R, 33, 49,141, 325, 34, 20, 30
References Cited UNITED STATES PATENTS 6/1942 Wesley et al 204/34 4/1940 Lindetal 2,198,268 204/49 2,299,054 10/1942 Harshaw et al. 204/14] 2,702,785 2/1955 Eyerund 204/33 OTHER REFERENCES Smith, R. S. Nickel Plating Directly onto Aluminum, IBM Technical Disclosure Bulletin. Vol. 9, No. 8, January 1967.
Primary Examiner-John H. Mack Assistant Examiner-W. l. Solomon Att0rneys- Edgar J. Brower, H. H. Losche and Paul S.
Collignon ABSTRACT: A process for plating nickel onto a nickel surface comprising first etching said nickel surface by anodic treatment in a bath, and then electroplating in the same bath. The bath is comprised of nickel chloride, nickel sulfate and boric acid to which are added small amounts of a brightener and a wetting agent.
NICKEL ETCI-IING AND PLATING BATH BACKGROUND OF THE INVENTION The present invention relates to a process for electroplating nickel onto a nickel surface and has particular utility in applying a nickel coating onto a nickel coated printed circuit board.
One of the major problems that must be overcome to obtain good adhesion on a nickel coated printed circuit board is the removal of its passive nickel oxide coating in a manner which will not affect its thin nickel coating. Most mild-cleaning methods, such as a HCl dip, do not completely remove the oxide coating and more active cleaning methods, such as electroetching and electropolishing can damage the thin nickel coating on the printed circuit board.
Conventional baths and processes for electroplating nickel are described in Principles of Electroplating and Electroforming, by Blum and Hogaboom, pages 362-381, revised third addition, 1949, McGraw-Hill Book Co., Inc., New York; and in Modern Electroplating," edited by A. G. Gray, the Electrochemical Society, 1953, pages 299-355. Almost all baths for electroplating nickel contain nickel sulfate, a chloride, such as nickel chloride, a buffering agent, such as boric acid, and a wetting agent such as sodium lauryl sulfate, sodium lauryl ether sulfate or sodium 7-ethyl-2-methyl-4-undecanol sulfate. Such baths include the well-known Watts bath and other baths containing, as the source of the nickel, a combination of nickel fluoborate with nickel sulfate and nickel chloride, or a combination of nickel fluoborate with nickel chloride.
Various methods have been employed in the past to cleanse the nickel oxide film from a part which is to receive subsequent plating. In U.S. Pat. No. 2,299,054, which was issued Oct. 13, 1942, to William J. Harshaw and Kenneth E. Long, there is described an anodic-cathodic treatment for preparing a nickel plated article for chromium plating. The nickel plated article is placed in an aqueous solution of sodium cyanide and connected as an anode while passing an electric current therethrough as a voltage of from 2 to 10 volts for a period of about 1 second. The current is then reversed, by connecting the piece as a cathode for a few seconds.
Another anodic method for cleaning nickel is described in U.S. Pat. No. 3,362,894, which issued Jan. 9, 1968, to William A. Pennington and Stephen D. Cramer. In this patent, a cleaning method for nickel is described wherein a metal substrate is given an anodic treatment in a concentrated aqueous solution of a lithium halide. The metal substrate is then rinsed and plated in a conventional plating bath.
SUMMARY OF THE INVENTION The present invention provides an improved process for plating nickel onto a nickel surface by providing a bath which serves as both a cleaning bath and a plating bath. The article is first reverse plated, that is, the article is immersed as anode in the bath and, after about 1 minute of current application, the
current flow is reversed and the article is connected as cathode in the bath. Plating is accomplished in the normal manner. The bath is a nickel sulfate-nickel chloride bath to which a buffering agent, a brightener, and a wetting agent are added.
DESCRIPTION OF THE PREFERRED EMBODIMENT ticing the present invention.
EXAMPLE I A nickel coated printed circuit board having an area of 1.7 square inches was prepared for plating by first cleaning. The article was degreased in a methanol rinse and then dipped in an acid bath (50 percent I-ICI dip at about F The plating bath was comprised as follows:
Nickel chloride 10 ozJgal. Nickel sulfate 30 oz./gal. Boric acid 5 oz./gal. Saccharine 0.1 oz./gal. Sodium lauryl sulfate 0.0] oz./gal. Temperature I60 F.
A nickel coated printed circuit board was reverse plated for 1 minute at 500 ma. in the plating bath and then plated at 500 ma. for 1 hour without removing the circuit board from the plating bath after reverse plating.
Bend tests and metallurgical examinations revealed the plated product had excellent adhesion. Leads were welded to the plated product and pull tests were conducted by pulling on the leads both parallel and perpendicular to the surface. Metallographic examination revealed that adhesion between nickel layers was satisfactory.
I claim:
1. A process for electroplating nickel onto a thin nickelcoated surface on a printed circuit board comprising first removing oxide coating from said nickel-coated surface by reverse plating in a bath with said nickel-coated surface being connected as anode and then plating in the same bath with said nickel-coated surface being connected as cathode, said bath consisting of about 10 oz./gal. of nickel chloride, about 30 oz./gal. of nickel sulfate, about 5 oz./gal. of boric acid, about 0.1 oz./gal. of saccharine, about 0.0l oz./gal. of sodium lauryl sulfate and the balance of water.
2. The process as set forth in claim I wherein said reverse plating is carried on for about 1 minute and said plating is carried on for about 60 minutes.

Claims (1)

  1. 2. The process as set forth in claim 1 wherein said reverse plating is carried on for about 1 minute and said plating is carried on for about 60 minutes.
US855420A 1969-09-04 1969-09-04 Nickel etching and plating bath Expired - Lifetime US3634207A (en)

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US85542069A 1969-09-04 1969-09-04

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5164069A (en) * 1990-11-05 1992-11-17 Shipley Company Inc. Nickel electroplating solution and acetylenic compounds therefor
US20130341197A1 (en) * 2012-02-06 2013-12-26 Honeywell International Inc. Methods for producing a high temperature oxidation resistant mcralx coating on superalloy substrates
RU2626700C1 (en) * 2016-02-10 2017-07-31 Федеральное государственное бюджетное образовательное учреждение высшего образования "Саратовский государственный технический университет имени Гагарина Ю.А." (ФГБОУ ВПО "СГТУ имени Гагарина Ю.А.") Method of electrochemical application of nickel coating
US10087540B2 (en) 2015-02-17 2018-10-02 Honeywell International Inc. Surface modifiers for ionic liquid aluminum electroplating solutions, processes for electroplating aluminum therefrom, and methods for producing an aluminum coating using the same
US11965265B1 (en) 2020-01-30 2024-04-23 The United States Of America As Represented By The Secretary Of The Navy Hybrid electro-processing of a metal workpiece

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2198268A (en) * 1939-12-14 1940-04-23 Harshaw Chem Corp Electrodeposition of metals
US2285549A (en) * 1938-04-26 1942-06-09 Int Nickel Co Process of electrodepositing an adherent layer of copper from copper refinery electrolyte on alloys of iron and/or nickel containing chromium
US2299054A (en) * 1939-06-20 1942-10-13 Harshaw Chem Corp Electroplating
US2702785A (en) * 1950-06-16 1955-02-22 Metallgesellschaft Ag Process of producing hard chromium platings on light metals

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2285549A (en) * 1938-04-26 1942-06-09 Int Nickel Co Process of electrodepositing an adherent layer of copper from copper refinery electrolyte on alloys of iron and/or nickel containing chromium
US2299054A (en) * 1939-06-20 1942-10-13 Harshaw Chem Corp Electroplating
US2198268A (en) * 1939-12-14 1940-04-23 Harshaw Chem Corp Electrodeposition of metals
US2702785A (en) * 1950-06-16 1955-02-22 Metallgesellschaft Ag Process of producing hard chromium platings on light metals

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Smith, R. S. Nickel Plating Directly onto Aluminum, IBM Technical Disclosure Bulletin. Vol. 9, No. 8, January 1967. *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5164069A (en) * 1990-11-05 1992-11-17 Shipley Company Inc. Nickel electroplating solution and acetylenic compounds therefor
US20130341197A1 (en) * 2012-02-06 2013-12-26 Honeywell International Inc. Methods for producing a high temperature oxidation resistant mcralx coating on superalloy substrates
US9771661B2 (en) * 2012-02-06 2017-09-26 Honeywell International Inc. Methods for producing a high temperature oxidation resistant MCrAlX coating on superalloy substrates
US10087540B2 (en) 2015-02-17 2018-10-02 Honeywell International Inc. Surface modifiers for ionic liquid aluminum electroplating solutions, processes for electroplating aluminum therefrom, and methods for producing an aluminum coating using the same
RU2626700C1 (en) * 2016-02-10 2017-07-31 Федеральное государственное бюджетное образовательное учреждение высшего образования "Саратовский государственный технический университет имени Гагарина Ю.А." (ФГБОУ ВПО "СГТУ имени Гагарина Ю.А.") Method of electrochemical application of nickel coating
US11965265B1 (en) 2020-01-30 2024-04-23 The United States Of America As Represented By The Secretary Of The Navy Hybrid electro-processing of a metal workpiece

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