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EP0168705B1 - Bain et procédé d'électroplacage d'or dur - Google Patents

Bain et procédé d'électroplacage d'or dur Download PDF

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Publication number
EP0168705B1
EP0168705B1 EP85108129A EP85108129A EP0168705B1 EP 0168705 B1 EP0168705 B1 EP 0168705B1 EP 85108129 A EP85108129 A EP 85108129A EP 85108129 A EP85108129 A EP 85108129A EP 0168705 B1 EP0168705 B1 EP 0168705B1
Authority
EP
European Patent Office
Prior art keywords
bath
aqueous solution
gold
hard
solution contains
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.)
Expired
Application number
EP85108129A
Other languages
German (de)
English (en)
Other versions
EP0168705A1 (fr
Inventor
Jacky Dr. Vanhumbeeck
Rudy De Doncker
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.)
Siemens AG
Original Assignee
Siemens AG
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
Priority claimed from DE19853509245 external-priority patent/DE3509245A1/de
Application filed by Siemens AG filed Critical Siemens AG
Priority to AT85108129T priority Critical patent/ATE38061T1/de
Publication of EP0168705A1 publication Critical patent/EP0168705A1/fr
Application granted granted Critical
Publication of EP0168705B1 publication Critical patent/EP0168705B1/fr
Expired legal-status Critical Current

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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
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/56—Electroplating: Baths therefor from solutions of alloys
    • C25D3/62—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of gold
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/48—Electroplating: Baths therefor from solutions of gold
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
    • H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
    • H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
    • H01H11/041—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by bonding of a contact marking face to a contact body portion
    • H01H2011/046—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by bonding of a contact marking face to a contact body portion by plating

Definitions

  • the invention relates to an acidic cyanide bath for the galvanic hard gold plating of electrical contact components according to the preamble of claim 1, and methods for the galvanic hard gold plating of electrical contact components using this bath.
  • Galvanic gold deposits are characterized by their excellent corrosion resistance and their relatively good electrical properties. These two properties are of particular importance in the case of electrical contact components such as connectors, contacts for relays and switches and the like, since here the galvanically deposited gold layers have to take over the corrosion protection of the carrier material and the loss-free transmission of the energy. Great importance is attached to a low and constant contact resistance. With regard to the mechanical stress on the contact components, the hardness and wear resistance of the gold layers also play an important role. Corresponding abrasion-resistant hard gold layers are mostly produced from baths that contain so-called hardness additives, with the metals cobalt and nickel being used as hardness additives in particular.
  • base metals such as cobalt and nickel
  • other properties of the deposited layers can also be influenced.
  • the base metals diffuse to the surface of the deposited layers and thereby lead to an undesirable increase in the contact resistance.
  • the invention is based on an acidic cyanide bath known from DE-PS 3 121 509, which uses potassium gold cyanide as a gold source, malic acid as a conductive salt, nitrilotriacetic acid as a complexing agent, cobalt sulfate as a hardness additive and for adjusting a pH between 3.8 and 4.7 Contains potassium hydroxide.
  • the gold layers deposited from this bath are hard and wear-resistant.
  • Additive-free bath for galvanic hard gold plating which as the gold source is alkali gold cyanide. contains in particular potassium gold cyanide, potassium dihydrogen phosphate as a buffer system and possibly potassium hydroxide and hydrazine hydrate as a reducing agent.
  • the term additive-free bath is intended to express that hardness additives such as cobalt or nickel can be dispensed with entirely or should only be present in small amounts of less than 10 mg / l.
  • the gold layers deposited from this additive-free bath are hard, so-called adhesive wear occurs in electrical contact components such as connectors and the like. If there is friction between two such gold layers, they can weld to one another, which then leads to corresponding wear.
  • an acidic cyanide gold bath which contains gold as sodium gold cyanide or potassium gold cyanide, cobalt or nickel in the form of a water-soluble salt of a hydroxycarboxylic acid and a mixture contains two hydroxycarboxylic acids - such as citric acid and trihydroxyglutamic acid or malic acid and tetrahydroxyadipic acid.
  • pH values between 3.8 and 6.0 and bath temperatures between 20 and 50 ° C shiny gold layers are deposited with current densities between 0.1 and 1.5 A / dm 2 .
  • galvanic hard gold plating of parts of mass production - such as electrical contact components - higher current densities or higher deposition rates are required for economical work.
  • an acidic cyanide bath for galvanic hard gold plating which in aqueous solution alkali gold cyanide - such as.
  • alkali gold cyanide - such as.
  • potassium gold cyanide or sodium gold cyanide - a weak Lewis acid - such as. B. quinaldic acid or boric acid -, a weak polyfunctional water-soluble aliphatic acid - such.
  • citric acid or malic acid - a non-separating metal compound - such as. B. an aluminum, barium or magnesium compound - and as a hardening additive contains a metal such as cobalt, nickel, cadmium, silver, copper, iron or platinum in the form of a water-soluble salt.
  • the hard gold layers are deposited with current densities between 0.05 and 2.1 A / dm 2 .
  • a simpler composition of the bath and the achievement of higher current densities would be desirable.
  • the invention has for its object to provide a bath for the galvanic hard gold plating of contact components, which has a simple composition and an economy hard and wear-resistant gold layers with low and, above all, constant contact resistance. This object is achieved in a generic bath by the characterizing features of claim 1.
  • the invention is based on the finding that in the bath known from DE-PS 3 121 509, the nitrilotriacetic acid provided as a complexing agent can be omitted without substitute, provided that the concentrations specified in the characterizing features of claim 1 are observed for the other constituents of the bath.
  • the malic acid contained in the bath according to the invention thus acts simultaneously as a conductive salt, as a buffer and as a complexing agent.
  • the gold layers deposited from the bath are hard and wear-resistant and have a low contact resistance.
  • the aqueous solution can be free from additions of hardness, whereby matt precipitates are deposited which are hard and wear-resistant and have low contact resistances with a particularly good stability over time.
  • the aqueous solution can also contain 30 to 250 mg / l, preferably 40 to 100 mg / l as a hardness additive and approximately 50 mg / l cobalt or 50 to 300 mg / l as an optimum and approximately 100 mg / l as an optimum Contain nickel.
  • shiny precipitates are deposited, which are hard and wear-resistant and have low, constant contact resistances over time.
  • the current density window in which acceptable precipitation is achieved, is considerably larger than in an additive-free bath.
  • the aqueous solution preferably contains the cobalt in the form of cobalt sulfate or the nickel preferably in the form of nickel sulfate.
  • the aqueous solution contains 10 to 25 g / l gold, optimal results being achieved at approximately 15 g / l gold.
  • the aqueous solution contains 150 to 250 g / l malic acid.
  • An optimal quality of the precipitates is achieved when the aqueous solution contains approximately 200 g / l malic acid.
  • the aqueous solution contains potassium hydroxide for adjusting a pH between 4.2 and 4.7, preferably for adjusting a pH of approximately 4.5.
  • the invention also specifies a preferred method for the galvanic hard gold plating of electrical contact components using an additive-free bath according to the invention. It is provided that the hard gold plating is carried out in a jet plating system at a current density between 2 and 20 A / dm 2 and at a spraying speed of the aqueous solution between 1 and 10 m / s. A particularly good quality of the deposited precipitates is achieved if the hard gold plating is carried out at a current density between 2 and 13 A / dm 2 .
  • the invention further specifies a preferred method for the galvanic hard gold plating of electrical contact components using a bath according to the invention containing cobalt or nickel as a hardness additive. It is provided that the hard gold plating is carried out in a jet plating system at a current density between 2 and 45 A / dm 2 and at a spraying speed of the aqueous solution between 1 and 10 m / s. A particularly good quality of the deposited layers is achieved when the hard gold plating with a current density between 2 and. 35 A / dm 2 is carried out.
  • the hard gold plating is carried out at a spraying speed of the aqueous solution of approximately 2 m / s. In both cases it is also particularly favorable if the hard gold plating is carried out at a bath temperature between 40 and 65 ° C., preferably between 50 and 60 ° C., a bath temperature of approximately 55 ° C. being regarded as optimal.
  • the bath temperature was set to 55 ° C when the jet plating system was in operation.
  • the aqueous bath solution with Spr i was tz Oberen of about 2 m / s on the areas to be plated of the plug contacts directed and plating at current densities 2-13 ALDM 2 pre- taken, the cathodic current yield was 90 to 95%.
  • Matte_hard gold layers with a layer thickness of approx. 2.5 ⁇ m were deposited, which had very good wear resistance, excellent ductility and a low contact resistance. After storing the plug contacts at an elevated temperature, there was no noticeable increase in the contact resistance.
  • the hardness HV (50) was always in the range between 170 and 180 kp / mm 2 .
  • the bath temperature was set to 55 ° C and the spraying speed to approx. 2 m / s.
  • cathodic current yields between 40 and 70% shining hard gold layers with a layer thickness of approx. 2.5 ⁇ m were deposited, which had very good wear resistance, good ductility and a low contact resistance.
  • the measured hardness HV (50) was always in the range between 120 and 180 kp / mm 2 .
  • the baths described in Examples 1, 2 and 3 contained no further constituents or additives apart from the constituents indicated.
  • similarly good results can be achieved if the cobalt or nickel used as the hardness additive is added in the form of other water-soluble salts, for example in the form of cobalt chloride or nickel chloride.

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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)

Claims (23)

1. Bain acide au cyanure, pour le dépôt par électrolyse d'or dur sur des éléments électriques de contact, qui contient en solution aqueuse du cyanure de potassium et d'or, de l'acide malique et l'hydroxyde de potassium, caractérisé en ce que la solution aqueuse est préparée à partir
a) de 5 à 45 g de cyanure de potassium et d'or par litre ;
b) de 50 à 300 g d'acide malique par litre ;
c) d'hydroxyde de potassium pour régler le pH entre 3,8 et 5,0 ;
d) de 0 à 300 mg de cobalt ou de nickel par titre sous forme d'un sel soluble dans l'eau ; et
e) d'eau.
2. Bain suivant la revendication 1, caractérisé en ce que la solution aqueuse est exempte de durcisseur comme le sont le cobalt ou le nickel.
3. Bain suivant la revendication 1, caractérisé en ce que la solution aqueuse contient comme durcisseur de 30 à 250 mg de cobalt par litre.
4. Bain suivant la revendication 3, caractérisé en ce que la solution aqueuse contient de 40 à 100 mg de cobalt par litre.
5. Bain suivant la revendication 4, caractérisé en ce que la solution aqueuse contient environ 50 mg de cobalt par litre.
6. Bain suivant la revendication 1, 3, 4 ou 5, caractérisé en ce que la solution aqueuse contient du cobalt sous la forme de sulfate de cobalt.
7. Bain. suivant la revendication 1, caractérisé en ce que la solution aqueuse contient comme durcisseur de 50 à 300 mg de nickel par litre.
8. Bain suivant la revendication 7, caractérisé en ce que la solution aqueuse contient comme durcisseur environ 100 mg de nickel par litre.
9. Bain suivant la revendication 1, 7 ou 8, caractérisé en ce que la solution aqueuse contient du nickel sous forme de sulfate de nickel.
10. Bain suivant l'une des revendications précédentes, caractérisé en ce que la solution aqueuse contient de 10 à 25 g d'or par litre.
11. Bain suivant la revendication 10, caractérisé en ce que la solution aqueuse contient environ 15 g d'or par litre.
12. Bain suivant l'une des revendications précédentes, caractérisé en ce que la solution aqueuse contient de 150 à 250 g d'acide malique par litre.
13. Bain suivant la revendication 12, caractérisé en ce que la solution aqueuse contient environ 200 g d'acide malique par litre.
14. Bain suivant l'une des revendications précédentes, caractérisé en ce que la solution aqueuse contient de l'hydroxyde de potassium pour régler le pH entre 4,2 et 4,7.
15. Bain suivant la revendication 14, caractérisé en ce que la solution aqueuse contient de l'hydroxyde de potassium pour régler le pH à 4,5 environ.
16. Procédé de dépôt électrolytique d'or dur sur des éléments électriques de contact, en utilisant un bain suivant la revendication 2 ou suivant la revendication 2 et l'une des revendications 10 à 15, caractérisé en ce que on effectue le dépôt d'or dur dans une installation Jet-Plating, sous une densité de courant comprise entre 2 et 20 A/dm2 et avec une vitesse de projection de la solution aqueuse comprise entre 1 et 10 m/s.
17. Procédé suivant la revendication 16, caractérisé en ce qu'on effectue le dépôt électrolytique d'or dur sous une densité de courant comprise entre 2 et 13 Aldm2.
18. Procédé de dépôt électrolytique d'or dur sur des éléments électriques de contact en utilisant un bain suivant l'une des revendications 3 à 9 ou suivant l'une des revendications 10 à 15, caractérisé en ce que, on effectue le dépôt d'or dur dans une installation Jet-Plating, sous une densité de courant comprise entre 2 et 45 A/dm2 avec une vitesse de projection de la solution aqueuse comprise entre 1 et 10 m/s.
19. Procédé suivant la revendication 18, caractérisé en ce que l'on effectue le dépôt d'or dur sous une densité de courant comprise entre 2 et 35 A/dm2.
20. Procédé suivant l'une des revendications 16 à 19, caractérisé en ce qu'on effectue le dépôt d'or dur à une vitesse de projection de la solution aqueuse de 2 m/s environ.
21. Procédé suivant l'une des revendications 16 à 20, caractérisé en ce qu'on effectue le dépôt d'or dur à une température du bain comprise entre 40 et 65 °C.
22. Procédé suivant la revendication 21, caractérisé en ce qu'on effectue le dépôt d'or dur à une température du bain comprise entre 50 et 60 °C.
23. Procédé suivant la revendication 22, caractérisé en ce qu'on effectue le dépôt d'or dur à une température du bain de 55 °C environ.
EP85108129A 1984-07-05 1985-07-01 Bain et procédé d'électroplacage d'or dur Expired EP0168705B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT85108129T ATE38061T1 (de) 1984-07-05 1985-07-01 Bad und verfahren zur galvanischen hartvergoldung.

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE3424757 1984-07-05
DE3424757 1984-07-05
DE3509245 1985-03-14
DE19853509245 DE3509245A1 (de) 1985-03-14 1985-03-14 Bad und verfahren zur galvanischen hartvergoldung

Publications (2)

Publication Number Publication Date
EP0168705A1 EP0168705A1 (fr) 1986-01-22
EP0168705B1 true EP0168705B1 (fr) 1988-10-19

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ID=25822654

Family Applications (1)

Application Number Title Priority Date Filing Date
EP85108129A Expired EP0168705B1 (fr) 1984-07-05 1985-07-01 Bain et procédé d'électroplacage d'or dur

Country Status (2)

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EP (1) EP0168705B1 (fr)
DE (1) DE3565697D1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN120666187B (zh) * 2025-08-21 2025-11-25 长春黄金研究院有限公司 低氰化物浸金药剂体系及其堆浸工艺

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH494284A (fr) * 1968-11-28 1970-07-31 Sel Rex Corp Procédé pour le dépôt électrolytique d'un alliage d'or avec au moins un autre métal commun et bain aqueux de placage pour la mise en oeuvre de ce procédé
PL86754B1 (fr) * 1974-12-11 1977-12-15
US4075065A (en) * 1975-07-07 1978-02-21 Handy & Harman Gold plating bath and process
DE3121509C2 (de) * 1981-05-29 1983-04-14 Siemens AG, 1000 Berlin und 8000 München Bad zur galvanischen Hartvergoldung

Also Published As

Publication number Publication date
DE3565697D1 (en) 1988-11-24
EP0168705A1 (fr) 1986-01-22

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