EP0416342B1 - Bain d'alliage d'or galvanique - Google Patents
Bain d'alliage d'or galvanique Download PDFInfo
- Publication number
- EP0416342B1 EP0416342B1 EP90115670A EP90115670A EP0416342B1 EP 0416342 B1 EP0416342 B1 EP 0416342B1 EP 90115670 A EP90115670 A EP 90115670A EP 90115670 A EP90115670 A EP 90115670A EP 0416342 B1 EP0416342 B1 EP 0416342B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- cyanide
- potassium
- gold
- copper
- silver
- 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 - Lifetime
Links
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
Definitions
- the invention relates to a galvanic gold alloy bath containing 1 to 15 g / l gold as potassium gold (I) cyanide, 5 to 50 g / l copper as potassium copper (I) cyanide, 0.05 to 5 g / l silver as potassium silver ( I) cyanide, free alkali cyanide, dipotassium hydrogen phosphate, as well as a selenium compound and a pH of 8.5 to 11.
- the galvanic deposition of gold alloys has become particularly important for decorative and technical purposes.
- the soft, cell yellow, matt pure gold layers can be characterized by the deposition of other metals in their properties, e.g. change in gloss, hardness, wear resistance or color in many ways.
- a substantial proportion of the deposited gold alloy coatings have 14 - 18 carat, yellow or rose-colored coatings, which, in addition to copper as an alloy metal to lighten the resulting red color, contain a white-coloring metal such as cadmium, silver or zinc.
- Such coatings are used, for example, in the jewelry and glasses industry, where double layers have been largely replaced by galvanic coatings. Such coatings are also used in electrical engineering when low contact resistance is not required, such as with slip ring and rotary contacts.
- the galvanic deposition of gold / copper / silver alloy coatings causes considerable difficulties due to the potential position of the metals in the electrolyte and has so far only been solved unsatisfactorily.
- the basis for the joint deposition are aqueous solutions of the cyano complexes of the three metals. In the alkaline range, in which these baths are only stable, the potential of silver is much nobler than that of gold and copper, so that silver is preferentially deposited and therefore only coatings, depending on the silver content, are obtained with a whitish-yellow or greenish-yellow color .
- DE-PS 801 312 therefore attempts to shift the potential of the silver to less noble values by using the lowest possible pH.
- DD-PS 59022 also works in neutral and attempts to achieve glossy layers by applying current changes with a low concentration of free alkali metal cyanide, which in practice often leads to coatings with a non-uniform color.
- the gloss formation of the coatings can also be achieved with chemical compounds.
- DE-PS 750 185 the deposition of silver or copper coatings from an alkaline cyanide bath has a shine or tellurium effect.
- JP-A-59 76891 (Chem. Abstr. Vol. 101, No. 12, page 587, 100245f) describes a galvanic gold-silver-copper bath which contains gold, silver and copper as alkali metal cyanides, free cyanide in quantities 10 g / l and hydrogen carbonate, but contains no selenium compounds. Shiny layers can only be obtained if two gold alloy layers of different compositions are deposited one above the other with different current densities and then thermal diffusion of the two layers into one another is carried out at 600 ° C.
- FR-A-22 02 954 discloses a galvanic gold-copper-cadmium bath which calculates the alloy metals as alkali metal cyanides, free alkali metal cyanide and a selenium compound in amounts of 0.1 mg / l up to 5 g / l as selenium Contains brightener. References to galvanic gold-silver-copper baths are not contained in this document.
- the US-A-4,121,982 describes a galvanic gold-silver bath, which acts as a brightener, a combination of 0.1 to 0.5 mg / l selenium compound and 4 to 75 mg / l of a polyethyleneimine per gram of silver or gold content of the bath contains. Again, there is no evidence of galvanic gold-silver-copper baths.
- It was therefore an object of the present invention to develop a galvanic gold alloy bath which contains 1 to 15 g / l gold as potassium gold (I) cyanide, 5 to 50 g / l copper as potassium copper (I) cyanide, 0.05 to 5 g / l of silver as potassium silver (I) cyanide, free alkali metal cyanide dipotassium hydrogen phosphate, and also contains a selenium compound and has a pH value of 8.5 to 11, which is stable and shiny without expensive aids, and depending on the copper content and current density, yellow to supplies rose gold-copper-silver alloy plating.
- This object is achieved in that the content of free alkali cyanide is at most 10 g / l and that it contains 0.1 to 1 mg / l selenium as potassium selenocyanate.
- the bath preferably additionally contains 0.1 to 5 ml / l of a surfactant from the group of nonionic wetting agents of the ethylene oxide adduct type and their phosphate esters.
- a surfactant from the group of nonionic wetting agents of the ethylene oxide adduct type and their phosphate esters.
- alkyl polyglycol ether butyl or nonylphenol polyglycol ether and their phosphate esters can be used.
- the galvanic gold alloy baths according to the invention are preferably composed as follows: 1 - 15 g / l gold as KAu (CN) 2 5 - 50 g / l copper as K2Cu (CN) 3 0.05 - 5 g / l silver as KAg (CN) 2 0.1-10 g / l free alkali cyanide 1 - 10 g / l di-potassium hydrogen phosphate 0.1 - 5 m / l surfactant 0.1 - 1 mg / l selenium as KSeCN
- a phosphate ester such as, for example, nonylphenol polyglycol ether phosphate ester, is suitable as the surfactant which supports the formation of gloss.
- the bath has a pH between 8.5 and 11 and is preferably operated at a bath temperature of 60 - 75 ° C and current densities of 0.2 - 2.5 A / dm2.
- the following bath composition is preferably used for the 14-18 carat yellow or rose-colored gold alloy coatings that are deposited most frequently in practice: 3 - 5 g / l gold as KAu (CN) 2 20 - 25 g / l copper as K2Cu (CN) 3 0.2 - 0.5 g / l silver as KAg (CN) 2 2-4 g / l free alkali cyanide 2-4 g / l di-potassium hydrogen phosphate 0.1-1 ml / l surfactant 0.1 - 0.5 mg / l selenium as KSeCN.
- the bath is preferably operated at a pH of 9-10 and a bath temperature of 60-70 ° C.
- Shiny coatings are obtained in the current density range between 0.3 and 1.5 A / dm2, the carat content of the layers decreasing with increasing current density.
- the deposited layers are very ductile and even low-carat coatings have good corrosion resistance in the copper chloride test.
- the pH is adjusted to 9 with potassium hydroxide.
- the bath is now heated to 65 ° C and a prepared, shiny nickel-plated copper sheet with a surface area of 0.25 dm2 is gold-plated with 2.5 amine at a current density of 0.5 A / dm2.
- the result is a shiny coating with a weak rose color, which has a carat content of 17.2.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Engineering & Computer Science (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Cosmetics (AREA)
- Dental Preparations (AREA)
- Laminated Bodies (AREA)
- Materials For Medical Uses (AREA)
- Manufacture And Refinement Of Metals (AREA)
Claims (2)
- Bain d'alliage d'or galvanique qui contient 1 à 15 g/l d'or sous forme de cyanure d'or (I) et de potassium, 5 à 50 g/l de cuivre sous forme de cyanure de cuivre (I) et de potassium, 0,05 à 5 g/l d'argent sous forme de cyanure d'argent (I) et de potassium, du cyanure alcalin libre, de l'hydrogénophosphate dipotassique, ainsi qu'un composé de sélénium et qui présente un pH compris entre 8,5 et 11, caractérisé en ce que la teneur en cyanure alcalin libre dans le bain est au plus de 10 g/l et qu'il contient entre 0,1 et 1 mg/l de sélénium sous forme de sélénocyanate de potassium.
- Bain d'alliage d'or galvanique selon la revendication 1, caractérisé en ce qu'il contient en plus 0,1 à 5 ml/l d'un tensioactif du groupe des mouillants non ioniques du type des produits d'addition d'oxyde d'éthylène et de leurs esters phosphates.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE3929569 | 1989-09-06 | ||
DE3929569A DE3929569C1 (fr) | 1989-09-06 | 1989-09-06 | |
SG79294A SG79294G (en) | 1989-09-06 | 1994-06-16 | Galvante gold alloy bath. |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0416342A1 EP0416342A1 (fr) | 1991-03-13 |
EP0416342B1 true EP0416342B1 (fr) | 1994-03-16 |
Family
ID=25884802
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP90115670A Expired - Lifetime EP0416342B1 (fr) | 1989-09-06 | 1990-08-16 | Bain d'alliage d'or galvanique |
Country Status (13)
Country | Link |
---|---|
US (1) | US5006208A (fr) |
EP (1) | EP0416342B1 (fr) |
JP (1) | JPH03100194A (fr) |
AT (1) | ATE103018T1 (fr) |
BR (1) | BR9004378A (fr) |
DD (1) | DD297668A5 (fr) |
DE (2) | DE3929569C1 (fr) |
DK (1) | DK0416342T3 (fr) |
ES (1) | ES2050317T3 (fr) |
FI (1) | FI93661C (fr) |
HK (1) | HK67794A (fr) |
NO (1) | NO903868L (fr) |
SG (1) | SG79294G (fr) |
Families Citing this family (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5256275A (en) * | 1992-04-15 | 1993-10-26 | Learonal, Inc. | Electroplated gold-copper-silver alloys |
DE4317210C2 (de) * | 1993-05-21 | 1998-10-15 | Norbert Muerrle | Halbzeug zur Herstellung von Schmuck und Verfahren zu dessen Bearbeitung |
DE10107675B4 (de) | 2001-02-19 | 2004-11-25 | Implantcast Gmbh | Endoprothese und Verfahren zu ihrer Herstellung |
DE10354760A1 (de) * | 2003-11-21 | 2005-06-23 | Enthone Inc., West Haven | Verfahren zur Abscheidung von Nickel und Chrom(VI)freien metallischen Mattschichten |
SG127854A1 (en) * | 2005-06-02 | 2006-12-29 | Rohm & Haas Elect Mat | Improved gold electrolytes |
US20090104463A1 (en) | 2006-06-02 | 2009-04-23 | Rohm And Haas Electronic Materials Llc | Gold alloy electrolytes |
JP4711227B2 (ja) * | 2005-11-09 | 2011-06-29 | 央 澤栗 | 浴用ガス溶解製造装置 |
CH714243B1 (fr) * | 2006-10-03 | 2019-04-15 | Swatch Group Res & Dev Ltd | Procédé d'électroformage et pièce ou couche obtenue par ce procédé. |
EP1983077B1 (fr) | 2007-04-19 | 2016-12-28 | Enthone, Inc. | Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre |
CH710184B1 (fr) | 2007-09-21 | 2016-03-31 | Aliprandini Laboratoires G | Procédé d'obtention d'un dépôt d'alliage d'or jaune par galvanoplastie sans utilisation de métaux ou métalloïdes toxiques. |
EP2312021B1 (fr) * | 2009-10-15 | 2020-03-18 | The Swatch Group Research and Development Ltd. | Procédé d'obtention d'un dépôt d'alliage d'or jaune par galvanoplastie sans utilisation de métaux toxiques |
EP2505691B1 (fr) | 2011-03-31 | 2014-03-12 | The Swatch Group Research and Development Ltd. | Procédé d'obtention d'un dépôt d'alliage d'or 18 carats 3N |
DE102013109400A1 (de) * | 2013-08-29 | 2015-03-05 | Harting Kgaa | Kontaktelement mit Goldbeschichtung |
CN112663095A (zh) * | 2020-11-10 | 2021-04-16 | 杭州科尔贵金属有限公司 | 一种改进型3d硬金电铸药水配方及制备工艺 |
Family Cites Families (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE750185C (de) * | 1939-07-08 | 1944-12-27 | Baeder zur elektrolytischen Abscheidung von glaenzenden Metallniederschlaegen | |
DE801312C (de) * | 1949-05-05 | 1950-11-23 | Pforzheimer Elektrizitäts - Gesellschaft m. b. H., Pforzheim | Verfahren zur elektrolvtischen Abscheidung von Gold und Goldlegierungen |
NL219700A (fr) * | 1956-09-08 | |||
CH418085A (fr) * | 1964-08-19 | 1966-07-31 | Pilot Pen Co Ltd | Electrolyte pour le dépôt galvanique d'alliages d'or |
US3532610A (en) * | 1967-10-27 | 1970-10-06 | Kewanee Oil Co | Selenium compounds as brighteners in copper plating baths |
CH522740A (de) * | 1968-06-28 | 1972-06-30 | Degussa | Verfahren zur galvanischen Abscheidung von Gold-Kupfer-Cadmium-Legierungsüberzügen |
DE2251285C3 (de) * | 1972-10-14 | 1981-01-22 | Schering Ag, 1000 Berlin Und 4619 Bergkamen | Alkalisches Bad für die galvanische Abscheidung von Goldlegierungen |
US4121982A (en) * | 1978-02-03 | 1978-10-24 | American Chemical & Refining Company Incorporated | Gold alloy plating bath and method |
JPS585273B2 (ja) * | 1979-07-24 | 1983-01-29 | 日本電鍍工業株式会社 | 硬質金合金被膜の製造方法 |
CH662583A5 (fr) * | 1985-03-01 | 1987-10-15 | Heinz Emmenegger | Bain galvanique pour le depot electrolytique d'alliages d'or-cuivre-cadmium-zinc. |
-
1989
- 1989-09-06 DE DE3929569A patent/DE3929569C1/de not_active Expired - Lifetime
-
1990
- 1990-08-16 ES ES90115670T patent/ES2050317T3/es not_active Expired - Lifetime
- 1990-08-16 EP EP90115670A patent/EP0416342B1/fr not_active Expired - Lifetime
- 1990-08-16 AT AT90115670T patent/ATE103018T1/de not_active IP Right Cessation
- 1990-08-16 DK DK90115670.3T patent/DK0416342T3/da active
- 1990-08-16 DE DE90115670T patent/DE59004996D1/de not_active Expired - Fee Related
- 1990-08-29 US US07/574,359 patent/US5006208A/en not_active Expired - Fee Related
- 1990-09-04 BR BR909004378A patent/BR9004378A/pt not_active Application Discontinuation
- 1990-09-05 FI FI904377A patent/FI93661C/fi not_active IP Right Cessation
- 1990-09-05 DD DD90343836A patent/DD297668A5/de not_active IP Right Cessation
- 1990-09-05 NO NO90903868A patent/NO903868L/no unknown
- 1990-09-06 JP JP2234655A patent/JPH03100194A/ja active Pending
-
1994
- 1994-06-16 SG SG79294A patent/SG79294G/en unknown
- 1994-07-14 HK HK67794A patent/HK67794A/xx unknown
Also Published As
Publication number | Publication date |
---|---|
DE3929569C1 (fr) | 1991-04-18 |
FI93661C (fi) | 1995-05-10 |
EP0416342A1 (fr) | 1991-03-13 |
ATE103018T1 (de) | 1994-04-15 |
HK67794A (en) | 1994-07-22 |
DK0416342T3 (da) | 1994-04-05 |
NO903868L (no) | 1991-03-07 |
BR9004378A (pt) | 1991-09-03 |
SG79294G (en) | 1994-10-14 |
DE59004996D1 (de) | 1994-04-21 |
FI93661B (fi) | 1995-01-31 |
US5006208A (en) | 1991-04-09 |
ES2050317T3 (es) | 1994-05-16 |
JPH03100194A (ja) | 1991-04-25 |
FI904377A0 (fi) | 1990-09-05 |
NO903868D0 (no) | 1990-09-05 |
DD297668A5 (de) | 1992-01-16 |
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