EP1983077B1 - Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre - Google Patents

Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre Download PDF

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Publication number
EP1983077B1
EP1983077B1 EP07007963.7A EP07007963A EP1983077B1 EP 1983077 B1 EP1983077 B1 EP 1983077B1 EP 07007963 A EP07007963 A EP 07007963A EP 1983077 B1 EP1983077 B1 EP 1983077B1
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EP
European Patent Office
Prior art keywords
acid
electrolyte
gold
nitrilo
copper
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.)
Not-in-force
Application number
EP07007963.7A
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German (de)
English (en)
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EP1983077A1 (fr
Inventor
Guy Desthomas
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.)
MacDermid Enthone Inc
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Enthone Inc
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Application filed by Enthone Inc filed Critical Enthone Inc
Priority to EP16197251.8A priority Critical patent/EP3170924A1/fr
Priority to EP07007963.7A priority patent/EP1983077B1/fr
Priority to CN2008100934716A priority patent/CN101289756B/zh
Publication of EP1983077A1 publication Critical patent/EP1983077A1/fr
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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
    • C25D3/58—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of copper
    • 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

  • This invention relates to an electrolyte as well as a method for the electrolytic deposition of a gold-copper alloy on a substrate surface.
  • alloy layers which can be varied in respect of their physical properties like brightness, hardness, wear resistance or colour. These properties are influenced by the composites of the alloys, e. g. the metals co-plated, as well as by the composition of the bath used for the deposition of the alloy, e. g. the electrolyte. Further, also the method and the plating parameters like temperature and current density are influencing the plating result in important ways.
  • U.S. patent 5,006,208 discloses a galvanic gold alloying bath which contains beneath gold and copper in form of cyanide compounds a selenium compound.
  • the deposit achieved from this galvanic bath is soft, light yellow and matt.
  • the gold-alloy containing is constituted by 14 - 18 carat.
  • European patent EP 0 384 679 B1 discloses a bath for the electrolytic deposition of gold-copper alloy as well as a method for electroplating articles using such a bath.
  • An electrolyte is disclosed which contains gold in form of a cyanide compound, copper in the form of a cyanide compound as well as tellurium or bismuth in the form of watersoluble compounds.
  • European patent application EP 0 566 054 A1 discloses a solution for electroplating gold-copper alloys.
  • an electrolyte comprising a soluble gold compound present as a gold cyanide complex, a soluble copper compound present as a copper cyanide complex as well as a soluble divalent sulfur compound in an amount sufficient to brighten the alloys.
  • the brightening additive may be a thiocyanate, thiomalic acid, imidazolidinethione, a sulfite or thiobarbituric acid.
  • Further patent documents disclosing the deposition of gold-copper alloys are for instance EP 0 193 848 A1 , GB 1 375 611 A and GB 2 053 276 A .
  • an electrolyte for the electrolytic deposition of a gold-copper alloy on a substrate surface wherein the electrolyte comprises beneath a source of gold and copper potassium cyanide (KCN) in a concentration capable to maintain a copper to KCN ratio in the range of 3 to 7, and at least one complexing agent of the group consisting of ethylenediamine tetraacetic acid [EDTA], diethylenetriamine pentaacetic acid and nitrilo-triacetic acid [NTA] hydroxyethyl imino diacetic acid [HEIDA], nitrilo propionic diacetic acid [NPDA], imino diacetic acid [IDA], nitrilo trimethylphosphoric acid [NTMA, Dequest 2000], triethanol amine [FEA].
  • EDTA ethylenediamine tetraacetic acid
  • NDA nitrilo-triacetic acid
  • HEIDA hydroxyethyl imino diacetic acid
  • NPDA nitri
  • the electrolyte according to the invention can comprise gold in a concentration between 2 to 20 g/l and copper in a concentration between 10 to 50 g/l.
  • the at least one complexing agent of the group mentioned above is comprised in the inventive electrolyte in a concentration between 0,05 to 0,6 mol/l. It is believed that the strong chelating agents beneath functioning as complexing agent will contribute to the conductivity of the electrolyte.
  • the inventive electrolyte may further comprise one of at least one metal of the group consisting of Sb, Se, Ag,Pt, Ni and Zn.
  • Zinc and nickel can function as grain refiner as well as stabilizerto the free KCN.
  • Gold is believed to function as efficiency booster to yield in higher plating velocity and carat.
  • the metals mentioned above can be comprised in the inventive electrolyte in an amount between 0,1 mg/l and 10 g/l. It is within the scope of the invention that the electrolyte can comprise further additive metals to influence the physical properties of the deposit.
  • the inventive electrolyte can further comprise a surface active agent or wetting agent which will function as brightener.
  • a capable surface active agent which can be comprised in the electrolyte is for example sodium-lauryl-etherphosphate.
  • commercially available products known by name of nonionic, cationic, or amphoteric surfactants can be employed single or in combinations.
  • the amount of the surface active agent in the inventive electrolyte may vary in a range of 0,1 ti 5 ml/l.
  • the electrolyte can comprise secondary brightener and/or stabilizing agents.
  • secondary brightener and/or stabilizing agents are pyridin sulfonic acid and ammonium hydrogene difluoride.
  • the amount of these secondary brightener and/or stabilizing agents may vary in a range between 0,1 g/l to 10 g/l.
  • the pH-value of the inventive electrolyte may vary in a range of pH 8 to pH 13, with a preferred pH-value of about 11.
  • the inventive electrolyte may comprise alkaline hydroxide or alkaline earth hydroxide.
  • the current density conducted between the substrate and the anode may vary in a range of 0,2 to 2 A/dm 2 .
  • the temperature of the electrolyte is in the range of 70° C to 90° C.
  • the inventive electrolyte together with the inventive method permits to produce a large range of carat suitable for plating and electroforming producing accurate value of carat between 18 and 14.
  • the value of carat can be controlled by measurement of efficiency in Mg/A.nm. According to the relationship of temperature and current density disclosed above, the right efficiency for an adequate value of carat is obtained by tuning the current density and temperature respectively.
  • a further advantage of the deposit yield by the inventive electrolyte and the inventive method is the possibility to heat-treat the deposited alloys in order to get an optimum ductility for a gold alloy. This is advantageously for both decorative and functional applications.
  • heat-treating the alloys deposited a relatively high hardness is achieved. Relatively high in these terms means higher than that of the metallurgical alloy.
  • the hardness rises from 280 HV to 380 HV while the aspect of surface isn't changed by oxidation.
  • a further advantage of the deposits obtained from the inventive electrolyte is the good solder ability of the alloys. This characteristic is especially important in electroforming when it is necessary to close holes done to empty the mandrels and for further artistic work.
  • the electrolyte Due to the strong complexing power of the complexing agent used according to this invention, the electrolyte is relatively none-sensitive to possible contaminations from various metals like Sn, Zn, Ag, Ni or Cr coming from different sources like drag ins from pre-treatment, mandrels composition or replenishment products. Generally, such types of contamination create an instability of the relation between current density and efficiency which may cause problems during electroforming processes. So, the non-sensity of the electrolyte to this contaminations is a further advance of this invention.
  • gold-copper alloy deposits on substrate surfaces are obtainable showing a thickness of > 20 microns and a carat in the range of 12 to 19 carat.
  • gold-copper alloy deposits on substrate surfaces are obtainable showing a thickness of > 20 microns and a carat in the range of 12 to 19 carat.
  • electroforming at a thickness of 200 microns and more is possible.
  • inventive electrolyte is also of high economic interest since it shows a minimum turn-over of 0,25 kg/l.

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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 (14)

  1. Electrolyte pour le dépôt électrolytique d'un alliage or-cuivre sur une surface de substrat, où l'électrolyte comprend sous une source d'or et de cuivre cyanure de potassium (KCN) libre à une concentration en g/l capable de maintenir un rapport cuivre sur KCN libre dans la gamme de 3 à 7, et au moins un agent complexant du groupe constitué de l'acide éthylène diamine tétra acétique, de l'acide diéthylène triamine penta acétique, de l'acide nitrilo triacétique, de l'acide éthylène diamine tétra acétique [EDTA], de l'acide diéthylène triamine penta acétique et de l'acide nitrilo triacétique [NTA], de l'acide hydroxy éthyl imino diacétique [HEIDA], de l'acide nitrilo propionique diacétique [NPDA], de l'acide imino diacétique [IDA], de l'acide nitrilo triméthylphosphorique [NTMA, Dequest 2000], de la triéthanol amine [TEA], où l'électrolyte est capable de déposer des couches d'alliage d'or épais et brillant sans addition de cadmium.
  2. Electrolyte selon la revendication 1, comprenant de l'or à une concentration entre 2 et 20 g/l et du cuivre à une concentration entre 10 et 50 g/l.
  3. Electrolyte selon l'une des revendications 1 ou 2, dans lequel l'au moins un agent complexant du groupe constitué de l'acide éthylène diamine tétra acétique, de l'acide diéthylène triamine penta acétique, de l'acide nitrilo triacétique, de l'acide éthylène diamine tétra acétique [EDTA], de l'acide diéthylène triamine penta acétique et de l'acide nitrilo triacétique [NTA], de l'acide hydroxy éthyl imino diacétique [HEIDA], de l'acide nitrilo propionique diacétique [NPDA], de l'acide imino diacétique [IDA], de l'acide nitrilo triméthylphosphorique [NTMA, Dequest 2000], de la triéthanol amine [TEA] est compris à une concentration entre 0,05 et 0,6 mol/l.
  4. Electrolyte selon l'une des revendications 1 à 3, comprenant en outre des ions d'au moins un métal du groupe constitué de Te, Sb, Se, Ag, Pt, Ni et Zn.
  5. Electrolyte selon la revendication 4, comprenant des ions d'au moins un métal du groupe constitué de Sb, Se, Ag, Pt, Ni et Zn en une quantité entre 0,1 mg/l et 10 g/l.
  6. Electrolyte selon l'une des revendications 1 à 5, comprenant en outre un agent tensioactif.
  7. Electrolyte selon la revendication 6, dans lequel l'agent tensioactif est un laurylétherphosphate de sodium.
  8. Electrolyte selon la revendication 7, comprenant l'agent tensioactif en une quantité de 0,1 à 5 ml/l.
  9. Electrolyte selon l'une des revendications 1 à 8, comprenant en outre des agents secondaires de brillance et/ou de stabilisation.
  10. Electrolyte selon l'une des revendications 1 à 4, dans lequel la valeur du pH de l'électrolyte est dans la gamme de 8 à 13.
  11. Procédé de dépôt d'une couche d'alliage or-cuivre sur une surface de substrat, où le procédé comprend les étapes :
    de prétraitement de la surface du substrat devant être plaqué ;
    de mise en contact de la surface du substrat devant être plaqué avec un électrolyte selon l'une des revendications 1 à 10 ; et
    d'application d'un courant entre le substrat et une anode.
  12. Procédé selon la revendication 11, dans lequel la densité de courant appliquée entre le substrat et l'anode est dans la gamme de 0,2 à 2 A/dm2.
  13. Procédé selon la revendication 11, ou 12, dans lequel la température de l"électrolyte est dans la gamme de 70 °C à 90 °C.
  14. Dépôt d'alliage or-cuivre sur une surface de substrat par un procédé selon l'une des revendications 11 à 13, où l'épaisseur du dépôt est > 20 microns et le carat est dans la gamme de 12 à 19 ct.
EP07007963.7A 2007-04-19 2007-04-19 Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre Not-in-force EP1983077B1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP16197251.8A EP3170924A1 (fr) 2007-04-19 2007-04-19 Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre
EP07007963.7A EP1983077B1 (fr) 2007-04-19 2007-04-19 Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre
CN2008100934716A CN101289756B (zh) 2007-04-19 2008-04-21 用于金铜合金电解沉积的电解组合物及方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP07007963.7A EP1983077B1 (fr) 2007-04-19 2007-04-19 Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre

Related Child Applications (3)

Application Number Title Priority Date Filing Date
EP16197251.8A Division-Into EP3170924A1 (fr) 2007-04-19 2007-04-19 Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre
EP16197251.8A Division EP3170924A1 (fr) 2007-04-19 2007-04-19 Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre
EP16197251.8A Previously-Filed-Application EP3170924A1 (fr) 2007-04-19 2007-04-19 Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre

Publications (2)

Publication Number Publication Date
EP1983077A1 EP1983077A1 (fr) 2008-10-22
EP1983077B1 true EP1983077B1 (fr) 2016-12-28

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EP16197251.8A Withdrawn EP3170924A1 (fr) 2007-04-19 2007-04-19 Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre
EP07007963.7A Not-in-force EP1983077B1 (fr) 2007-04-19 2007-04-19 Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre

Family Applications Before (1)

Application Number Title Priority Date Filing Date
EP16197251.8A Withdrawn EP3170924A1 (fr) 2007-04-19 2007-04-19 Électrolyte et procédé pour le dépôt électrolytique d'alliages or-cuivre

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EP (2) EP3170924A1 (fr)
CN (1) CN101289756B (fr)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN105506686A (zh) * 2015-12-23 2016-04-20 苏州市金星工艺镀饰有限公司 一种装饰性镍铜金三元合金电镀液的电镀方法
CN108139306B (zh) * 2016-02-18 2021-03-26 日本制铁株式会社 金属化合物粒子的提取方法、分析方法及其使用的电解液
CN105671602A (zh) * 2016-03-15 2016-06-15 大连理工大学 一种无氰亚硫酸盐的Au-Cu合金电镀液及应用
CN109680310B (zh) * 2019-01-04 2020-07-07 中国计量大学 一种镍锑电镀液及其制备方法
CN110699721B (zh) * 2019-11-20 2021-08-20 长春黄金研究院有限公司 一种无氰镀金铜合金电镀液及其应用
CN111962104A (zh) * 2020-08-21 2020-11-20 深圳国韵黄金文化有限公司 一种22k无氰电铸黄金及其制备工艺
CN114875456B (zh) * 2021-06-25 2024-03-08 深圳市铭轩珠宝首饰有限公司 一种铜-金复合包金方法及其应用

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1375611A (fr) 1972-03-28 1974-11-27
EP0304315A1 (fr) 1987-08-21 1989-02-22 Engelhard Limited Bain de déposition électrolytique d'un alliage or-cuivre-zinc
EP0384679A1 (fr) 1989-02-20 1990-08-29 Engelhard Corporation Dépôt électrolytique d'alliages d'or
EP0416342A1 (fr) 1989-09-06 1991-03-13 Degussa Aktiengesellschaft Bain d'alliage d'or galvanique
EP0566054A1 (fr) 1992-04-15 1993-10-20 LeaRonal, Inc. Electrodéposition d'alliages or-cuivre-argent
EP1103637A1 (fr) 1999-11-29 2001-05-30 ENTHONE-OMI, Inc. Procédé de fabrication d'une couche en alliage AuCuGa en utilisant l'électrolyse et les alliages obtenus par ce procédé
EP1728898A2 (fr) 2005-06-02 2006-12-06 Rohm and Haas Electronic Materials LLC Electrolyte pour le dêpot des alliages à base d'or

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH632533A5 (fr) * 1979-06-14 1982-10-15 Aliprandini P Procede pour le depot galvanoplastique d'un alliage d'or.
CH662583A5 (fr) * 1985-03-01 1987-10-15 Heinz Emmenegger Bain galvanique pour le depot electrolytique d'alliages d'or-cuivre-cadmium-zinc.

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1375611A (fr) 1972-03-28 1974-11-27
EP0304315A1 (fr) 1987-08-21 1989-02-22 Engelhard Limited Bain de déposition électrolytique d'un alliage or-cuivre-zinc
EP0384679A1 (fr) 1989-02-20 1990-08-29 Engelhard Corporation Dépôt électrolytique d'alliages d'or
EP0416342A1 (fr) 1989-09-06 1991-03-13 Degussa Aktiengesellschaft Bain d'alliage d'or galvanique
EP0566054A1 (fr) 1992-04-15 1993-10-20 LeaRonal, Inc. Electrodéposition d'alliages or-cuivre-argent
EP1103637A1 (fr) 1999-11-29 2001-05-30 ENTHONE-OMI, Inc. Procédé de fabrication d'une couche en alliage AuCuGa en utilisant l'électrolyse et les alliages obtenus par ce procédé
EP1728898A2 (fr) 2005-06-02 2006-12-06 Rohm and Haas Electronic Materials LLC Electrolyte pour le dêpot des alliages à base d'or

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
C. POHLANDT: "A critical evaluation of methods applicable for the determination of cyanides", JOURNAL OF THE SOUTH AFRICAN INSTITUTE OF MINING AND METALLURGY, January 1983 (1983-01-01), pages 11 - 19, XP055425861
H. P. ROTHBAUM: "The Composition of Copper Complexes in Cuprocyanide Solutions", JOURNAL OF THE ELECTROCHEMICAL SOCIETY, vol. 104, no. 11, November 1957 (1957-11-01), pages 682 - 686, XP055425845
I.-M. MIHAESCU: "Cyanide Determination with a modified Ninhydrin Reagent using N- Acetyl Cysteine in the presence of Heavy Metal Ions", J. CHIL. CHEM. SOC., vol. 55, no. 4, 2010, pages 467 - 468, XP055425848
T. MICHALOWSKI: "Liebig-Deniges Method of Cyanide Determination: A comparative Study of Two Approaches", J. SOLUTION CHEM, vol. 41, 2012, pages 1224 - 1239, XP035094245

Also Published As

Publication number Publication date
EP1983077A1 (fr) 2008-10-22
EP3170924A1 (fr) 2017-05-24
CN101289756B (zh) 2012-06-20
CN101289756A (zh) 2008-10-22

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