EP3332044B1 - Palladiumhaltige zinn-/kupferlegierungen, verfahren zu deren herstellung und verwendung davon - Google Patents

Palladiumhaltige zinn-/kupferlegierungen, verfahren zu deren herstellung und verwendung davon Download PDF

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Publication number
EP3332044B1
EP3332044B1 EP16767356.5A EP16767356A EP3332044B1 EP 3332044 B1 EP3332044 B1 EP 3332044B1 EP 16767356 A EP16767356 A EP 16767356A EP 3332044 B1 EP3332044 B1 EP 3332044B1
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EP
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Prior art keywords
cyanide
alloy
palladium
grain
potassium
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English (en)
French (fr)
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EP3332044A2 (de
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Lorenzo Cavaciocchi
Leandro Luconi
Gabriele Gori
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Bluclad SpA
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Bluclad SpA
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C9/00—Alloys based on copper
    • C22C9/02—Alloys based on copper with tin as the next major constituent
    • 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
    • C25D7/00—Electroplating characterised by the article coated
    • C25D7/005—Jewels; Clockworks; Coins

Definitions

  • the present invention relates to the field of alloys, in particular bronzes containing palladium in small amounts, and to the galvanic baths used for their electrodeposition in galvanic processes.
  • Tin and copper alloys containing palladium are already known due to their resistance as possible low cost substitutes of pure palladium deposits and as substitutes of nickel for objects which must comply with non-allergenic characteristics.
  • Patent JP 06293990 describes an alloy of 10-20% tin, 10-80% copper and 10-50% palladium plus other elements in small amounts, which has color and strength comparable to pure palladium.
  • Patent JP 0978286 describes a galvanic bath for the deposition of copper, tin, zinc and palladium alloys with high concentrations of palladium in non-cyanide environment.
  • Patent JP 10204677 describes generic tin-palladium alloys where tin is present at a variable concentration in the alloy from 21 to 35%, while palladium is present at a variable concentration in the alloy from 35 to 60%.
  • the above alloys require relatively high concentrations of palladium and thus, the plating bath has a considerable initial cost, moreover while there is a net saving of palladium during plating, since a palladium alloy replaces a pure palladium deposit, there is still a fairly high palladium consumption.
  • Tin/copper alloys containing palladium, optionally zinc and optionally brighteners or grain finishers in traces, meaning in an amount of less than 0,25%, are described, where the palladium content is from 0.25 to 10% by weight calculated on the total weight of the alloy.
  • the present invention allows to overcome the above drawbacks by means of shiny and bright bronze alloys consisting of copper, tin, palladium, optionally zinc, and optionally brighteners or grain finishers in traces, meaning in an amount of less than 0,25%, which exhibit high oxidation resistance and a greater hardness (therefore, greater wear resistance) and where the palladium is present in small amounts.
  • the low presence of palladium allows to reduce production costs considerably compared to the use of pure palladium and alloys thereof, such as those mentioned above.
  • the alloys according to the present invention have the following composition (the percentages are expressed by weight with respect to the total weight of the alloy): Sn 25-45% Zn 0-15% Pd 0.25-10% Cu as needed to 100%
  • the alloys according to the invention may optionally contain brighteners or grain finishers elements in traces, where traces mean amounts of less than 0.25% by weight of the alloy and brighteners or grain finishers are those normally used for this purpose in this field of activity.
  • the alloys according to the invention have the following composition: Sn 34-40% Zn 5-10% Pd 0.7- 3% Cu as needed to 100%
  • alloy having the following composition: Cu 52% Sn 38% Zn 8% Pd 2%
  • the present invention also relates to galvanic baths used for making the alloys according to the invention, where "galvanic baths” means the aqueous solutions used in electrogalvanic processes for the electrodeposition of alloys.
  • the galvanic baths as defined above are therefore aqueous solutions consisting of Cu, Sn, Zn, Pd and cyanide and optionally comprising also one or more complexing agents which, in addition to modulating the performance of alloy metals, ensure stability in solution thereof, one or more surfactants, one or more brighteners and grain finishers in traces, as normally used in the solutions of this type.
  • the cyanide content in the solutions is equal to 1 - 100 g/L.
  • the metals listed above are present in solution as soluble oxides, sulfates, cyanides, ammonia salts and other suitable soluble compounds and the cyanide is in the form of sodium or potassium cyanide, or is derived from metal salts constituting the alloy in the form of cyanide complexes, such as for example copper cyanide and zinc cyanide.
  • the copper content in solution is normally from 2 to 30 g/L, more suitably from 5 to 15 g/L, with a ratio of copper to cyanide in the electrolyte preferably from 1:1 to 1:10, calculated based on the potassium or sodium cyanide.
  • the tin concentration in the electrolyte can range between 2 and 30 g/L with an amount of free hydroxide in the range from 0 to 20 g/L calculated on the basis of potassium or sodium hydroxide.
  • the Zn content in the solution may be from 0.1 to 5 g/L, based on the relative concentration of the other metals to obtain the alloy of the invention.
  • the content of the fourth component of the alloy, Palladium may range between 0.001 g/L and 5 g/L, preferably to obtain the desired alloy it may range between 0.005 and 0.5 g/L.
  • the solution may further contain one or more complexing agents capable of regulating the deposition of the metal components and ensuring stability in solution, as is known for compositions of this type.
  • complexing agents are for example complexing agents suitable for the purpose, they may be nitrilotriacetic acid (NTA), ethylenediaminetetraacetic acid (EDTA), of diethylenetriaminepentaacetic acid (DTPA), phosphonate salts of alkali metals such as ethylenediamine tetra(methylene phosphonic acid) (EDTMPA), 1-hydroxyethane 1,1-diphosphonic acid (HEDP), derivatives or salts of polyhydroxylated organic substances such as gluconates and more or less complex sugars.
  • NTA nitrilotriacetic acid
  • EDTA ethylenediaminetetraacetic acid
  • DTPA diethylenetriaminepentaacetic acid
  • phosphonate salts of alkali metals such as ethylenediamine tetra(methylene phosphonic acid) (EDTMPA), 1-hydroxyethane 1,1-diphosphonic acid (HEDP), derivatives or salts of polyhydroxylated organic substances such as
  • surfactants and mixtures of surfactants well known to those skilled in the art may also be present in the solutions, such as wetting agents of the family of alkyl ether phosphonates, alkyl ether sulfonates, alkyl aryl polyethoxylates and sulfonated derivatives thereof, quaternary ammonium salts of alkanes or aromatic compounds.
  • the brighteners and grain finishers commonly used for this purpose may also be included in the solutions, including metals such as bismuth, tellurium, gallium, indium, silver, molybdenum, thallium, antimony in traces.
  • the thickness of white bronze deposited is equal to 2 microns.
  • the deposit has a concentration by weight of palladium in the alloy of 1.2%.
  • the deposited alloy has the following composition: Cu 52.4% Sn 38.1% Zn 8.3% Pd 1.2%
  • the thickness of white bronze deposited is equal to 3 microns.
  • the deposit has a concentration by weight of palladium in the alloy of 5.5%.
  • the deposited alloy has the following composition: Cu 54.4% Sn 36.3% Zn 3.8% Pd 5.5%
  • the bronze alloys as described above can be used as a intermediate protective deposit having high resistance between the base material and the deposits of precious material forming the finish, or if with a higher percentage of palladium, they may be used as a finish itself.
  • the alloy is ideal for plating clothing accessories, costume jewelry, footwear and leather goods (e.g. buckles, self-locking devices, chains, bracelets, sliders, zippers, hooks, shoe clamps, etc.) for high fashion.
  • leather goods e.g. buckles, self-locking devices, chains, bracelets, sliders, zippers, hooks, shoe clamps, etc.

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

Claims (9)

  1. Bronzelegierung mit der folgenden Zusammensetzung, wobei die Prozentsätze nach Masse, bezogen auf die Gesamtmasse der Legierung, ausgedrückt sind: Sn 25 - 45 % Zn 0 - 15 % Pd 0,25 - 10 %
    gegebenenfalls Aufheller oder Feinstrukturschleifmittel in Spuren, d.h. in einer Menge von weniger als 0,25 %, Cu nach Bedarf bis 100 %
  2. Legierung nach Anspruch 1, umfassend: Sn 34 - 40 % Zn 5 - 10 % Pd 0,7 - 3 %
  3. Legierung nach Anspruch 2 mit der folgenden Zusammensetzung: Cu 52 % Sn 38 % Zn 8 % Pd 2 %
  4. Legierung nach den Ansprüchen 1 - 3, die auch Glanzmittel oder Feinstrukturschleifmittel in Spuren enthält.
  5. Verfahren zur Herstellung der Legierungen nach den Ansprüchen 1 - 4 durch galvanische elektrolytische Abscheidung, wobei galvanische Bäder verwendet werden, die aus wässrigen Lösungen bestehen, die Cyanid, Cu, Sn, Pd und gegebenenfalls Zn enthalten und gegebenenfalls auch ein oder mehrere Komplexbildner, ein oder mehrere Tenside, einen oder mehrere Glanzmittel und Abscheide-Feinstrukturschleifmittel-Elemente in Spuren enthalten.
  6. Verfahren nach Anspruch 5, wobei die vorgenannten Metalle in Lösung als lösliche Oxide, Sulfate, Cyanide, Ammoniaksalze vorhanden sind und Cyanid in Form von Natrium- oder Kaliumcyanid vorliegt oder aus den Salzen der die Legierung bildenden Metalle in Form von Cyanidkomplexen abgeleitet ist.
  7. Verfahren nach den Ansprüchen 5 und 6, wobei die Lösungen Folgendes enthalten: Cyanid 1 - 100 g/l. Kupfer 2 - 30 g/l mit einem Kupfer/Cyanid-Verhältnis zwischen 1:1 und 1:10, berechnet auf Basis des Kaliums oder Natriumcyanids. Zinn 2 - 30 g/l mit einer Menge an freiem Hydroxid im Bereich zwischen 0 bis 20 g/l, berechnet auf Basis von Kalium oder Natriumhydroxid. Zink 0 - 5 g/l, bezogen auf die relative Konzentration der anderen Metalle. Palladium 0,001 g/l - 5 g/l, vorzugsweise zwischen 0,005 und 0,5 g/l.
  8. Verfahren nach den Ansprüchen 5 und 6, wobei die Lösungen auch ein(en) oder mehrere Komplexbildner, Netzmittel und Feinstrukturschleifmittel enthalten.
  9. Verwendung der Legierungen nach den Ansprüchen 1 - 4 zum Beschichten von Bekleidungszubehör, Modeschmuck, Schuhwerk oder Lederwaren, z.B. Schnallen, selbstsichernden Vorrichtungen, Ketten, Armbändern, Gleitern, Reißverschlüssen, Haken, Schuhklemmen für Top-Mode.
EP16767356.5A 2015-08-05 2016-08-04 Palladiumhaltige zinn-/kupferlegierungen, verfahren zu deren herstellung und verwendung davon Active EP3332044B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ITUB2015A002876A ITUB20152876A1 (it) 2015-08-05 2015-08-05 Leghe stagno/rame contenenti palladio, metodo per la loro preparazione e loro uso.
PCT/IB2016/054703 WO2017021916A2 (en) 2015-08-05 2016-08-04 Tin/copper alloys containing palladium, method for their preparation and use thereof

Publications (2)

Publication Number Publication Date
EP3332044A2 EP3332044A2 (de) 2018-06-13
EP3332044B1 true EP3332044B1 (de) 2020-01-01

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ID=54364603

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EP16767356.5A Active EP3332044B1 (de) 2015-08-05 2016-08-04 Palladiumhaltige zinn-/kupferlegierungen, verfahren zu deren herstellung und verwendung davon

Country Status (5)

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EP (1) EP3332044B1 (de)
CN (1) CN108138263A (de)
HK (1) HK1253577A1 (de)
IT (1) ITUB20152876A1 (de)
WO (1) WO2017021916A2 (de)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ITUB20152876A1 (it) 2015-08-05 2017-02-05 Bluclad S R L Leghe stagno/rame contenenti palladio, metodo per la loro preparazione e loro uso.
EP3150744B1 (de) * 2015-09-30 2020-02-12 COVENTYA S.p.A. Galvanikbad zur elektrochemischen abscheidung einer cu-sn-zn-pd legierungsschicht, verfahren zur elektrochemischen abscheidung der legierungsschicht, substrat mit der legierungsschicht und verwendungen des beschichteten substrats
IT201700014377A1 (it) * 2017-02-09 2018-08-09 Bluclad S R L Bronzo giallo/rosa inox e suo impiego in prodotti galvanizzati
IT201800004235A1 (it) * 2018-04-05 2019-10-05 Lega di bronzo bianco, bagno galvanico e procedimento al fine di produrre la lega di bronzo bianco tramite deposizione elettrogalvanica
IT202000011203A1 (it) * 2020-05-15 2021-11-15 Bluclad S P A Lega di bronzo inossidabile e suo impiego in prodotti galvanizzati

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06293990A (ja) 1993-04-07 1994-10-21 Nippon Shinkinzoku Kako Kk Ｓｎ−Ｃｕ−Ｐｄ合金めっき部材、その製造に用いるめっき浴
US5972526A (en) 1995-12-07 1999-10-26 Citizen Watch Co., Ltd. Decorative member
US20140055026A1 (en) 2011-03-09 2014-02-27 Umicore Ag & Co. Kg Amalgam balls having an alloy coating
EP2799595A1 (de) 2013-05-03 2014-11-05 Delphi Technologies, Inc. Elektrisches Kontaktelement
WO2015039152A1 (de) 2013-09-18 2015-03-26 Ing.W.Garhöfer Gesellschaft M.B.H. Abscheidung von cu, sn, zn-beschichtungen auf metallischen substraten
WO2017021916A2 (en) 2015-08-05 2017-02-09 Bluclad S.R.L. Tin/copper alloys containing palladium, method for their preparation and use thereof

Family Cites Families (2)

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CN1097644C (zh) * 1995-12-07 2003-01-01 西铁城钟表有限公司 装饰件
EP1930478B1 (de) * 2006-12-06 2013-06-19 Enthone, Inc. Zusammensetzung eines Elektrolyten und Verfahren zur Beschichtung von quaternären Kupferlegierungen

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06293990A (ja) 1993-04-07 1994-10-21 Nippon Shinkinzoku Kako Kk Ｓｎ−Ｃｕ−Ｐｄ合金めっき部材、その製造に用いるめっき浴
US5972526A (en) 1995-12-07 1999-10-26 Citizen Watch Co., Ltd. Decorative member
US20140055026A1 (en) 2011-03-09 2014-02-27 Umicore Ag & Co. Kg Amalgam balls having an alloy coating
EP2799595A1 (de) 2013-05-03 2014-11-05 Delphi Technologies, Inc. Elektrisches Kontaktelement
WO2015039152A1 (de) 2013-09-18 2015-03-26 Ing.W.Garhöfer Gesellschaft M.B.H. Abscheidung von cu, sn, zn-beschichtungen auf metallischen substraten
WO2017021916A2 (en) 2015-08-05 2017-02-09 Bluclad S.R.L. Tin/copper alloys containing palladium, method for their preparation and use thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
RICHARD E DEPOTO AND AL GRUENWALD C., UYEMURA & CO. LTD., & JOERG WEBER AND KLAUS LEYENDECKER, UMICORE GALVANOTECHNIK GMBH: "White Bronze, Copper-Tin-Zinc Tri-metal: Expand- ing Applications and New Developments in a Changing Landscape", ELECTROPLATING, 20 May 2013 (2013-05-20), pages 1 - 16, XP055739739, Retrieved from the Internet <URL:www.pfonline.com/articles/white-bronze-copper-tin-zi nc-tri-metal- ex panding-applications-and-new-developments-in-a-changing-landscape>

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WO2017021916A2 (en) 2017-02-09
EP3332044A2 (de) 2018-06-13
HK1253577A1 (zh) 2019-06-21
WO2017021916A3 (en) 2017-03-16
CN108138263A (zh) 2018-06-08
ITUB20152876A1 (it) 2017-02-05

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