EP0126921B1 - Bath for the galvanic deposition of gold alloys - Google Patents
Bath for the galvanic deposition of gold alloys Download PDFInfo
- Publication number
- EP0126921B1 EP0126921B1 EP84103995A EP84103995A EP0126921B1 EP 0126921 B1 EP0126921 B1 EP 0126921B1 EP 84103995 A EP84103995 A EP 84103995A EP 84103995 A EP84103995 A EP 84103995A EP 0126921 B1 EP0126921 B1 EP 0126921B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- acid
- bismuth
- aqueous bath
- alkali
- liter
- 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
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 an aqueous bath for the galvanic deposition of uniform rose to violet-colored gold-copper bismuth alloys, exclusively containing an alkali metal or ammonium cyanoaurate-I, alkali copper cyanide, alkali metal cyanide, a bismuth compound and optionally organic wetting and glossing agents.
- Bismuth-containing baths are already known, from which two- or three-substance alloys can be galvanically deposited.
- Bismuth trifluoride or bismuth triperchlorate or alkali bismuth mutates are generally used as bismuth compounds, of which the former can only be used in the acidic range and the latter only in the strongly alkaline range, since these compounds are sparingly soluble in the pH range from 6 to 13.
- Baths of this composition are of no technical importance, since they are unstable and deposit coatings with only a low gloss.
- FR 2 353 656 also describes additional mixtures for baths for the electrolytic deposition of gold or gold alloys, which are intended to modify the galvanic properties of the baths and thereby improve the electrolytically deposited deposits of gold or gold alloys.
- Organic water-soluble nitro compounds and water-soluble compounds of arsenic, antimony, bismuth, thallium and selenium are proposed as such additives.
- the object of the present invention is to provide a stable bismuth-containing gold alloy bath, which enables the deposition of shiny ternary gold alloys with a high bismuth content.
- the bismuth compound being a water-soluble complex compound of bismuth with ethylenediaminetetramethylphosphonic acid, 2,3-dihydroxypropylphosphonic acid, 1-hydroxyrelihiphiphonic acid, nitrilotriacetic acid, 4-oxyphenylmalonic acid, 1,2-diaminocyclohexanoic acid, dantaminocyclohexane Contains sugar acid, d-manno sugar acid, mucic acid, 1,2,3,4-tetrahydroxy-butane-1,1,4-tricarboxylic acid, 3,4,5-trihydroxybenzoic acid or ethylenediaminetetra-isopropyl alcohol.
- the bathroom according to the invention is outstandingly suitable for the deposition of shiny rose-colored to violet-colored ternary gold alloys on decorative objects, such as jewelry, watches and glasses, which is not possible with the known bathrooms of similar composition.
- the bismuth can be incorporated in the alloys with extraordinarily high contents of up to 30 percent by weight, which opens up further areas of application.
- the bathroom according to the invention is surprisingly also suitable for finishing electronic components, such as plug-in connections, since the precipitates deposited thereby are particularly hard and have good electrical conductivity and excellent abrasion resistance.
- the soluble complex compounds of bismuth can be prepared before their use according to the invention, for example by reacting the complexing agents with bismuth hydroxide or bismuth nitrate in aqueous solution in a molar ratio of 1 mol bismuth to 1 to 4 mol complexing agent at room temperature.
- bismuth hydroxide or bismuth nitrate and complexing agent directly to the bath solution.
- An aqueous solution is used as the bath, which contains exclusively alkali metal or ammonium dicyanoaurate-I, alkali copper cyanide, alkali metal cyanide, the water-soluble complex compound of bismuth and, if appropriate, organic wetting and brightening agents.
- the preferred concentrations are:
- Sodium and potassium salts are advantageously used as the alkali salt.
- the bath can contain customary non-ionic, cationic or anionic wetting agents. These substances can also act as brighteners, in concentrations of 0.01 to 20 g / liter.
- the pH can be from 6 to 13 and, if desired, is adjusted by adding alkali metal hydroxide.
- the bath is expediently operated at temperatures of 20 to 70 ° C., current densities of 0.1 to 3 A / dm 2 preferably being used.
- the pH of 11.5 is adjusted with potassium hydroxide.
- a rose-colored coating with a fineness of 750/000 is deposited at an average current density of 0.4 A / dm 2 .
- the coatings have a hardness of HK 420.
- Precipitation with a purity of 850/000 is separated from this electrolyte.
- the coatings have an unexpectedly high resistance to corrosion and behave excellently in the wear test.
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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)
- Cosmetics (AREA)
Description
Die Erfindung betrifft ein wässriges Bad für die galvanische Abscheidung von gleichmässigen rose- bis violett-farbenen Gold-Kupfer-Wismut-Legierungen, ausschliesslich enthaltend ein Alkali- oder Ammoniumcyanoaurat-I, Alkalikupfercyanid, Alkalicyanid, eine Wismutverbindung sowie gegebenfalls organische Netz- und Glanzmittel.The invention relates to an aqueous bath for the galvanic deposition of uniform rose to violet-colored gold-copper bismuth alloys, exclusively containing an alkali metal or ammonium cyanoaurate-I, alkali copper cyanide, alkali metal cyanide, a bismuth compound and optionally organic wetting and glossing agents.
Es sind bereits wismuthaltige Bäder bekannt, aus denen galvanisch Zwei- oder Dreistofflegierungen abgeschieden werden können. Als Wismutverbindungen werden in der Regel Wismuttrifluorid oder Wismuttriperchlorat beziehungsweise Alkaliwismutate verwendet, von denen erstere nur im sauren Bereich und letztere nur im stark alkalischen Bereich eingesetzt werden können, da diese Verbindungen im pH-Bereich von 6 bis 13 schwerlöslich sind.Bismuth-containing baths are already known, from which two- or three-substance alloys can be galvanically deposited. Bismuth trifluoride or bismuth triperchlorate or alkali bismuth mutates are generally used as bismuth compounds, of which the former can only be used in the acidic range and the latter only in the strongly alkaline range, since these compounds are sparingly soluble in the pH range from 6 to 13.
Bäder dieser Zusammensetztung sind ohne technsiche Bedeutung, da sie instabil sind und Überzüge mit nur geringem Glanz abscheiden.Baths of this composition are of no technical importance, since they are unstable and deposit coatings with only a low gloss.
In der FR 2 353 656 werden weiterhin Zusatzgemische für Bäder zur elektrolytischen Abscheidung von Gold oder Goldlegierungen beschrieben, welche die Modifizierung der galvanischen Eigenschaften der Bäder und dadurch die Verbesserung von elektrolytisch abgeschiedenen Niederschlägen von Gold oder Goldlegierungen bewirken sollen. Als derartige Zusatzstoffe werden vorgeschlagen organische wasserlösliche Nitroverbindungen und wasserlösliche Verbindungen des Arsens, Antimons, Wismuts, Thalliums und Selens.FR 2 353 656 also describes additional mixtures for baths for the electrolytic deposition of gold or gold alloys, which are intended to modify the galvanic properties of the baths and thereby improve the electrolytically deposited deposits of gold or gold alloys. Organic water-soluble nitro compounds and water-soluble compounds of arsenic, antimony, bismuth, thallium and selenium are proposed as such additives.
Diese Gemische sollen hauptsächlich in reinen Vergoldungsbädern die Verteilungseigenschaften wesentlich verbessern.These mixtures are said to improve the distribution properties substantially, especially in gold-plating baths.
Aufgabe der vorliegenden Erfindung ist die Zurverfügungstellung eines stabilen wismuthaltigen Goldlegierungsbades, welches die Abscheidung glänzender ternärer Goldlegierungen mit einem hohen Wismutgehalt ermöglicht.The object of the present invention is to provide a stable bismuth-containing gold alloy bath, which enables the deposition of shiny ternary gold alloys with a high bismuth content.
Diese Aufgabe wird erfindungsgemäss gelöst durch ein wässriges Bad der eingangs bezeichneten Art, wobei es als Wismutverbindung eine wasserlösliche Komplexverbindung des Wismuts mit Äthylendiamintetramethylphosphonsäure, 2,3-Dihydroxipropylphosphonsäure, 1-Hydroxyäthandiphosphonsäure, Nitrilotriessigsäure, 4-Oxyphenylmalonsäure, 1,2-Diaminocyclohexantetraessigsäure, d-Zuckersäure, d-Mannozuckersäure, Schleimsäure, 1,2,3,4-Tetrahydroxi-butan-1,1,4-tricarbonsäure, 3,4,5-Trihydroxibenzoesäure oder Äthylendiamintetra-isopropylalkohol enthält.This object is achieved according to the invention by an aqueous bath of the type mentioned at the beginning, the bismuth compound being a water-soluble complex compound of bismuth with ethylenediaminetetramethylphosphonic acid, 2,3-dihydroxypropylphosphonic acid, 1-hydroxyäthiphiphonic acid, nitrilotriacetic acid, 4-oxyphenylmalonic acid, 1,2-diaminocyclohexanoic acid, dantaminocyclohexane Contains sugar acid, d-manno sugar acid, mucic acid, 1,2,3,4-tetrahydroxy-butane-1,1,4-tricarboxylic acid, 3,4,5-trihydroxybenzoic acid or ethylenediaminetetra-isopropyl alcohol.
Das erfindungsgemässe Bad eignet sich in hervorragender Weise zur Abscheidung von glänzenden rose- bis violett-farbenen ternären Goldlegierungen auf dekorativen Gegenständen, wie beispielsweise Schmuck, Uhren und Brillen, was mit den bekannten Bädern ähnlicher Zusammensetzung nicht möglich ist.The bathroom according to the invention is outstandingly suitable for the deposition of shiny rose-colored to violet-colored ternary gold alloys on decorative objects, such as jewelry, watches and glasses, which is not possible with the known bathrooms of similar composition.
Von besonderer technischer Bedeutung ist es, dass das Wismut in die Legierungen mit ausserordentlich hohen Gehalten bis zu 30 Gewichtsprozent und höher eingebaut werden kann, womit sich weitere Anwendungsbereiche erschliessen.It is of particular technical importance that the bismuth can be incorporated in the alloys with extraordinarily high contents of up to 30 percent by weight, which opens up further areas of application.
So eignet sich das erfindungsgemässe Bad überraschenderweise auch zur Veredelung von elektronischen Bauteilen, wie Steckverbindungen, da die hiermit abgeschiedenen Niederschläge besonders hart sind und eine gute elektrische Leitfähigkeit sowie eine hervorragende Abriebbeständigkeit aufweisen.The bathroom according to the invention is surprisingly also suitable for finishing electronic components, such as plug-in connections, since the precipitates deposited thereby are particularly hard and have good electrical conductivity and excellent abrasion resistance.
Die löslichen Komplexverbindungen des Wismuts können vor ihrer erfindungsgemässen Verwendung hergestellt werden, indem zum Beispiel die Komplexierungsmittel mit Wismuthydroxid oder Wismutnitrat in wässriger Lösung in einem Molverhältnis von 1 Mol Wismut auf 1 bis 4 Mol Komplexierungsmittel bei Zimmertemperatur umgesetzt werden. Es ist jedoch auch möglich, Wismuthydroxid oder Wismutnitrat und Komplexierungsmittel der Badlösung direkt zuzusetzen.The soluble complex compounds of bismuth can be prepared before their use according to the invention, for example by reacting the complexing agents with bismuth hydroxide or bismuth nitrate in aqueous solution in a molar ratio of 1 mol bismuth to 1 to 4 mol complexing agent at room temperature. However, it is also possible to add bismuth hydroxide or bismuth nitrate and complexing agent directly to the bath solution.
Als Bad wird eine wässrige Lösung verwendet, welche ausschliesslich Alkali- oder Ammoniumdicyanoaurat-I, Alkalikupfercyanid, Alkalicyanid, die wasserlösliche Komplexverbindung des Wismuts sowie gegebenenfalls organische Netz- und Glanzmittel enthält.An aqueous solution is used as the bath, which contains exclusively alkali metal or ammonium dicyanoaurate-I, alkali copper cyanide, alkali metal cyanide, the water-soluble complex compound of bismuth and, if appropriate, organic wetting and brightening agents.
Die bevorzugten Konzentrationen betragen:The preferred concentrations are:
Als Zusatzstoffe kann das Bad übliche Netzmittel in nichtionoger, kation- oder anionaktiver Natur enthalten. Diese Stoffe können auch als Glanzbildner wirken, und zwar in Konzentrationen von 0,01 bis 20 g/Liter.As additives, the bath can contain customary non-ionic, cationic or anionic wetting agents. These substances can also act as brighteners, in concentrations of 0.01 to 20 g / liter.
Der pH-Wert kann je nach eingesetztem Komplexbildner von 6 bis 13 betragen und wird gewünschtenfalls durch Zusatz von Alkalihydroxid eingestellt.Depending on the complexing agent used, the pH can be from 6 to 13 and, if desired, is adjusted by adding alkali metal hydroxide.
Das Bad wird zweckmässigerweise bei Temperaturen von 20 bis 70°C betrieben, wobei bevorzugt Stromdichten von 0,1 bis 3 A/dm2 zur Anwendung kommen.The bath is expediently operated at temperatures of 20 to 70 ° C., current densities of 0.1 to 3 A / dm 2 preferably being used.
Die folgenden Beispiele dienen zur Erläuterung der Erfindung.The following examples serve to illustrate the invention.
Bei einer mittleren Stromdichte von 0,4 A/dm2 wird ein rose-farbener Überzug mit einem Feingehalt von 750/000 abgeschieden. Die Überzüge weisen eine Härte von HK 420 auf.A rose-colored coating with a fineness of 750/000 is deposited at an average current density of 0.4 A / dm 2 . The coatings have a hardness of HK 420.
Aus diesem Elektrolyten werden Niederschläge abgeschieden mit einem Feingehalt von 850/000. Die Überzüge haben eine unerwartet hohe Korrosionsbeständigkeit und verhalten sich im Verschleisstest hervorragend.Precipitation with a purity of 850/000 is separated from this electrolyte. The coatings have an unexpectedly high resistance to corrosion and behave excellently in the wear test.
Claims (4)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19833319772 DE3319772A1 (en) | 1983-05-27 | 1983-05-27 | BATH FOR GALVANIC DEPOSITION OF GOLD ALLOYS |
| DE3319772 | 1983-05-27 |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| EP0126921A2 EP0126921A2 (en) | 1984-12-05 |
| EP0126921A3 EP0126921A3 (en) | 1985-01-30 |
| EP0126921B1 true EP0126921B1 (en) | 1989-01-18 |
Family
ID=6200354
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP84103995A Expired EP0126921B1 (en) | 1983-05-27 | 1984-04-10 | Bath for the galvanic deposition of gold alloys |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US4517060A (en) |
| EP (1) | EP0126921B1 (en) |
| JP (1) | JPS59232289A (en) |
| AT (1) | AT383148B (en) |
| DE (2) | DE3319772A1 (en) |
| ES (1) | ES532837A0 (en) |
| HK (1) | HK74389A (en) |
| IE (1) | IE56353B1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10110743A1 (en) * | 2001-02-28 | 2002-09-05 | Wieland Dental & Technik Gmbh | Bath for the electrodeposition of gold and gold alloys and its use |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB8903818D0 (en) * | 1989-02-20 | 1989-04-05 | Engelhard Corp | Electrolytic deposition of gold-containing alloys |
| DE3905705A1 (en) * | 1989-02-24 | 1990-08-30 | Degussa | BATHROOM FOR GALVANIC DEPOSITION OF FINE GOLD COATINGS |
| GB2309032A (en) * | 1996-01-11 | 1997-07-16 | Procter & Gamble | Bismuth salts and complexes with nitrogen-free organic diphosphonic acids |
| 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 |
| US20240271306A1 (en) | 2021-09-16 | 2024-08-15 | P & S, Galvasols | High-speed pure gold electroforming/electroplating bath |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CH494284A (en) * | 1968-11-28 | 1970-07-31 | Sel Rex Corp | Process for the electrolytic deposition of a gold alloy with at least one other common metal and aqueous plating bath for carrying out this process |
| FR2053770A5 (en) * | 1969-07-17 | 1971-04-16 | Radiotechnique Compelec | Electrolytic deposition of gold-bismuth - alloys |
| CH615464A5 (en) * | 1976-06-01 | 1980-01-31 | Systemes Traitements Surfaces | Special compositions and particular additives for gold electrolysis baths and their use |
| US4199416A (en) * | 1977-05-03 | 1980-04-22 | Johnson, Matthey & Co., Limited | Composition for the electroplating of gold |
| JPS5951058B2 (en) * | 1977-07-20 | 1984-12-12 | 松下電器産業株式会社 | magnetic recording and reproducing device |
| FR2405312A1 (en) * | 1977-10-10 | 1979-05-04 | Oxy Metal Industries Corp | Bath for electrodeposition of gold-zinc alloys - contains alkali sulphite, gold-sulphite complex, zinc salt, complex or chelate, complexing or chelating agent and metal |
| JPS609117B2 (en) * | 1980-06-19 | 1985-03-07 | セイコーエプソン株式会社 | gold alloy plating bath |
-
1983
- 1983-05-27 DE DE19833319772 patent/DE3319772A1/en active Granted
-
1984
- 1984-04-10 DE DE8484103995T patent/DE3476225D1/en not_active Expired
- 1984-04-10 EP EP84103995A patent/EP0126921B1/en not_active Expired
- 1984-05-22 IE IE1268/84A patent/IE56353B1/en not_active IP Right Cessation
- 1984-05-22 AT AT0168784A patent/AT383148B/en not_active IP Right Cessation
- 1984-05-25 ES ES532837A patent/ES532837A0/en active Granted
- 1984-05-25 JP JP59104892A patent/JPS59232289A/en active Granted
- 1984-05-29 US US06/615,471 patent/US4517060A/en not_active Expired - Lifetime
-
1989
- 1989-09-14 HK HK743/89A patent/HK74389A/en not_active IP Right Cessation
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10110743A1 (en) * | 2001-02-28 | 2002-09-05 | Wieland Dental & Technik Gmbh | Bath for the electrodeposition of gold and gold alloys and its use |
Also Published As
| Publication number | Publication date |
|---|---|
| AT383148B (en) | 1987-05-25 |
| HK74389A (en) | 1989-09-22 |
| EP0126921A2 (en) | 1984-12-05 |
| JPS59232289A (en) | 1984-12-27 |
| DE3319772C2 (en) | 1991-05-16 |
| IE56353B1 (en) | 1991-07-03 |
| ES8502741A1 (en) | 1985-02-01 |
| DE3319772A1 (en) | 1984-11-29 |
| US4517060A (en) | 1985-05-14 |
| IE841268L (en) | 1984-11-27 |
| ES532837A0 (en) | 1985-02-01 |
| ATA168784A (en) | 1986-10-15 |
| DE3476225D1 (en) | 1989-02-23 |
| EP0126921A3 (en) | 1985-01-30 |
| JPH0565598B2 (en) | 1993-09-20 |
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