DE1446043C3 - Bath for galvanic deposition of gold alloys - Google Patents
Bath for galvanic deposition of gold alloysInfo
- Publication number
- DE1446043C3 DE1446043C3 DE19611446043 DE1446043A DE1446043C3 DE 1446043 C3 DE1446043 C3 DE 1446043C3 DE 19611446043 DE19611446043 DE 19611446043 DE 1446043 A DE1446043 A DE 1446043A DE 1446043 C3 DE1446043 C3 DE 1446043C3
- Authority
- DE
- Germany
- Prior art keywords
- nickel
- gold
- bath
- cobalt
- value
- 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
- 229910001020 Au alloy Inorganic materials 0.000 title claims description 4
- 239000003353 gold alloy Substances 0.000 title claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 28
- 229910052759 nickel Inorganic materials 0.000 claims description 16
- 239000010931 gold Substances 0.000 claims description 11
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 10
- 229910052737 gold Inorganic materials 0.000 claims description 10
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 8
- 229910052803 cobalt Inorganic materials 0.000 claims description 8
- 239000010941 cobalt Substances 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K Trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- 239000011778 trisodium citrate Substances 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 claims description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-K 2qpq Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 3
- FEWJPZIEWOKRBE-XIXRPRMCSA-N Mesotartaric acid Chemical compound OC(=O)[C@@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-XIXRPRMCSA-N 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K [O-]P([O-])([O-])=O Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- IZLAVFWQHMDDGK-UHFFFAOYSA-N gold(1+);cyanide Chemical compound [Au+].N#[C-] IZLAVFWQHMDDGK-UHFFFAOYSA-N 0.000 claims description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 3
- 229910052738 indium Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- JVTAAEKCZFNVCJ-UHFFFAOYSA-M lactate Chemical compound CC(O)C([O-])=O JVTAAEKCZFNVCJ-UHFFFAOYSA-M 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000011572 manganese Substances 0.000 claims description 3
- BDAGIHXWWSANSR-UHFFFAOYSA-M methanoate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- IIACRCGMVDHOTQ-UHFFFAOYSA-M sulfamate Chemical compound NS([O-])(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-M 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 229940095064 tartrate Drugs 0.000 claims description 3
- ODGCEQLVLXJUCC-UHFFFAOYSA-N tetrafluoroborate Chemical compound F[B-](F)(F)F ODGCEQLVLXJUCC-UHFFFAOYSA-N 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 150000002736 metal compounds Chemical class 0.000 claims description 2
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- WXLSIVAACGPAMC-UHFFFAOYSA-N CN(CCO)C.[Ni] Chemical compound CN(CCO)C.[Ni] WXLSIVAACGPAMC-UHFFFAOYSA-N 0.000 claims 2
- MGFYIUFZLHCRTH-UHFFFAOYSA-K nitrilotriacetate(3-) Chemical compound [O-]C(=O)CN(CC([O-])=O)CC([O-])=O MGFYIUFZLHCRTH-UHFFFAOYSA-K 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 239000003792 electrolyte Substances 0.000 description 8
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 description 3
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating Effects 0.000 description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N edta Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 description 2
- -1 alkali metal pyrophosphate Chemical class 0.000 description 2
- 229910002065 alloy metal Inorganic materials 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 1
- WOFVPNPAVMKHCX-UHFFFAOYSA-N N#C[Au](C#N)C#N Chemical compound N#C[Au](C#N)C#N WOFVPNPAVMKHCX-UHFFFAOYSA-N 0.000 description 1
- 229950004864 Olamine Drugs 0.000 description 1
- ARHBWGMHXPPGCZ-UHFFFAOYSA-N [K].[Au](C#N)(C#N)C#N Chemical compound [K].[Au](C#N)(C#N)C#N ARHBWGMHXPPGCZ-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- JHIDGGPPGFZMES-UHFFFAOYSA-N acetic acid;N-(2-aminoethyl)hydroxylamine Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.NCCNO JHIDGGPPGFZMES-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 231100000078 corrosive Toxicity 0.000 description 1
- 231100001010 corrosive Toxicity 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- HZAXFHJVJLSVMW-UHFFFAOYSA-N ethanolamine Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- SDKPSXWGRWWLKR-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-1-sulfonic acid Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)O SDKPSXWGRWWLKR-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- SOBHUZYZLFQYFK-UHFFFAOYSA-K trisodium;hydroxy-[[phosphonatomethyl(phosphonomethyl)amino]methyl]phosphinate Chemical compound [Na+].[Na+].[Na+].OP(O)(=O)CN(CP(O)([O-])=O)CP([O-])([O-])=O SOBHUZYZLFQYFK-UHFFFAOYSA-K 0.000 description 1
Description
Das Hauptpatent 1111 897 betrifft ein Bad zur galvanischen Abscheidung einer glänzenden Goldschicht, das 1 bis 15 g/l Gold als Alkali-gold-(I)-cyanid, 10 bis 150 g/l einer schwachen organischen Säure und 1 bis 50 g/l mindestens eines wasserlöslichen Sulfats, Sulfamats, Formiats, Acetats, Citrats, Lactats, Tartrats, Fluoroborats, Borats oder Phosphats des Nickels, Zinks, Kobalts, Indiums, Eisens, Mangans, Antimons oder Kupfers enthält und das einen pH-Wert von 3 bis 5 aufweist.The main patent 1111 897 relates to a bath for the galvanic deposition of a shiny gold layer, the 1 to 15 g / l of gold as alkali gold (I) cyanide, 10 to 150 g / l of a weak organic Acid and 1 to 50 g / l of at least one water-soluble sulfate, sulfamate, formate, acetate, citrate, Lactate, tartrate, fluoroborate, borate or phosphate of nickel, zinc, cobalt, indium, iron, Contains manganese, antimony or copper and has a pH of 3 to 5.
Aus der BE-PS 5 70 261 sind saure Goldbäder mit einem pH-Wert von 3 bis 5, enthaltend Alkaligoldcyanid sowie eine organische Säure und einfache Metallsalze bekannt.From BE-PS 5 70 261 are acidic gold baths with a pH of 3 to 5, containing alkali gold cyanide as well as an organic acid and simple metal salts are known.
Aus der CH-PS 2 77 997 sind Goldelektrolyten, enthaltend ein Goldsalz und Alkalipyrophosphat bekannt. Diese Elektrolyten arbeiten zwar im schwachsauren Bereich, enthalten jedoch Cyanide des Nickels, die sich bekanntlich bei einem pH-Wert von weniger als 5 zersetzen.Gold electrolytes containing a gold salt and alkali metal pyrophosphate are known from CH-PS 2 77 997. These electrolytes work in the weakly acidic range, but contain cyanides of nickel, which are known to decompose at a pH of less than 5.
Aus der DT-PS 10 33 987 sind alkalische Elektrolyten für Goldlegierungen bekannt, die Nickelchelate enthalten. Es besteht jedoch ein wesentlicher Unterschied, da es sich beim erfindungsgemäßen Gegenstand um saure Elektrolyten zum Unterschied zu den alkalischen Elektrolyten nach der DT-PS handelt.From DT-PS 10 33 987 alkaline electrolytes for gold alloys are known, the nickel chelates contain. There is, however, an essential difference, since it is the subject of the invention to acidic electrolytes in contrast to the alkaline electrolytes according to the DT-PS.
Es hat sich nun gezeigt, daß bei Verwendung von speziellen Chelatbildnern zur Komplexierung der Legierungsmetalle Nickel und Kobalt man gewisse Vorteile erreicht. So kann man duktile harte korrosions- und abriebbeständige Nickel bzw. Kobalt enthaltende Goldlegierungsschichten mit gleichmäßig heller Farbe und homogener Zusammensetzung nach dem Hauptpatent erhalten. Ein weiterer Vorteil ist, daß für diese Überzüge eine geringere Menge an Legierungsmetallverbindung angewandt zu werden braucht und trotzdem über lange Betriebszeiten ein arbeitsfähiger Elektrolyt für gleichmäßige Abscheidungen vorliegt.It has now been shown that when using special chelating agents to complex the Alloy metals nickel and cobalt one achieves certain advantages. This is how ductile, hard, corrosive and abrasion-resistant nickel and cobalt-containing gold alloy layers with uniformly light color and homogeneous composition obtained according to the main patent. Another advantage is that a smaller amount of alloy metal compound should be used for these coatings needs an electrolyte capable of working for even deposits over long operating times is present.
Nach der Erfindung werden nun in dem Bad nach dem Hauptpatent 1111 897, das 1 bis 15 g/l Gold als Alkaligold-(I)-cyanid, 10 bis 150 g/l einer schwachen organischen Säure und 1 bis 50 g/l mindestens eines wasserlöslichen Sulfats, Sulfamats, Formiats, Acetats, Citrats, Lactats, Tartrats, Fluoroborats, Borats oderAccording to the invention are now in the bath according to the main patent 1111 897, the 1 to 15 g / l gold as Alkali gold (I) cyanide, 10 to 150 g / l of a weak organic acid and 1 to 50 g / l of at least one water-soluble sulfate, sulfamate, formate, acetate, citrate, lactate, tartrate, fluoroborate, borate or
Ein Bad wurde durch Auflösen folgender Sub stanzen hergestellt:A bath was prepared by dissolving the following substances:
Gold als KAu(CN)2 8 g/lGold as KAu (CN) 2 8 g / l
Natriumeitrat 50 g/lSodium citrate 50 g / l
Zitronensäure 12 g/lCitric acid 12 g / l
Nickel als Ni-Dimethyläthan-Nickel as Ni-dimethylethane
olamin 450 mg/1olamine 450 mg / l
pH eingestellt auf 3,5pH adjusted to 3.5
Temperatur 35° CTemperature 35 ° C
Stromdichte 1,07 A/dm2 Current density 1.07 A / dm 2
Die aus diesem Bad erhaltenen Überzüge auf einei Metallscheibe von 9 · 2,54 cm waren glänzend und ziemlich gelb.The coatings obtained from this bath on a 9 x 2.54 cm metal disc were shiny and pretty yellow.
Beipiel 2Example 2
Gold als KAu(CN)2 8 g/lGold as KAu (CN) 2 8 g / l
Natriumeitrat 50 g/lSodium citrate 50 g / l
Zitronensäure 12 g/lCitric acid 12 g / l
Kobalt als Salz der Nitrilotriessigsäure 350 mg/1Cobalt as the salt of nitrilotriacetic acid 350 mg / 1
pH eingestellt auf 3,5pH adjusted to 3.5
Temperatur ' 22° CTemperature '22 ° C
Stromdichte 1,07 A/dm2 Current density 1.07 A / dm 2
Die aus diesem Bad nach 1 Stunde erhaltenen Überzüge auf einer Metallplatte von 9 · 2,54 cm waren stark glänzend.The coatings obtained from this bath after 1 hour on a 9 x 2.54 cm metal plate were very shiny.
VergleichsversucheComparative experiments
'Alle Versuche wurden durchgeführt mit einem Grundelektrolyt entsprechend dem Beispiel 1, nämlich 8 g/ Au (als Kaliumgoldcyanid), 50 g/l Natriumeitrat, 12 g/l Zitronensäure. Der Elektrolyt hatte einen pH-Wert von 3,5 und eine Temperatur von 35° C. Gearbeitet wurde mit einer Stromdichte von 1 A/dm2. Die Elektrolysezeit betrug einheitlich 10 min.All experiments were carried out with a base electrolyte according to Example 1, namely 8 g / Au (as potassium gold cyanide), 50 g / l sodium citrate, 12 g / l citric acid. The electrolyte had a pH of 3.5 and a temperature of 35 ° C. Work was carried out with a current density of 1 A / dm 2 . The electrolysis time was a uniform 10 minutes.
In folgender Tabelle sind die untersuchten Nickelchelate, die Abscheidegeschwindigkeit und das Aus-The following table shows the examined nickel chelates, the deposition rate and the
sehen der Plattierung zusammengefaßt. Die Bedeutung der erwähnten Chelate:see the plating summarized. The meaning of the mentioned chelates:
EDTA — Nickelkomplex von Dinatriumäthy-EDTA - nickel complex of disodium ethy-
lendiamintetraacetat DTPA — Nickelkomplex von Trinatriumdi-lendiamine tetraacetate DTPA - nickel complex of trisodium di-
äthylentriaminpentaacetat HEDTA — Nickelkomplex von Mononatrium-ethylene triamine pentaacetate HEDTA - nickel complex of monosodium
hydroxyäthylendiamintriacetat DMEA — Nickelkomplex von Dimethylätha-hydroxyethylenediamine triacetate DMEA - nickel complex of dimethylethyl
nolaminnolamine
EDTAEDTA
DTPADTPA
HEDTA DMEAHEDTA DMEA
mg/A-min 62,5 8,2
matt matt
streifigmg / A-min 62.5 8.2
matt matt
streaky
6,8 30,76.8 30.7
glänzend glänzendshiny shiny
Daraus ergibt sich folgendes:This results in the following:
1. Die Abscheidegeschwindigkeit ist mit EDTA am höchsten, jedoch sind die Überzüge unbrauchbar, weil sie matt und streifig sind.1. The separation speed is highest with EDTA, but the coatings are unusable, because they are dull and streaky.
2. Die Abscheidegeschwindigkeit mit HEDTA ist so gering, daß nur eine hauchdünne Schicht gebildet wurde, die im Bereich der hohen Stromdichten verschleiert war. Bei doppelter Elektrolysezeit, also halber Abscheidungsgeschwindigkeit (3,4 mg/A · min) ίο erhielt man eine Schicht mit etwa Vs der Stärke nach der Erfindung. Diese Schicht war jedoch matt und damit auch unbrauchbar.2. The deposition rate with HEDTA is so low that only a very thin layer is formed which was obscured in the area of high current densities. With double the electrolysis time, i.e. half Deposition rate (3.4 mg / A · min) ίο a layer was obtained with about Vs in thickness the invention. However, this layer was matt and therefore unusable.
3. DTPA führt bei geringer Abscheidegeschwindigkeit zu unbrauchbaren Schichten.
4. Lediglich der erfindungsgemäße Nickelkomplex führt zu einwandfreien Schichten bei ausgesprochen
guter Abscheidegeschwindigkeit.3. If the deposition rate is slow, DTPA leads to unusable layers.
4. Only the nickel complex according to the invention leads to perfect layers with an extremely good deposition rate.
Claims (1)
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US677818A US2905601A (en) | 1957-08-13 | 1957-08-13 | Electroplating bright gold |
| BE385099 | 1960-07-26 | ||
| BE471502 | 1960-07-26 | ||
| DES0074420 | 1961-06-19 |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| DE1446043A1 DE1446043A1 (en) | 1969-04-10 |
| DE1446043B2 DE1446043B2 (en) | 1970-10-29 |
| DE1446043C3 true DE1446043C3 (en) | 1976-07-22 |
Family
ID=
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