EP0239876B1 - Bad zum elektrolytischen Abscheiden von Silber-Palladium-Legierungen - Google Patents
Bad zum elektrolytischen Abscheiden von Silber-Palladium-Legierungen Download PDFInfo
- Publication number
- EP0239876B1 EP0239876B1 EP87103932A EP87103932A EP0239876B1 EP 0239876 B1 EP0239876 B1 EP 0239876B1 EP 87103932 A EP87103932 A EP 87103932A EP 87103932 A EP87103932 A EP 87103932A EP 0239876 B1 EP0239876 B1 EP 0239876B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- palladium
- bath
- bath according
- silver
- acid
- 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
- 229910001252 Pd alloy Inorganic materials 0.000 title claims description 12
- SWELZOZIOHGSPA-UHFFFAOYSA-N palladium silver Chemical compound [Pd].[Ag] SWELZOZIOHGSPA-UHFFFAOYSA-N 0.000 title claims description 12
- 238000009713 electroplating Methods 0.000 title 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 54
- 229910052763 palladium Inorganic materials 0.000 claims description 27
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 claims description 17
- 229910052709 silver Inorganic materials 0.000 claims description 13
- 239000004332 silver Substances 0.000 claims description 13
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 claims description 10
- 235000011176 polyphosphates Nutrition 0.000 claims description 8
- 229920000388 Polyphosphate Polymers 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- 239000001205 polyphosphate Substances 0.000 claims description 7
- 229960002317 succinimide Drugs 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 5
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 239000001177 diphosphate Substances 0.000 claims description 4
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical class [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 claims description 4
- 235000011180 diphosphates Nutrition 0.000 claims description 4
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 4
- RXWQRLQUJZRVHB-UHFFFAOYSA-M silver;5-oxo-3,4-dihydropyrrol-2-olate Chemical compound [Ag+].[O-]C1=NC(=O)CC1 RXWQRLQUJZRVHB-UHFFFAOYSA-M 0.000 claims description 4
- 150000001299 aldehydes Chemical class 0.000 claims description 3
- 150000003934 aromatic aldehydes Chemical class 0.000 claims description 3
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 claims description 3
- ZRSNZINYAWTAHE-UHFFFAOYSA-N p-methoxybenzaldehyde Chemical compound COC1=CC=C(C=O)C=C1 ZRSNZINYAWTAHE-UHFFFAOYSA-N 0.000 claims description 3
- 150000002941 palladium compounds Chemical class 0.000 claims description 3
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 claims description 3
- NXJCBFBQEVOTOW-UHFFFAOYSA-L palladium(2+);dihydroxide Chemical compound O[Pd]O NXJCBFBQEVOTOW-UHFFFAOYSA-L 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 239000007795 chemical reaction product Substances 0.000 claims 2
- -1 palladium nitrite compound Chemical class 0.000 claims 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 claims 1
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 238000005282 brightening Methods 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- OQZCJRJRGMMSGK-UHFFFAOYSA-M potassium metaphosphate Chemical compound [K+].[O-]P(=O)=O OQZCJRJRGMMSGK-UHFFFAOYSA-M 0.000 claims 1
- 235000019828 potassium polyphosphate Nutrition 0.000 claims 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 claims 1
- 239000004094 surface-active agent Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 3
- 239000004327 boric acid Substances 0.000 description 3
- SMQUZDBALVYZAC-UHFFFAOYSA-N salicylaldehyde Chemical class OC1=CC=CC=C1C=O SMQUZDBALVYZAC-UHFFFAOYSA-N 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- AEPKDRAICDFPEY-UHFFFAOYSA-L palladium(2+);dinitrite Chemical compound [Pd+2].[O-]N=O.[O-]N=O AEPKDRAICDFPEY-UHFFFAOYSA-L 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 235000019830 sodium polyphosphate Nutrition 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000000080 wetting agent Substances 0.000 description 2
- KJPRLNWUNMBNBZ-QPJJXVBHSA-N (E)-cinnamaldehyde Chemical class O=C\C=C\C1=CC=CC=C1 KJPRLNWUNMBNBZ-QPJJXVBHSA-N 0.000 description 1
- BHYLCQRRNWUVHE-UHFFFAOYSA-N 3-ethylpyrrolidine-2,5-dione Chemical compound CCC1CC(=O)NC1=O BHYLCQRRNWUVHE-UHFFFAOYSA-N 0.000 description 1
- KAJJUFUPJGVIFJ-UHFFFAOYSA-N 3-methylpyrrolidine-2,5-dione Chemical compound CC1CC(=O)NC1=O KAJJUFUPJGVIFJ-UHFFFAOYSA-N 0.000 description 1
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 239000012928 buffer substance Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- HBEQXAKJSGXAIQ-UHFFFAOYSA-N oxopalladium Chemical compound [Pd]=O HBEQXAKJSGXAIQ-UHFFFAOYSA-N 0.000 description 1
- 229910003445 palladium oxide Inorganic materials 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000000153 supplemental effect Effects 0.000 description 1
- MWOOGOJBHIARFG-UHFFFAOYSA-N vanillin Chemical class COC1=CC(C=O)=CC=C1O MWOOGOJBHIARFG-UHFFFAOYSA-N 0.000 description 1
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
-
- 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
- C25D3/64—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of silver
Definitions
- the present invention relates to an aqueous bath for the electrolytic deposition of silver-palladium alloys with the features specified in the preamble of claim 1.
- a bath with these features which is used to deposit silver-palladium alloys with up to 5 percent by weight of palladium, is known from DE-OS 27 04 691.
- it contains silver as silver nitrate, palladium as palladium-ethylenediamine sulfate and succinimide and sodium hydroxide solution, with which a pH of 8 is set.
- the known bath composition is unsuitable for the deposition of silver-palladium alloys with a higher palladium content.
- the invention has for its object to provide an aqueous, cyanide-free, alkaline bath for the deposition of silver-palladium alloys with a higher proportion of palladium and with the largest possible composition range.
- potassium hydroxide or sodium hydroxide can additionally be added in a manner known per se. Usable separation conditions are achieved with a pH between 7 and 12; a pH value between 8 and 10 is optimal.
- a buffer substance can be added in a manner known per se; Standard buffers are suitable, for example borates, phosphates and dicarboxylic acids; e.g. the pH value can be stabilized to values between 8 and 10 using a boric acid / sodium hydroxide solution.
- the bath according to the invention contains the silver in the form of a complex compound with succinimide or its derivatives (e.g. 2-methylsuccinimide, 2-ethylsuccinimide or maleimide) insofar as they are easily soluble in weakly alkaline, aqueous solution.
- succinimide or its derivatives e.g. 2-methylsuccinimide, 2-ethylsuccinimide or maleimide
- the bath according to the invention can contain between 0.5 and 15 g / l of silver and between 1 and 25 g / l of palladium. It can be used to deposit silver-palladium alloys in which the weight ratio of silver to palladium can be set between 20/80 and 80/20; the setting is made by appropriately setting the silver concentration and palladium concentration in the bath and by choosing the bath temperature.
- the palladium is contained in the bath according to the invention in the form of palladium diphosphate and / or palladium polyphosphate. These compounds can be added directly to the bath; it is also possible to add a palladium nitrite complex compound to the bath and to react it in excess with diphosphoric acid or polyphosphoric acid or its salts, for example with potassium diphosphate. Instead of a palladium nitrite complex compound, it is also possible to start from other palladium compounds, in particular from palladium hydroxide, and to react this in excess with di- or polyphosphoric acid or its salts. The succinimide should expediently also be present in excess. The excess of complexing substances is intended to make it possible for the palladium and the silver, which have been in the bath from the beginning or have been added in the form of a supplemental salt over time, to be bound in a completely complex manner.
- the bath according to the invention expediently contains an additive which acts as a wetting agent and favors the formation of a fine-grained and crack-free silver-palladium alloy.
- an additive which acts as a wetting agent and favors the formation of a fine-grained and crack-free silver-palladium alloy.
- Water-soluble, sulfonated, aromatic aldehydes, of which anisaldehyde sulfonic acid and benzaldehyde disulfonic acid are particularly noteworthy, have proven to be particularly suitable fine grain additives and wetting agents for the bath according to the invention.
- sulfonated aromatic aldehydes are sulfonated vanillin, sulfonated salicylaldehyde and sulfonated cinnamaldehyde.
- the sulfonated aldehydes are advantageously added to the bath in an amount of 0.1 to 5 g / l, preferably 1 to 3 g / l.
- Ductile, crack-free coatings made of silver-palladium alloys with a satin-gloss surface can be deposited with baths of the composition according to the invention.
- a pH of 9.5 is set in the bath by adding potassium hydroxide and the deposition is carried out at a temperature of 25 ° C. and a current density of 0.5 A / dm 2 through. It is best to use platinum-coated titanium as anodes, which do not dissolve in the bath.
- the deposited silver-palladium alloy is ductile and crack-free and has a satin surface.
- a pH of 9.5 is set by adding potassium hydroxide and the deposition is carried out at a temperature of 40 ° C. and a current density of 0.5 A. / dm2.
- Platinum-plated titanium is best chosen as the anode material.
- the deposited silver-palladium alloy is ductile and crack-free and has a satin surface.
- a pH of 9.5 is set by adding potassium hydroxide and the deposition is carried out at a temperature of 40 ° C. and a current density of 0.5 ⁇ m 2 performed.
- Platinum-plated titanium is best chosen as the anode material.
- the deposited silver-palladium alloy is ductile and crack-free and has a satin surface.
Landscapes
- 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)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3609309 | 1986-03-20 | ||
| DE19863609309 DE3609309A1 (de) | 1986-03-20 | 1986-03-20 | Bad zum elektrolytischen abscheiden von silber-palladium-legierungen |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0239876A1 EP0239876A1 (de) | 1987-10-07 |
| EP0239876B1 true EP0239876B1 (de) | 1990-09-05 |
Family
ID=6296792
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP87103932A Expired - Lifetime EP0239876B1 (de) | 1986-03-20 | 1987-03-18 | Bad zum elektrolytischen Abscheiden von Silber-Palladium-Legierungen |
Country Status (2)
| Country | Link |
|---|---|
| EP (1) | EP0239876B1 (enrdf_load_stackoverflow) |
| DE (2) | DE3609309A1 (enrdf_load_stackoverflow) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02104699A (ja) * | 1988-10-11 | 1990-04-17 | C Uyemura & Co Ltd | 銀の電解剥離剤及び電解剥離方法 |
| DE4412253C2 (de) * | 1993-04-07 | 1996-05-15 | Atotech Deutschland Gmbh | Elektrolytische Abscheidung von Palladium oder Palladiumlegierungen |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52105540A (en) * | 1976-03-01 | 1977-09-05 | Tech Inc | Silver bath for lusterous plating of nonncyanide |
| BR8001854A (pt) * | 1979-04-04 | 1980-11-18 | Engelhard Min & Chem | Banho de revestimento de prata ou liga da mesma e respectivo processo de estabilizacao |
| US4487665A (en) * | 1980-12-17 | 1984-12-11 | Omi International Corporation | Electroplating bath and process for white palladium |
| US4478692A (en) * | 1982-12-22 | 1984-10-23 | Learonal, Inc. | Electrodeposition of palladium-silver alloys |
-
1986
- 1986-03-20 DE DE19863609309 patent/DE3609309A1/de active Granted
-
1987
- 1987-03-18 DE DE8787103932T patent/DE3764685D1/de not_active Expired - Lifetime
- 1987-03-18 EP EP87103932A patent/EP0239876B1/de not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| DE3609309A1 (de) | 1987-09-24 |
| DE3609309C2 (enrdf_load_stackoverflow) | 1988-06-01 |
| DE3764685D1 (de) | 1990-10-11 |
| EP0239876A1 (de) | 1987-10-07 |
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