DE2729116A1 - Aqueous BAEDER FOR THE ELECTROLYTIC DEPOSITION OF PALLADIUM AND ITS ALLOYS - Google Patents
Aqueous BAEDER FOR THE ELECTROLYTIC DEPOSITION OF PALLADIUM AND ITS ALLOYSInfo
- Publication number
- DE2729116A1 DE2729116A1 DE19772729116 DE2729116A DE2729116A1 DE 2729116 A1 DE2729116 A1 DE 2729116A1 DE 19772729116 DE19772729116 DE 19772729116 DE 2729116 A DE2729116 A DE 2729116A DE 2729116 A1 DE2729116 A1 DE 2729116A1
- Authority
- DE
- Germany
- Prior art keywords
- acid
- palladium
- salts
- alkali
- alloys
- 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.)
- Granted
Links
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical group [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims description 27
- 229910052763 palladium Inorganic materials 0.000 title description 10
- 230000008021 deposition Effects 0.000 title description 3
- 229910045601 alloy Inorganic materials 0.000 title description 2
- 239000000956 alloy Substances 0.000 title description 2
- 239000003513 alkali Substances 0.000 claims description 7
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 claims description 6
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 150000002941 palladium compounds Chemical class 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- LCTONWCANYUPML-UHFFFAOYSA-N Pyruvic acid Chemical compound CC(=O)C(O)=O LCTONWCANYUPML-UHFFFAOYSA-N 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- 229920000768 polyamine Polymers 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims 1
- RGHNJXZEOKUKBD-SQOUGZDYSA-M D-gluconate Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O RGHNJXZEOKUKBD-SQOUGZDYSA-M 0.000 claims 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims 1
- 229910002651 NO3 Inorganic materials 0.000 claims 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims 1
- YRZBVIGIGZTWGT-UHFFFAOYSA-N [2-(diphosphonoamino)ethyl-phosphonoamino]phosphonic acid Chemical compound OP(O)(=O)N(P(O)(O)=O)CCN(P(O)(O)=O)P(O)(O)=O YRZBVIGIGZTWGT-UHFFFAOYSA-N 0.000 claims 1
- 229940022663 acetate Drugs 0.000 claims 1
- 150000001412 amines Chemical class 0.000 claims 1
- 150000007514 bases Chemical class 0.000 claims 1
- 239000012928 buffer substance Substances 0.000 claims 1
- 229940001468 citrate Drugs 0.000 claims 1
- 229940050410 gluconate Drugs 0.000 claims 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims 1
- IIACRCGMVDHOTQ-UHFFFAOYSA-M sulfamate Chemical compound NS([O-])(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-M 0.000 claims 1
- 229940095064 tartrate Drugs 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 239000002244 precipitate Substances 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- IIACRCGMVDHOTQ-UHFFFAOYSA-N sulfamic acid Chemical class NS(O)(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-N 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 2
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 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
- C25D3/50—Electroplating: Baths therefor from solutions of platinum group metals
- C25D3/52—Electroplating: Baths therefor from solutions of platinum group metals characterised by the organic bath constituents used
-
- 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
- C25D3/567—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of platinum group metals
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)
- Chemically Coating (AREA)
Description
nungen und Poren sind.openings and pores are.
Es sind auf dem Gebiet der elektrolytischen Abscheidung von Palladium oder seinen Legierungen mehrere Typen von Bädern bekannt. Insbesondere sind die Bäder auf Basis von Palladiumverbindungen zu nennen, wie Diaminodinitro-Palladium (Pd(NO2)2(NH3)2, Dicyanodiamino-Palladium Pd(CN)2(NH3)2, fähige Salze oder Puffersubstanzen enthalten, wie Alkali-Sulfate, -Sulfamate, -Sulfite, -Phosphate, -Pyrophosphate usw. (wobei unter "Alkalien" Alkali- und Erdalkalimetalle und Ammonium zu verstehen sind).Several types of baths are known in the electrodeposition art of palladium or its alloys. In particular, the baths based on palladium compounds should be mentioned, such as diaminodinitro-palladium (Pd (NO2) 2 (NH3) 2, dicyanodiamino-palladium Pd (CN) 2 (NH3) 2, contain capable salts or buffer substances, such as alkali sulfates, sulfamates, sulfites, phosphates, pyrophosphates, etc. (whereby "alkalis" are to be understood as being alkali and alkaline earth metals and ammonium).
lich brüchig sind. Schließlich sind sie bei einer Schichtdicke von 1 bis 2 Mikron fast immer sehr porös, und bei Schichtdicken von mehr als 2 Mikron sind sie oft nicht mehr hochglänzend.are brittle. After all, with a layer thickness of 1 to 2 microns they are almost always very porous, and with a layer thickness of more than 2 microns they are often no longer highly glossy.
zentrationen (SO3") empfindlich reagieren. Wenn deshalb während der Anwendung diese Konzentration ansteigt, so bewirkt dies einen Verlust an Hochglanz und eine zunehmende Porosität der erhaltenen Niederschläge, die gleichzeitig der Sitz von sehr beträchtlichen inneren Spannungen sind.If this concentration rises during use, this causes a loss of gloss and an increasing porosity of the precipitates obtained, which are at the same time the seat of very considerable internal stresses.
thodenleistung weniger als 100 % beträgt. An der Kathode wird dann Wasserstoff freigesetzt, der von dem Niederschlag absorbiert werden kann und der somit die Kristallisation des Metalls oder der metallischen Niederschläge stört. Schließlich ist auch bekannt, dass bestimmte für die elektrolytische Abscheidung von Palladium verwendete Bäder, besonders die Bäder auf Basis von Sulfiten, die Abscheidung dieses Metalls bei einer Kathodenleistung nahe bei 100 % erlauben. Diese Nieder schläge sind allerdings ziemlich brüchig,
denn sie sind
<NichtLesbar>
ten, zeichnen sie sich durch Instabilität im
<NichtLesbar>
aus (Bildung von unlöslichen Niederschlägen), so dass der Benutzer nicht sicher ist, eine zuverlässige Ausbeute und Produkte mit gleichmäßig guter Qualität zu erhalten.method performance is less than 100%. Hydrogen is then released at the cathode, which can be absorbed by the precipitate and which thus interferes with the crystallization of the metal or the metallic precipitates. Finally, it is also known that certain baths used for the electrolytic deposition of palladium, especially baths based on sulfites, allow the deposition of this metal with a cathode output close to 100%. However, these precipitations are quite fragile because they are
<notreadable>
ten, they are characterized by instability in the
<notreadable>
out (formation of insoluble precipitates) so that the user is unsure of a reliable yield and products of consistently good quality.
glänzenden Niederschlägen mit Schichtdicken von mehr als 3 Mikron erlauben, bei denen die inneren Spannungen in beträchtlichem Maße vermindert sind.allow shiny deposits with thicknesses of more than 3 microns, in which the internal stresses are considerably reduced.
konzentration der zwei- oder vierwertigen Palladiumverbindung darstellt) während des Elektrolysevorganges so konstant wie möglich gehalten wird.concentration of the bivalent or tetravalent palladium compound) is kept as constant as possible during the electrolysis process.
konzentration liegen. Was das Verhältnis (SO3")/(Pd) angeht, so sollte es zwischen 2 und 4 gehalten werden. um beschichtet sind.concentration lying. As for the (SO3 ") / (Pd) ratio, it should be kept between 2 and 4. to are coated.
derschläge zu bevorzugen ist, in der Lösung ein Molverhältnis von (SO3")/(Pd) von zwischen 2
<NichtLesbar>
umverbindungen, wie Na2
<NichtLesbar>
gen, die kein Sulfit enthalten. De Zugabe von Sulfit erfolgt vorzugsweise, indem man dem Bad ein Alkalisulfit in angemessener Menge zusetzt.However, it is preferable to have a molar ratio of (SO3 ") / (Pd) of between 2
<notreadable>
reconnections, such as Na2
<notreadable>
genes that do not contain sulfite. Sulfite is preferably added by adding an appropriate amount of alkali sulfite to the bath.
te, Sulfamate, Sulfate, Citrate u. dgl. von Alkalien oder einem aliphatischen Polyamin, wie Diäthylentri-amin, Triäthylentetramin oder Tetraäthylenpentamin.te, sulfamates, sulfates, citrates and the like of alkalis or an aliphatic polyamine, such as diethylenetriamine, triethylenetetramine or tetraethylenepentamine.
Der pH-Wert der erfindungsgemäßen Bäder sollte mit Hilfe von mineralischen oder organischen Alkaliverbindungen, wie vorzugen ist.The pH of the baths according to the invention should with the help of mineral or organic alkali compounds, such as is preferable.
tel enthalten.tel included.
tration an Palladium sowie der von anderen Badbestandteilen beträchtlich variieren.Tration of palladium as well as that of other bath components vary considerably.
Beispiel 1example 1
(NH4)2HPO4 10 g/l Tetraäthylenpentamin 20 ml/l Na2SO3 34 g/l Acetylameisensäure 3 ml/l Pd (in Form von PdNa2Cl4) 10 g/l(NH4) 2HPO4 10 g / l tetraethylene pentamine 20 ml / l Na2SO3 34 g / l acetylformic acid 3 ml / l Pd (in the form of PdNa2Cl4) 10 g / l
Der pH-Wert wird mit Kaliumhydroxid auf 11 eingestellt.The pH is adjusted to 11 with potassium hydroxide.
Man führt mit diesem Bad die Elektrolyse bei 60° C und einer Stromdichte von 0,5 A/dm2 10 Minuten lang durch. Man erhält mit einer Kathodenleistung von 32 bis 33 mg/A.min einen hochglänzenden, unporösen Palladiumniederschlag. bene Weise verfährt, erhält man trübe und schleirige Palladiumniederschläge.The electrolysis is carried out with this bath at 60 ° C. and a current density of 0.5 A / dm2 for 10 minutes. A high-gloss, non-porous palladium precipitate is obtained with a cathode output of 32 to 33 mg / A.min. If this is done in the same way, cloudy and hazy palladium precipitates are obtained.
Beispiel 2
<NichtLesbar>
Example 2
<notreadable>
*) = 30%ige wässrige Lösung eines Chelatbildners (Henkel & Cie.)*) = 30% aqueous solution of a chelating agent (Henkel & Cie.)
Der pH-Wert wird mit Ammoniumhydroxid auf 9,5 eingesellt.The pH is adjusted to 9.5 with ammonium hydroxide.
Man elektrolysiert in diesem Bad bei 30° C und einer Stromdichte von 0,25 A/dm2. Man erhält einen stark hochglänzenden Palladiumniederschlag, der bei einer Schichtdicke von 1,5 bis 2 Mikron praktisch porenfrei ist. Außerdem ist anzumerken, dass die mit diesem Bad erhaltenen Niederschläge selbst bei Schichtdicken von mehr als 10 Mikron keinerlei Risse aufweisen.Electrolysis is carried out in this bath at 30 ° C. and a current density of 0.25 A / dm2. A very high-gloss palladium deposit is obtained which, with a layer thickness of 1.5 to 2 microns, is practically pore-free. It should also be noted that the precipitates obtained with this bath do not show any cracks, even if the layers are thicker than 10 microns.
hält, erhält man schleierige, weißliche Niederschläge, und die Lösung neigt sehr rasch dazu, Schwierigkeiten zu bereiten.holds, haze, whitish precipitates are obtained, and the solution tends very quickly to cause difficulties.
Beispiel 3Example 3
(NH4)2HPO4 30 g/l (NH4)2SO3 26 g/l Pd (in Form von Pd(NH3)2Cl2) 10 g/l(NH4) 2HPO4 30 g / l (NH4) 2SO3 26 g / l Pd (in the form of Pd (NH3) 2Cl2) 10 g / l
Der pH-Wert wird mit Ammoniumhydroxid auf 9,5 eingestellt. stehenden Versuch verfährt, erhält man einen Palladiumniederschlag, der praktisch frei von inneren Spannungen ist. Das Blättchen weist somit auch keine feststellbare oder bemerkenswerte Krümmung auf und bleibt praktisch eben.The pH is adjusted to 9.5 with ammonium hydroxide. If the test is not carried out, a palladium deposit is obtained which is practically free from internal stresses. The leaflet therefore has no noticeable or noticeable curvature and remains practically flat.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CH832276A CH597372A5 (en) | 1976-06-28 | 1976-06-28 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| DE2729116A1 true DE2729116A1 (en) | 1978-01-05 |
| DE2729116C2 DE2729116C2 (en) | 1987-01-29 |
Family
ID=4338548
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DE19772729116 Expired DE2729116C2 (en) | 1976-06-28 | 1977-06-28 | Aqueous bath for the electrolytic deposition of palladium or its alloys and process for the preparation of this bath |
Country Status (3)
| Country | Link |
|---|---|
| CH (1) | CH597372A5 (en) |
| DE (1) | DE2729116C2 (en) |
| FR (1) | FR2356747A1 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3118908C2 (en) * | 1981-05-13 | 1986-07-10 | Degussa Ag, 6000 Frankfurt | Galvanic palladium bath |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1035850A (en) * | 1964-06-12 | 1966-07-13 | Johnson Matthey Co Ltd | Improvements in and relating to the electrodeposition of palladium |
| CH479715A (en) * | 1967-09-08 | 1969-10-15 | Sel Rex Corp | Process for electrolytic plating of palladium, and bath for carrying out this process |
| CH572989A5 (en) * | 1973-04-27 | 1976-02-27 | Oxy Metal Industries Corp | |
| DE2506467C2 (en) * | 1975-02-07 | 1986-07-17 | Schering AG, 1000 Berlin und 4709 Bergkamen | Bath and process for the electrodeposition of palladium-nickel alloys |
-
1976
- 1976-06-28 CH CH832276A patent/CH597372A5/xx not_active IP Right Cessation
-
1977
- 1977-06-27 FR FR7719674A patent/FR2356747A1/en active Granted
- 1977-06-28 DE DE19772729116 patent/DE2729116C2/en not_active Expired
Non-Patent Citations (1)
| Title |
|---|
| NICHTS-ERMITTELT * |
Also Published As
| Publication number | Publication date |
|---|---|
| DE2729116C2 (en) | 1987-01-29 |
| FR2356747A1 (en) | 1978-01-27 |
| CH597372A5 (en) | 1978-03-31 |
| FR2356747B1 (en) | 1981-04-30 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| 8110 | Request for examination paragraph 44 | ||
| D2 | Grant after examination | ||
| 8364 | No opposition during term of opposition | ||
| 8339 | Ceased/non-payment of the annual fee |