EP0770710B1 - Procédé de dépÔt électrolytique de nickel lisse - Google Patents

Procédé de dépÔt électrolytique de nickel lisse Download PDF

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Publication number
EP0770710B1
EP0770710B1 EP96116639A EP96116639A EP0770710B1 EP 0770710 B1 EP0770710 B1 EP 0770710B1 EP 96116639 A EP96116639 A EP 96116639A EP 96116639 A EP96116639 A EP 96116639A EP 0770710 B1 EP0770710 B1 EP 0770710B1
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EP
European Patent Office
Prior art keywords
electrolyte
process according
adducts
operated
nickel
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
Application number
EP96116639A
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German (de)
English (en)
Other versions
EP0770710B2 (fr
EP0770710A1 (fr
Inventor
Carmen Elligsen
Gerd Schöngen
Detlef Kowczyk
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LPW Chemie GmbH
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LPW Chemie GmbH
Priority date (The priority date 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 date listed.)
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Publication date
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Application filed by LPW Chemie GmbH filed Critical LPW Chemie GmbH
Publication of EP0770710A1 publication Critical patent/EP0770710A1/fr
Publication of EP0770710B1 publication Critical patent/EP0770710B1/fr
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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
    • C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt

Definitions

  • the invention relates to a method for galvanic Separation of glare-free nickel deposits on one metallic surface.
  • nickel precipitation also includes nickel alloy precipitation.
  • metallic surface also includes metallized surfaces of non-metallic objects.
  • the deposition is operated so that the electrolyte has a temperature in the Has a range of 40 to 75 ° C.
  • the adducts are like this selected that the adducts in the working electrolyte form a finely dispersed emulsion that turns out to be turbidity expresses.
  • the droplets of the emulsion are the reason for this viewed that a glare-free surface forms.
  • the Glare-free is in need of improvement.
  • nonionic surfactant can be used can, because the cloud point, that is, the electrolyte temperature, at which the surfactant precipitates, from which chemical structure and concentration of substances in the Electrolyte depends.
  • the drop of emulsion increases the risk of agglomeration unsuitably large conglomerates of emulsion drops that satin-like deposition disturb, so large that special Measures are mandatory to complete the procedure to be able to use it permanently in practice.
  • the invention is based on the technical problem that Procedure of the structure described at the beginning and of the beginning described purpose so that reproducibly a much improved defined Glare-free is achieved.
  • the usual basic gloss agents used are "sulfonic acids such as benzenesulfonic acid, naphthalenetrisulfonic acid, alkanesulfonic acids or also sulfonamides or sulfonimides or the corresponding alkali salts" or mixtures thereof, in an amount of 0.5 to 10 g / l.
  • a substance from the group "the unsaturated aliphatic sulfonic acids or their alkali metal salts" or mixtures thereof are used for the purpose of producing the glare-free nickel deposits.
  • the concentration of the adducts added is expediently chosen in the range from 0.5 to 10 g / l.
  • the electrolyte is preferably operated in a temperature range of 50 to 65 ° C during the electrolytic deposition. Wetting agents and organic sulfinic acids or their alkali salts can also be added to the electrolyte.
  • the invention is based on the knowledge that even without Formation of a visible, cloudy emulsion and corresponding organic foreign matter in the electrolyte high quality glare control is achieved when after the teaching of the invention is proceeded.
  • the invention applied nickel layer has a completely different structure than the known method described above generated. That is related below Exemplary embodiments explained. It can be left open remain whether according to the invention are still teardrop-shaped at all Precipitations occur. Drop-shaped precipitates are in the Precipitation mainly related to the surface tension is stabilized as drops. In any case, the effects occur for the qualitative high-quality, reproducible glare control is required - and surprisingly, disruptive conglomerates that disturb the glare-free and have to be filtered, not observed.
  • the current densities can largely be adapted to the operating conditions. It has proven useful to operate the electrolyte with a current density of 0.1 to 10 A / dm 2 .
  • the electrolyte is preferably operated with a current density of approximately 4 A / dm 2 .
  • the treatment time for the nickel deposition is largely arbitrary and can be adapted to the operating conditions, in particular also the layer thickness. Within the scope of the invention, the treatment time for the nickel deposition is preferably 1 to 120 min., Preferably about 10 min. is.
  • the electrolyte can always be operated without secondary circulation. Secondary circuit free means that a secondary circuit with filter devices or cooling devices is not required.
  • Example 1 The anti-glare of the coating according to Example 1 is compared to the embodiment of Example 2 clearly improved.

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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)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)
  • Physical Vapour Deposition (AREA)
  • Electrolytic Production Of Metals (AREA)

Claims (10)

  1. Procédé de dépôt par électrolyse de précipités de nickel antireflets sur une surface métallique, caractérisé par le fait que :
    1.1) on utilise un électrolyte du groupe "électrolyte de Watts, électrolytes à base de sulfamate, de sulfonate, de fluoroborate" ou des mélanges de ceux-ci, auquel on ajoute un brillanteur de fond usuel,
    1.2) pour produire les précipités de nickel antireflets, on utilise des produits d'addition d'oxyde d'éthylène ou d'oxyde de propylène ou d'oxyde d'éthylène-oxyde de propylène, substitués ou non substitués, et on les ajoute à l'électrolyte,
    1.3) la concentration du produit d'addition ajouté selon 1.2) est choisie dans l'intervalle allant de >0 à 5 mg/l,
    1.4) lors du dépôt par électrolyse, l'électrolyte est mis en oeuvre dans un intervalle de température allant de 40 à 75 °C,
    sous réserve que la concentration mentionnée au 1.3) et la température mentionnée au 1.4) soient choisies de façon à ce que, lors de l'observation visuelle, l'électrolyte utilisé paraisse transparent et que l'on n'observe pratiquement pas de dispersion diffuse de la lumière traversant l'électrolyte.
  2. Procédé selon la revendication 1, dans lequel on utilise un électrolyte de Watts pour lequel l'analyse recommandée est :
    70 à 140 g/l de nickel,
    1 à 20 g/l de chlorure,
    30 à 50 g/l de H3BO3
    le reste étant constitué par le brillanteur de fond, le produit d'addition et de l'eau.
  3. Procédé selon la revendication 1 ou 2, dans lequel on utilise, en tant que brillanteur de fond, une substance du groupe "2-sulfobenzoimide, acide 1,3-benzènedisulfonique et acide naphtalène-trisulfonique ou leurs sels alcalins" ou des mélanges de ceux-ci ou du groupe "acides arylsulfoniques, acides alkylsulfoniques, sulfonamides et sulfonimides et leurs sels alcalins " ou des mélanges de ceux-ci et ce, en une quantité allant de 0,5 à 10 g/l.
  4. Procédé selon l'une quelconque des revendications 1 à 3, dans lequel on utilise, en tant que brillanteur de fond, une substance du groupe "acides sulfoniques aliphatiques insaturés ou leurs sels alcalins" ou des mélanges de ceux-ci.
  5. Procédé selon la revendication 4, dans lequel la concentration du brillanteur de fond est choisie dans un intervalle allant de 0,5 à 10 g/l.
  6. Procédé selon l'une quelconque des revendications 1 à 5, dans lequel, lors du dépôt par électrolyse, l'électrolyte est mis en oeuvre dans un intervalle de température allant de 50 à 65 °C.
  7. Procédé selon l'une quelconque des revendications 1 à 6, dans lequel l'électrolyte est mis en oeuvre avec une densité de courant allant de 0,1 à 10 A/dm2.
  8. Procédé selon l'une quelconque des revendications 1 à 7, dans lequel l'électrolyte est mis en oeuvre avec une densité de courant d'environ 4 A/dm2.
  9. Procédé selon l'une quelconque des revendications 1 à 8, dans lequel le temps de traitement pour le dépôt de nickel atteint 1 à 120 minutes, de préférence environ 10 minutes.
  10. Procédé selon l'une quelconque des revendications 1 à 9, dans lequel l'électrolyte est mis en oeuvre sans recirculation secondaire.
EP96116639A 1995-10-27 1996-10-17 Procédé de dépôt électrolytique de nickel lisse Expired - Lifetime EP0770710B2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19540011 1995-10-27
DE9540011U 1995-10-27
DE19540011A DE19540011C2 (de) 1995-10-27 1995-10-27 Verfahren zur galvanischen Abscheidung von blendfreien Nickel- oder Nickellegierungsniederschlägen

Publications (3)

Publication Number Publication Date
EP0770710A1 EP0770710A1 (fr) 1997-05-02
EP0770710B1 true EP0770710B1 (fr) 1999-01-07
EP0770710B2 EP0770710B2 (fr) 2002-08-14

Family

ID=7775920

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96116639A Expired - Lifetime EP0770710B2 (fr) 1995-10-27 1996-10-17 Procédé de dépôt électrolytique de nickel lisse

Country Status (6)

Country Link
US (1) US5897763A (fr)
EP (1) EP0770710B2 (fr)
JP (1) JPH09202987A (fr)
AT (1) ATE175453T1 (fr)
DE (2) DE19540011C2 (fr)
ES (1) ES2128135T5 (fr)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6251253B1 (en) * 1999-03-19 2001-06-26 Technic, Inc. Metal alloy sulfate electroplating baths
JP2002540291A (ja) * 1999-03-19 2002-11-26 テクニツク・インコーポレーテツド 電気めっき槽
US6248228B1 (en) * 1999-03-19 2001-06-19 Technic, Inc. And Specialty Chemical System, Inc. Metal alloy halide electroplating baths
US6797141B1 (en) * 1999-11-25 2004-09-28 Enthone Inc. Removal of coagulates from a non-glare electroplating bath
US6306275B1 (en) * 2000-03-31 2001-10-23 Lacks Enterprises, Inc. Method for controlling organic micelle size in nickel-plating solution
DE10025552C1 (de) * 2000-05-19 2001-08-02 Atotech Deutschland Gmbh Saures galvanisches Nickelbad und Verfahren zum Abscheiden eines satinglänzenden Nickel- oder Nickellegierungsüberzuges
DE10222962A1 (de) * 2002-05-23 2003-12-11 Atotech Deutschland Gmbh Saurer galvanischer Badelektrolyt und Verfahren zur elektrolytischen Abscheidung satinglänzender Nickelniederschläge
JP4811880B2 (ja) * 2006-01-06 2011-11-09 エントン インコーポレイテッド 艶消し金属層を堆積するための電解液および工程
EP2620529B1 (fr) * 2012-01-25 2014-04-30 Atotech Deutschland GmbH Procédé de production de dépôts de cuivre mate
JP6760166B2 (ja) 2017-03-23 2020-09-23 トヨタ自動車株式会社 ニッケル皮膜の形成方法及び当該方法に使用するためのニッケル溶液
US11505867B1 (en) 2021-06-14 2022-11-22 Consolidated Nuclear Security, LLC Methods and systems for electroless plating a first metal onto a second metal in a molten salt bath, and surface pretreatments therefore

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2238861A (en) * 1938-07-06 1941-04-15 Harshaw Chem Corp Electrodeposition of metals
DE1134258B (de) * 1959-05-06 1962-08-02 Dehydag Gmbh Saures galvanisches Nickelbad
US3839166A (en) * 1967-05-16 1974-10-01 Henkel & Cie Gmbh Method for obtaining nickel deposits with satin finish
DE1621085C3 (de) * 1967-05-16 1980-02-14 Henkel Kgaa, 4000 Duesseldorf Saures galvanisches Bad zur Abscheidung satinglanzender Nickelniederschlage
US3839165A (en) * 1967-08-26 1974-10-01 Henkel & Cie Gmbh Nickel electroplating method
BE794695A (fr) * 1972-01-29 1973-05-16 W Kampschulte & Cie K G Dr Bain galvanique de nickel pour la separation de revetements de nickel satines mats
DE2327881B2 (de) * 1973-06-01 1978-06-22 Langbein-Pfanhauser Werke Ag, 4040 Neuss Verfahren zur galvanischen Abscheidung mattglänzender Nickel- bzw. Nickel/Kobalt-Niederschläge
JPS56152988A (en) * 1980-04-30 1981-11-26 Nobuyuki Koura Nickel satin finish plating bath of heavy ruggedness
JPS61238993A (ja) * 1985-04-16 1986-10-24 Dai Ichi Kogyo Seiyaku Co Ltd 電気メツキ浴用添加剤
JPS62205041A (ja) * 1986-03-05 1987-09-09 Nisso Yuka Kogyo Kk １，４−ブチンジオ−ルのヒドロキシアルキルエ−テル化物の製造方法およびこれを用いたニツケルメツキ処理液

Also Published As

Publication number Publication date
ES2128135T3 (es) 1999-05-01
DE59601103D1 (de) 1999-02-18
US5897763A (en) 1999-04-27
ATE175453T1 (de) 1999-01-15
EP0770710B2 (fr) 2002-08-14
EP0770710A1 (fr) 1997-05-02
JPH09202987A (ja) 1997-08-05
DE19540011A1 (de) 1997-04-30
DE19540011C2 (de) 1998-09-10
ES2128135T5 (es) 2003-03-01

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