EP0770710B2 - Verfahren zur galvanischen Abscheidung von blendfreien Nickelniederschlägen - Google Patents

Verfahren zur galvanischen Abscheidung von blendfreien Nickelniederschlägen Download PDF

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Publication number
EP0770710B2
EP0770710B2 EP96116639A EP96116639A EP0770710B2 EP 0770710 B2 EP0770710 B2 EP 0770710B2 EP 96116639 A EP96116639 A EP 96116639A EP 96116639 A EP96116639 A EP 96116639A EP 0770710 B2 EP0770710 B2 EP 0770710B2
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EP
European Patent Office
Prior art keywords
electrolyte
process according
adducts
nickel
operated
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)
French (fr)
Other versions
EP0770710A1 (de
EP0770710B1 (de
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
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Publication date
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    • 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 a metallic surface.
  • Nikkel precipitation also includes nickel alloy precipitation.
  • metallic surface also metallized surfaces of non-metallic Objects.
  • a concentration of adducts in the range of 5 to 100 mg / l worked.
  • the deposition is operated that the electrolyte has a temperature in the range from 40 to 75 ° C.
  • the adducts are selected so that the adducts in the working electrolyte form a finely dispersed emulsion that turns out to be turbidity manifests.
  • the droplets of the emulsion are used as the reason considered that there is a glare-free surface forms. Glare-free is in need of improvement. The printout does not become glare for identification the.
  • the cloud point that is, the electrolyte temperature at which the surfactant fails, from the chemical structure and the concentration depends on the substances in the electrolyte. additionally the salt load of the electrolyte also goes into the Height of the cloud point.
  • the danger of agglomeration is too large Conglomerates of emulsion drops that are satin-like Disrupt separation, so big 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 the procedure of the structure described at the beginning and the intended use described at the beginning to be reproducible so that an essential improved defined glare control is achieved.
  • the usual base gloss agents used are "sulfonic acids such as benzenesulfonic acid, naphthalene trisulfonic 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 the formation of a visible, cloudy emulsion and corresponding organic foreign bodies in the Electrolytes achieved high quality glare control is when proceeding according to the teaching of the invention becomes.
  • the nickel layer applied according to the invention has a completely different structure than that after generated known methods described above. This is discussed below in connection with exemplary embodiments explained. It can be left open whether according to the invention is still drop-shaped at all Precipitations occur. Drop-shaped precipitates are within the scope of the invention, the mainly about the surface tension as drops are stabilized. In any case, the effects occur for the high quality reproducible glare-free are required - and surprisingly disruptive conglomerates that disrupt freedom from glare and need 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 minutes, preferably about 10 minutes. 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.
  • An electrolyte was used to separate out a glare-free nickel deposit 265 g / l NiSO 4 x 7 H 2 O, 53 g / l NiCl 2 x 6 H 2 O, 33 g / l H 3 BO 3 , 1 g / l of benzoic acid sulfonimide sodium salt and 30 mg of propylene oxide / ethylene oxide block polymer (molecular weight 2500) were added.
  • the non-glare of the coating according to Example 1 is compared to the embodiment according to Example 2 clearly improved.

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)
  • Physical Vapour Deposition (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)
  • Electrolytic Production Of Metals (AREA)
EP96116639A 1995-10-27 1996-10-17 Verfahren zur galvanischen Abscheidung von blendfreien Nickelniederschlägen Expired - Lifetime EP0770710B2 (de)

Applications Claiming Priority (3)

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

Publications (3)

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

Family

ID=7775920

Family Applications (1)

Application Number Title Priority Date Filing Date
EP96116639A Expired - Lifetime EP0770710B2 (de) 1995-10-27 1996-10-17 Verfahren zur galvanischen Abscheidung von blendfreien Nickelniederschlägen

Country Status (6)

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

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU773971B2 (en) * 1999-03-19 2004-06-10 Specialty Chemical Systems, Inc. Electroplating baths
US6251253B1 (en) * 1999-03-19 2001-06-26 Technic, Inc. Metal alloy sulfate electroplating baths
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
EP1969160B1 (de) * 2006-01-06 2011-04-27 Enthone, Incorporated Elektrolyt und verfahren zur abscheidung einer matten metallschicht
PL2620529T3 (pl) * 2012-01-25 2014-09-30 Atotech Deutschland Gmbh Sposób wytwarzania matowych warstw miedzianych
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

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1621085A1 (de) † 1967-05-16 1971-03-11 Henkel & Cie Gmbh Saures galvanisches Bad zur Erzeugung satinglaenzender Nickelniederschlaege

Family Cites Families (9)

* 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
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

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1621085A1 (de) † 1967-05-16 1971-03-11 Henkel & Cie Gmbh Saures galvanisches Bad zur Erzeugung satinglaenzender Nickelniederschlaege

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
G. Michael: "Verfahren zur Abscheidung von seidenmatten Nickelüberzügen", Metalloberfläche, Band 25 (1971), Heft 10, Seiten 345-380. †
K. Schulze-Berge: "Blendarmes Glanznickel als Matrix für farbige Beschichtungen, Galvanotechnik, Band 80 (1989), Heft 11, Seiten 3799-3804. †
Merkblatt "Mattierungsbad Supramatt KN 650000" Dr. Hesse & Cie. †
Römpp Chemielexikon, 9. Auflage 1992, Band 6, Seite 4754 †

Also Published As

Publication number Publication date
US5897763A (en) 1999-04-27
EP0770710A1 (de) 1997-05-02
DE19540011C2 (de) 1998-09-10
ATE175453T1 (de) 1999-01-15
JPH09202987A (ja) 1997-08-05
DE19540011A1 (de) 1997-04-30
ES2128135T5 (es) 2003-03-01
ES2128135T3 (es) 1999-05-01
DE59601103D1 (de) 1999-02-18
EP0770710B1 (de) 1999-01-07

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