EP0526497A1 - Bains de nickelage acides, contenant 1-(2-sulfoethyl)-betaine de pyridinium. - Google Patents

Bains de nickelage acides, contenant 1-(2-sulfoethyl)-betaine de pyridinium.

Info

Publication number
EP0526497A1
EP0526497A1 EP91907848A EP91907848A EP0526497A1 EP 0526497 A1 EP0526497 A1 EP 0526497A1 EP 91907848 A EP91907848 A EP 91907848A EP 91907848 A EP91907848 A EP 91907848A EP 0526497 A1 EP0526497 A1 EP 0526497A1
Authority
EP
European Patent Office
Prior art keywords
nickel baths
concentrations
acidic nickel
baths according
sulfoethyl
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
Application number
EP91907848A
Other languages
German (de)
English (en)
Other versions
EP0526497B1 (fr
Inventor
Wolfgang Dahms
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.)
Atotech Deutschland GmbH and Co KG
Original Assignee
Schering AG
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.)
Filing date
Publication date
Application filed by Schering AG filed Critical Schering AG
Publication of EP0526497A1 publication Critical patent/EP0526497A1/fr
Application granted granted Critical
Publication of EP0526497B1 publication Critical patent/EP0526497B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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
    • C25D3/14—Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
    • C25D3/18—Heterocyclic compounds

Definitions

  • the invention relates to acidic nickel baths containing l- (2-sulfoethyl) pyridinium betaine.
  • Acidic nickel baths are known, for example from the documents US Pat. No. 3,862,019, DE-PS 36 32 514, EP-A-0343 559, DD-PS 0266 814 and EP-A 0341 167.
  • a group of the additives also called basic gloss, are unsaturated, mostly aromatic sulfonic acids, sulfinic acids, sulfonamides, or their salts.
  • the best known compounds are, for example, m-benzene disulfonic acid or benzoic acid sulfimide (saccharin).
  • leveling agents substances which are referred to as leveling agents. They are practically always used together with one or more basic glosses.
  • levelers are, for example, triple unsaturated alcohols or triple unsaturated amines. They show above all during continuous operation and even with a slight overdose, dark deposits in the low current density range. It is often the case that no deposition occurs in the low current density range and the background material remains visible.
  • levelers quaternary aromatic nitrogen-containing compounds such as pyridinium or quinolinium compounds are known as levelers. All these leveling agents have in common that they embrittle the nickel deposit either at the beginning, but mostly in continuous operation. Subsequent deformation of the nickel-plated parts is no longer possible, and cracks also spontaneously occur that extend into the base material and cause corrosion (for example, rust).
  • the object of the present invention is to avoid the disadvantages described and to provide a bath which, with a sufficiently good depth spread, prevents a good leveling and, in the case of prolonged operation of the acidic nickel baths, prevents the deposition of brittle precipitates, with the lowest consumption of bath constituents.
  • 1- (2-Sulfoethyl) pyridinium betaine is a known substance (U.S. Patent 3,131,189, J. Org. Chem., 29, 2489 (1964), J. Org. Chem., 26, 4520 (1961) and differs of l- (3-sulfopropyl) pyridinium betaine (DE-PS 1004011) through a better effectiveness in the approach and consumption.
  • the bath for the deposition of nickel deposits with the addition of the substance according to the invention generally consists of a nickel salt solution, to which a weak acid is additionally added for buffering.
  • the pH is between 3 and 5.5; mainly between 4 and 5.
  • the temperature can be up to 75 ° C to increase the current density, usually it is between 50 ° and 60 ° C.
  • High-performance electrolytes have a chloride content of 10-50 g / 1 and show the best results when using the compounds according to the invention. Some or all of the nickel chloride can be replaced by sodium chloride.
  • the current density can be up to 10 A / dm 2 at 55 ° C for the designated high-performance electrolytes.
  • the substance according to the invention can be added to the electrolyte on its own, but optimum results can only be achieved by combining it with known base glossers and leveling agents (Tables 1 and 2). In this way, an excellent leveling can be achieved over the entire current density range required in practice, without the precipitation becoming brittle in continuous operation.
  • the concentration of the compounds according to the invention in nickel electrolytes is very low and can be between 0.005 and 5 g / 1, generally between 0.05 and 0.4 g / 1.
  • the concentration is particularly in the lower range when the - h - Compounds according to the invention can be used in combination of base glosses together with triple unsaturated compounds.
  • the basic glosses according to Table 1 are generally added to the electrolyte in amounts of 0.1-10 g / l.
  • Levelers according to Table 2 are expediently metered in between 0.005 and 0.25 g / l.
  • Wetting agents to prevent porous deposition can be added in amounts of up to 10 g / l.
  • levelers that can be added to the bath.
  • Example 1.0 In addition to the compound according to the invention, 1 g / 1 saccharin, sodium salt is added to the electrolyte according to Example 1.0.
  • the sheet shows a high-gloss and well-leveled deposition in the current density range of 2-8 A / dm 2 .
  • Example 2.0 If in Example 2.0 the N, N-diethylaminopropin is replaced by 0.07 g / 1 2-butynediol (1.4), a highly glossy and very good leveled separation is obtained in the range from 0.3 to 8 A / dm 2 .
  • Example 2.0 If, in Example 2.0, the N, N-diethylaminopropin is replaced by 0.03 g / 1 ethylene glycol monopropargyl ether, a high-gloss and very well-leveled deposit is obtained in the range from 0.2 to 8.2 A / dm 2 .
  • N-diethylaminopropin is replaced by 0.007 g / l of propargyl alcohol, the result is in the range from 0.3 to
  • Example 2 If in Example 2, .0 the N, N-diethylaminopropin is replaced by 0.15 g / 1 hydroxypropinsulfonic acid, sodium salt, a high-gloss and very well-leveled deposit is obtained in the range from 0.1 to 8 A / dm 2 .
  • Example 2.0 If in Example 2.0 the N, N-diethylaminopropin is replaced by 0.05 g / 1 propynesulfonic acid, sodium salt, the result is - a - range from 0.2 to 9 A / dm 2 a high-gloss and well-leveled deposition.
  • a consumption of 60 g is determined based on a charge passage of 1000 Ah.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
  • Pyridine Compounds (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
  • Chemically Coating (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Investigating Or Analysing Biological Materials (AREA)

Abstract

La présente invention se rapporte à des bains de nickelage acides, contenant 1-(2-sulfoéthyl)-bétaïne de pyridinium.
EP91907848A 1990-04-23 1991-04-22 Bains de nickelage acides, contenant 1-(2-sulfoethyl)-betaine de pyridinium Expired - Lifetime EP0526497B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE4013349A DE4013349A1 (de) 1990-04-23 1990-04-23 1-(2-sulfoaethyl)pyridiniumbetain, verfahren zu dessen herstellung sowie saure nickelbaeder enthaltend diese verbindung
DE4013349 1990-04-23
PCT/DE1991/000336 WO1991016474A1 (fr) 1990-04-23 1991-04-22 Bains de nickelage acides, contenant 1-(2-sulfoethyl)-betaïne de pyridinium

Publications (2)

Publication Number Publication Date
EP0526497A1 true EP0526497A1 (fr) 1993-02-10
EP0526497B1 EP0526497B1 (fr) 1995-02-08

Family

ID=6405158

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91907848A Expired - Lifetime EP0526497B1 (fr) 1990-04-23 1991-04-22 Bains de nickelage acides, contenant 1-(2-sulfoethyl)-betaine de pyridinium

Country Status (8)

Country Link
US (1) US5264112A (fr)
EP (1) EP0526497B1 (fr)
JP (1) JP3199729B2 (fr)
AT (1) ATE118253T1 (fr)
DE (2) DE4013349A1 (fr)
ES (1) ES2068577T3 (fr)
HK (1) HK3596A (fr)
WO (1) WO1991016474A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE69829188T2 (de) * 1997-08-01 2005-12-29 Reilly Industries, Inc., Indianapolis Supernukleophile in 4-stellung substituierte pyridinkatalysatoren und verfahren die nützlich zu deren herstellung sind
DE19805487A1 (de) 1998-02-11 1999-08-12 Basf Ag Synthese von 1-(2-Sulfoethyl)-pyridiniumbetain
DE102014207778B3 (de) * 2014-04-25 2015-05-21 Kiesow Dr. Brinkmann GmbH & Co. KG Verwendung einer Mischung zur Verwendung in einem galvanischen Bad oder eines galvanischen Bades zur Herstellung einer Glanznickelschicht sowie Verfahren zur Herstellung eines Artikels mit einer Glanznickelschicht
US10458032B2 (en) * 2017-06-15 2019-10-29 Rohm And Haas Electronic Materials Llc Environmentally friendly nickel electroplating compositions and methods
US10718059B2 (en) * 2017-07-10 2020-07-21 Rohm And Haas Electronic Materials Llc Nickel electroplating compositions with cationic polymers and methods of electroplating nickel
EP3456870A1 (fr) * 2017-09-13 2019-03-20 ATOTECH Deutschland GmbH Bain et procédé de remplissage d'une tranchée ou d'un accès d'interconnexion verticale d'une pièce à usiner, de nickel ou d'un alliage de nickel

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL100419C (fr) * 1955-03-16
US3131189A (en) * 1961-10-16 1964-04-28 Pure Oil Co Preparation of quaternary ammonium betaine salts
FR1529883A (fr) * 1967-05-11 1968-06-21 Conservatoire Nat Arts Procédé de sulfoéthylation d'amines tertiaires et nouveaux composés obtenus
DE1621157A1 (de) * 1967-08-16 1971-05-19 Riedel & Co Saures galvanisches Nickelbad
US3862019A (en) * 1974-04-26 1975-01-21 R O Hull & Company Inc Composition of electroplating bath for the electrodeposition of bright nickel
CA1242809A (fr) * 1985-12-20 1988-10-04 Mitel Corporation Systeme de stockage de donnees
US4673472A (en) * 1986-02-28 1987-06-16 Technic Inc. Method and electroplating solution for deposition of palladium or alloys thereof
DD266814A1 (de) * 1987-10-13 1989-04-12 Leipzig Galvanotechnik Verfahren zur elektrolytischen abscheidung glaenzender nickelschichten
FR2630753B1 (fr) * 1988-05-02 1992-01-03 Piolat Ind Cadres perfores en nickel et leur procede de fabrication
DE3817722A1 (de) * 1988-05-25 1989-12-14 Raschig Ag Verwendung von 2-substituierten ethansulfon-verbindungen als galvanotechnische hilfsstoffe
GB2242200B (en) * 1990-02-20 1993-11-17 Omi International Plating compositions and processes
US5164069A (en) * 1990-11-05 1992-11-17 Shipley Company Inc. Nickel electroplating solution and acetylenic compounds therefor

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO9116474A1 *

Also Published As

Publication number Publication date
DE59104555D1 (de) 1995-03-23
JPH05506695A (ja) 1993-09-30
WO1991016474A1 (fr) 1991-10-31
HK3596A (en) 1996-01-12
DE4013349A1 (de) 1991-10-24
US5264112A (en) 1993-11-23
JP3199729B2 (ja) 2001-08-20
ES2068577T3 (es) 1995-04-16
EP0526497B1 (fr) 1995-02-08
ATE118253T1 (de) 1995-02-15

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