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

• My invention relates to improvements in the electro-deposition of nickel from aqueous acidic baths. It is particularly concerned with the utilization of mixtures of certain types of agents for the purpose of decreasing grain size and increasing the luster of the nickel plate or deposit, and it is especially concerned with the production of electrodeposits of brilliant, highly lustrous, ductile nickel plates.
• the agents of Table I are illustrative of the class of compounds, found to be useful in the practice of my present invention, in accordance with the formula where zero, 1 or 2, the compounds can contain one or two nuclear halogen groups or, where x is zero, the nucleus is unsubstituted.
• fi-bromo isoquinolme. 003-. 02 13. (S-methyl isoquinoline. .'003. 03 14. 2,4-dibromo quinoline 005-. 03 15. 2,4-dichloro quinoline 005-. 03 .16. 2,8-dimethyl guinqline. 005-. 03 17. 1,3-dimetl1yl1soqumol1ne .003 02 18. 3-methyl isoquii'ioline. 003-. 03 19. 2-methyl-8-bromo quinoline. 005-. 03 20. 2-,metl1yl-8-ch10r0 quinoline 005-. 03 21. 3-chloro-2-methyl quinoline. .005-. 03 22. 8-bromo-2-metl1y1 quinoline 005-. 03 23. l-methyl isoquinoline .003. 03
• the agents of Table II are illustrative of the class of compounds which are employed in conjunctionwith the agents of'Table I, in the practice of my invention.
• the agents of Table II fallinto thecategory of organic sulfonamides, sulfonimides and sulfonic acids. They have heretofore been used as brighteners in nickel plating baths as is disclosed in part, for example, in my prior Patents Nos. 2,191,813
• Benzene sulionamide m-carboxylic amide 0. l-3 11. 7-Aldehydo o-benzoyl sulfimide 0.1-3 l2. N-Acetyl benzene sulfonimide 0. 1-2 13. Methoxy benzene sulfonamides 0. 1-1 14. Hydroxymethyl benzene sulfonami 0. 1-2 15, Vinyl snlfmnmide 4-12 16. Allyl sulionamide i-12 17. Benzene sulfonic acids (mono-, di-, and tri-) 1-15 18. p-Brom benzene sulfcnic acid 3-6 19.
• Benzaldehyde sulionic acids (0, m, p) 2-6 20.
• p-Ohlor benzene sulfonic acid " l-l 24.
• Diphenyl sulfonic acid 1-5 25.
• Allyl sulfonic acid 4-12 It will be understood that said sulfonic brighteners may be utilized in their acid form or in the form of salts as, for example, nickel, sodium, potassium or other salts. Especially satisfactory, for use in the practice'of my present invention, are the compounds of Table II corresponding to numbers 1, 2, 3; 1s, 19, 21 and 2a, the latter particularly in the form of their nickel salts.
• the compounds of Table 11 used alone, produce reasonably bright deposits on buffed metals such as bufied brass. However, at least in the ordinary case, they do not accomplish the same dark, brittle, easily stained and have poor adherence characteristics at higher concentrations. If, however, the two different types of compounds represented in Tables I and II are used together in the baths, as I have indicated above, brilliant mirror-like, adherent and ductile deposits are obtained even over matte surfaces.
• the optimum concentration of the compounds will be found to fall within the range of about results on steel polished with 180 emery or on matte (but unburnt) copper plate of 0.0003- '0.0005 thickness but, rather, generally yield plates of somewhat dull and gray appearance in these cases.
• the compounds of Table I in the usual case, when used alone, give a different type of plate than that produced by the compounds of Table II.
• the plates produced with the compounds of Table I alone are fine grained and cloudy at very low concentrations, and are rather 0.005 to about 0.03 gram/liter.
• the compounds of Table II are likewise used in small proportions, in conjunction with the compounds of Table I, amounts of the order of about 0.1 gram/liter to 2 or 3 grams/liter being effective in the usual case. Higher proportions, up to saturation, can, however, be utilized. Ordinarily, it is unnecessary to exceed about 0.5%.
• the aqueous nickel plating baths may be of various types but, in all cases, they are acidic in character.
• the preferred baths are of the socalled acidic grey type which are capable of producing thick, adherent, ductile deposits, those of the Watts type or modifications thereof being particularly desirable.
• the nickel salts may comprise nickel chloride, nickel sulfate, nickel fluoborate, nickel sulfamate, or other nickel salts or mixtures of any two or more of said nickel salts, preferably in conjunction with bufier materials as, for example, boric acid. I prefer to utilize boric acid in the bath as it is, in general, the best cathode film buffer.
• buffers of acidic character may, however, be employed as, for example, formic acid, citric acid, fiuoboric acid, and the like, and such may be used either in place of or in conjunction with boric acid.
• concentration of the boric acid or its equivalent should be above 30 grams per liter, especially in baths operated at somewhat elevated temperatures.
• the baths may also contain various supplemental agents such as anti-pitting agents and the like.
• the baths can be operated at temperatures ranging from about room temperature to almost boiling but, in general, the preferred temperature is in the range of about 40 degrees C. to 65 degrees C. In general, the baths can be operated at pH values ranging from about 2 to about 5.5
• the preferred pH values are from 2.5 to 4.8.
• the cathode current density ranges are quite variable, a range of about 5 to several hundred amperes per square foot being utilizable, the optimum depending upon agitation,
• a bath for the electrodeposition of bright nickel comprising an aqueous acidic solution containing at least one nickel salt selected from the group consisting of nickel chloride and nickel sulfate, said bath also containing, in solution, not more than 1 5 grams per liter of at least one brightener selected from the group consisting of organic sulfonamides, sulfonimides, and sulfonic acids, and, in addition, from about 0.005 to about 0.04 gram per liter of a bath-soluble compound in accordance with the formula where represents a compound selected from the group consisting of guinoline, isoquinoline and C-methyl and ethyl homologues thereof, R is halogen, and .z: is zero to 2.
• a bath for the electrodeposition of bright nickel comprising an aqueous acidic solution of at least one nickel salt, said bath also containing. in solution, not more than about 15 grams per liter of at least onebrightener selected from the group consisting of organic su1fonamides,.sulfonimides, and sulfonic acids, and, in addition, .005-.04 gram per liter of Z-methyl quinoline.
• a bath for the electrodeposition of bright nickel comprising an aqueous acidic solution containing at least one nickel salt selected from the group consisting of nickel, chloride and nickel sulfate, said bath also containing, in 5010mm, not more than about 15 grams per liter of at least one brightenerselected from the group consisting of organic sulfonamides, sulfonimides, and .sulfonic acida'and, in addition, from about 0.005 to about 0.04 gram per liter of Z-methyl quinoline.
• a bath for the electrodeposition of bright nickel comprising an aqueous acidic solution con,- taining at least one nickel salt selected from the group consisting of nickel chloride, and nickel sulfate, said bath also containing, in solution, not more than about 15 grams per liter of at least one brightener selected from the group consisting of organic sulfonamides, sulfonimidea. and sulfonic'acids, and, in additiomfrom about 0.005 to about 0.04 gram per liter of a bath-soluble compound in accordance with the formula 0.04 gram per liter of a mixture of isoquinolineand 2-methyl quinoline.
• a method of electrodepositing nickel to obtain a fine-grained, ductile deposit of high brilliance which comprises electrolyzing an aqueous acidic solution containing at least one nickel salt selected from the group consisting of nickel chloride and nickel sulfate, said bath also containing, in solution, not more than about 15 grams per liter of at least one brightener selected from the group consisting of organic sulfonamides, sulfonimides, and sulfonic acids, and, in addition, from about 0.005 to about 0.04 gram per liter of a bathsoluble compound in accordance with the formula represents a compound selected from the group consisting of quinoline, isoquinoline and C- methyl and ethyl homologues thereof, R. is halogen, and :1: is zero to 2.
• a method of electrodepositing nickel to obtain a fine-grained, ductile deposit of high brilliance which comprises electrolyzing an aqueous acidic solution of at least one nickel salt, said bath also containing, in solution, not more than about 0.5% of at least one brightener selected from the group consisting of organic sulfonamides, sulfonimides, and sulfonic acids, and, in addition, from about 0.005 to about 0.04 gram per liter of Z-methyl quinoline.
• a method of electrodepositing nickel to obtain a fine-grained, ductile deposit of high brilliance which comprise electrolyzing an aqueous acidic solution containing at least one nickel salt selected from the group consisting of nickel chloride and nickel sulfate, said bath also containing, in solution, not more than about 5% of at least one brightener selected from the group consisting of organic sulfonamides, sulfonimides, and sulfonic acids, and, in addition, .005-04 gram per liter of a bath-soluble compound in accordance with the formula 8 where R is a halogen selected from the group consisting of chlorine and bromine, and a: is zero to 2.
• a bath for the electrodeposition of bright nickel comprising an aqueous acidic solution containing at least one nickel salt selected from the group consisting of nickel chloride and nickel sulfate, an additive for use in an amount of about .005 to about .04 gram per liter in combination with at least one brightener selected from the group consisting of organic sulfonamides,sulfonimides and sulfonic acids in an amount of not more than about 15 grams per liter in said bath, said additive consisting of a compound having the formula represents a compound selected from the group consisting of quinoline, isoquinoline and C-methyl and ethyl homologues thereof, R. is halogen, and a: is zero to 2.

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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)

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  • BE BE504701D patent/BE504701A/xx unknown
• 1950
  • 1950-07-17 US US174375A patent/US2648628A/en not_active Expired - Lifetime
  • 1950-09-24 DE DEU621A patent/DE888191C/de not_active Expired
• 1951
  • 1951-07-14 NL NL162654A patent/NL82355C/xx active
  • 1951-07-16 FR FR1130462D patent/FR1130462A/fr not_active Expired

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