US3770730A - Electroplating of nickel - Google Patents
Electroplating of nickel Download PDFInfo
- Publication number
- US3770730A US3770730A US00223754A US3770730DA US3770730A US 3770730 A US3770730 A US 3770730A US 00223754 A US00223754 A US 00223754A US 3770730D A US3770730D A US 3770730DA US 3770730 A US3770730 A US 3770730A
- Authority
- US
- United States
- Prior art keywords
- nickel
- compound
- baths
- bath
- leveling
- 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
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D307/78—Benzo [b] furans; Hydrogenated benzo [b] furans
- C07D307/82—Benzo [b] furans; Hydrogenated benzo [b] furans with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to carbon atoms of the hetero ring
- C07D307/83—Oxygen atoms
-
- 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
- R is H, F, Cl or phenyl, and n is a number from 1 to 6 inclusive.
- This invention relates to the electrodeposition of semibright, or bright, sulfur-free, high leveling nickel plate from aqueous acidic nickel plating baths and more particularly, it relates to the use of an addition agent as an improved brightener in acidic nickel plating baths.
- Another object of the present invention is to provide an improved process for electroplating a ductile, lustrous nickel plate.
- the present invention includes a bath for electroplating ductile, lustrous nickel plate which comprises an aqueous acidic nickel plating solution containing at least one soluble nickel plating salt and a brightening amount of a compound having the formula:
- R is H, F, Cl or phenyl, and n is a number from 1 to 6 inclusive.
- the plating bath is an aqueous acidic nickel plating solution which contains at least one soluble nickel plating salt, desirably selected from nickel sulfate, nickel chloride, nickel bromide, nickel sulfamate and nickel fluoroborate, and a brightening amount of a compound falling within the Formula A given above.
- the compound used has the following structure:
- the brightening additives of the present invention may be prepared, generally, by condensing the lactone of an o-hydroxy phenyl acetic acid with an aldehyde. Such preparation is illustrated specifically with regard to the preparation of compound (B) above. In this preparation, the lactone of o-hydroxy phenyl acetic acid is condensed with formaldehyde, as follows:
- benzaldehyde may be used in place of formaldehyde in the above reaction to produce an additive having a phenyl substituted vinyl group.
- Similar reactions may be carried out using o-hydroxy phenyl acetic acid lactones having substituting groups on the benzene ring such as fluoro, chloro, bromo, methyl, methoxy, ethyl, ethoxy, acetyl, acetylamino, propionyl, propionylamino, and sulfoalkyl, or sulfoalkylether groups where the alkyl group is not more than 6 carbons. It is preferred, however, that not more than two such groups be present on the benzene ring.
- the starting materials for the above reaction are prepared according to the preparations described in Organic Syntheses, Collective, vol. III, John Wiley (1955), pp. 715, et seq.
- an aldehyde such as formaldehyde or benzaldehyde is reacted with (D) HOC H -CH CN in the presence of sodium ethoxide.
- the lactone is formed by acidifying the product of the preceding reaction.
- the halogenated materials may be used such as the fluoro, chloro, abromo.
- the alkyl (methyl and ethyl), alkoxy (methoxy and ethoxy) and ketones (methyl and ethyl ketone) are used in place of (D) in the reaction sodium ethoxide.
- NHC0CH and NHCOC H substituted materials that are to be used in place of (D) in the reaction with sodium ethoxide are prepared by reacting the amine precursor with CH COCl or C H COCl as follows:
- the O(CH SO H materials are prepared by reacting:
- the fluorinated materials (where R is F) are prepared by substituting chlorine with fluorine in the presence of SbF according to the Swartz reaction.
- the aqueous acidic nickel plating baths may be of various types, including the Watts type or modifications thereof.
- the nickel salts used in formulating the baths are desirably nickel sulfate, nickel chloride, nickel bromide, nickel sulfamate, nickel fluoborate, as well as mixtures of any two or more of these.
- the nickel salts are preferably used in conjunction with bufler materials, such as boric acid.
- Other acidic type buffers which may be used include formic acid, fluoboric acid, and the like, and these may be used either in place of or in conjunction with boric acid. It has generally been found that optimum results are obtained when the concentration of the boric acid, or its equivalent, is at least about 30 grams/liter.
- Compound (A) may be used in concentrations of 0.05 to 1 gram per liter, preferably 0.1 to 0.3 g./l., when used alone in the baths, especially Watts nickel baths, or dilute all chloride (about 100 g./l. NiCl .6H O) nickel baths. When used alone in such baths it allows the production of ductile, high leveling sulfur-free nickel plate.
- o-benzoyl sulfimide and/ or other class I nickel brightners benzene sulfonamide, naphthalene trisulfonic acid, propargyl sulfonic acid, and the like
- acidic nickel baths sulfate, chloride, bromide, fluoborate, sulfamate
- full bright nickel plate is obtained. It is preferred, however, to use compound (A) in the deposition of semi-bright high leveling, sulfur-free nickel plate.
- the presence of the low foaming wetting agent 2-ethyl hexyl sulfate (sodium salt) is desirable, in concentrations of 0.1 to 0.5 g./l.
- sulfur containing anodes S D nickel
- sodium lauryl sulfate is a preferred wetting agent in concentrations of 0.05 to 0.3 g./l.
- EXAMPLE 2 To the bath of Example 1, 2-10 mg./l. of the 1 to 1 mole 1,3-dioxolane adduct of propargyl alcohol or the 1 to 2 mole propylene oxide adduct of propargyl alcohol are added, thus making it possible to use slightly lower optimum concentrations of compound (B) in the bath, that is 0.1 to 0.2 g./l. instead of 0.2 to 0.6 g./l.
- Example 4 An example of fully bright plating nickel bath is shown in Example 4 below. Instead of o-benzoyl sulfimide, p-toluene sulfonamide and the other well known class I nickel brighteners shown in U.S. Pat. 2,781,306, col 6, Table II may be used.
- sodium lauryl sulfate wetting agent in concentrations of about 0.1 to 0.5 g./l. is preferred over the shorter chain similar surfactants.
- the electroplating baths of the preceding examples may be operated at temperatures from about room temperature to almost boiling, with temperatures within the range of about 40 to 60 0. being preferred.
- the pH values of these baths may range from about 2 to 5.5, although pH values within the range of about 3.0 to 4.8 are preferred.
- the cathode current densities used may also vary, values within the range of about 5 to several hundred amperes/square foot being useful. While the preferred range is about 20 to amperes/square foot, the optimum will depend in each instance on the agitation, temperature, and concentration and type of nickel salts used in the bath.
- the compounds having the Formula A are outstanding nickel brighteners and there is produced an excellent semi-bright or full bright, sulfur-free high leveling nickel plate.
- a more passive plate is produced than with coumarin and the compounds (A), do not hydrolyze in the warm acid nickel plating baths, forming harmful products which cause dulling of the plate and decrease leveling, as do the unsaturated esters such as dimethyl itaconate, and the like.
- R and R are independently selected from the group consisting of ll u -0 CH3 and C 02115 3.
- R and R are independently selected from the group consisting of if i -NHC OH! and NH0 C3115 4.
- R and R are independently selected from the group consisting of --(CH -SO H and O(CH SO H 5.
- R is hydrogen. 6.
- R is independently selected from the group consisting of F and Cl.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
2-(O=),3-(R-CH=),R1,R2-2,3-DIHYDROBENZOFURAN
WHEREIN R1 AND R2 ARE H, CH3, C2H5, F, CL, BR, CH3O-, C2H5O-, CH3CO-, CH3CONH-, -(CH2)N-SO3H, -O(CH2)N-SO3H, C2H5CONH-. R IS H, F, CL OR PHENYL, AND N IS A NUMBER FROM 1 TO 6 INCLUSIVE.
Description
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US12494171A | 1971-03-16 | 1971-03-16 | |
US22375472A | 1972-02-04 | 1972-02-04 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3770730A true US3770730A (en) | 1973-11-06 |
Family
ID=26823114
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US00223754A Expired - Lifetime US3770730A (en) | 1971-03-16 | 1972-02-04 | Electroplating of nickel |
Country Status (1)
Country | Link |
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US (1) | US3770730A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4333920A (en) * | 1979-02-23 | 1982-06-08 | Van Dyk & Company, Inc. | Benzalphthalides and broad spectrum sun screens |
US4983428A (en) * | 1988-06-09 | 1991-01-08 | United Technologies Corporation | Ethylenethiourea wear resistant electroless nickel-boron coating compositions |
-
1972
- 1972-02-04 US US00223754A patent/US3770730A/en not_active Expired - Lifetime
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4333920A (en) * | 1979-02-23 | 1982-06-08 | Van Dyk & Company, Inc. | Benzalphthalides and broad spectrum sun screens |
US4983428A (en) * | 1988-06-09 | 1991-01-08 | United Technologies Corporation | Ethylenethiourea wear resistant electroless nickel-boron coating compositions |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
AS | Assignment |
Owner name: OXY METAL INDUSTRIES CORPORATION Free format text: CHANGE OF NAME;ASSIGNOR:OXY METAL FINISHING CORPORATION;REEL/FRAME:003967/0084 Effective date: 19741220 |
|
AS | Assignment |
Owner name: HOOKER CHEMICALS & PLASTICS CORP. Free format text: MERGER;ASSIGNOR:OXY METAL INDUSTRIES CORPORATION;REEL/FRAME:004075/0885 Effective date: 19801222 |
|
AS | Assignment |
Owner name: OCCIDENTAL CHEMICAL CORPORATION Free format text: CHANGE OF NAME;ASSIGNOR:HOOKER CHEMICAS & PLASTICS CORP.;REEL/FRAME:004126/0054 Effective date: 19820330 |
|
AS | Assignment |
Owner name: OMI INTERNATIONAL CORPORATION, 21441 HOOVER ROAD, Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:OCCIDENTAL CHEMICAL CORPORATION;REEL/FRAME:004190/0827 Effective date: 19830915 |
|
AS | Assignment |
Owner name: MANUFACTURERS HANOVER TRUST COMPANY, A CORP OF NY Free format text: SECURITY INTEREST;ASSIGNOR:INTERNATIONAL CORPORATION, A CORP OF DE;REEL/FRAME:004201/0733 Effective date: 19830930 |