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US2852449A - Electrodeposition of nickel - Google Patents

Electrodeposition of nickel Download PDF

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US2852449A
US2852449A US683721A US68372157A US2852449A US 2852449 A US2852449 A US 2852449A US 683721 A US683721 A US 683721A US 68372157 A US68372157 A US 68372157A US 2852449 A US2852449 A US 2852449A
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nickel
dioxane
sulfonimides
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benzene
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Donald H Becking
Brown Henry
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Udylite Research Corp
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/12Electroplating: Baths therefor from solutions of nickel or cobalt
    • C25D3/14Electroplating: Baths therefor from solutions of nickel or cobalt from baths containing acetylenic or heterocyclic compounds
    • C25D3/18Heterocyclic compounds

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  • This invention relates to the electrodeposition of nickel and more particularly it relates to the electrodeposition of bright ductile nickel from aqueous acidic nickel electroplating baths.
  • the vinyl substituted saturated ring, m-dioxane, compounds of Table I give far superior brightening results than when the vinyl group is attached to an aromatictype ring such as benzene or pyridine. This is thought to be due to the fact that in the compounds of Table I the vinyl group is, in fact, an allylic group with the terminal, i. e. farthest from thedouble bond carbon atom of the allylic group as part of the dioxane ring.
  • the compounds of Table I are efiective in very low concentrations, and when fast agitation is used (air or mechanical, or hydraulic), concentrations as low as about two or three milligrams per liter show beneficial brightening effects. In general, however, concentrations of about 0.01 to 0.06 gram/liter are preferred, though much higher concentrations can be used, for example, up to about 0.2 gram/liter and in some cases as high as 0.5 gram/liter.
  • Sulfomethyl benzene sulfonamide 0, 1-6 10. Benzene sultonamide m-carboxylic 0. 1-3 11. 7-Aldehydo o-benzoyl sulfilnide 0.1-3 12. N-acetyl benzene sulfonimide. 0.1-2 18. Methoxy benzene sulionamides 0.1-1 14. Hydroxymethyl benzene sulf0namide 0. 1-2 15. Allyl sulfonamide 0. 4-12 16. Benzene sulionie acids (mono-, di-, and tri 1-15 17. p-Brom benzene sulfonic acid 3-6 18. Benzaldehyde sultonie acids (0, m, p) 2-6 19.
  • Di-benzene sulfonimide- 0. 1-3 30.
  • Di-toluene sulf0nimide 0.1-3 31.
  • Z-Butyne- 1,4-disulionie acid. 5-20 32.
  • 4-Hydr0xy-2-butyne-1-su1fonic acid 0.2-2 33.
  • 2-butene-1A-disulfonic acid .03-5 36.
  • fluoborate, and sulfamate baths and mixtures of these various nickel salts may be present, also ammonium ions, though the latter should preferably be kept below about 7 grams per liter for maximum ductility and brightness.
  • Boric acid is the preferred buffer.
  • the best pH range is from about 2.8 to 4.5, though pH values of 2 to 6 may be used.
  • the temperature of' 3 the bath may be from room to 190 F., though in general 120 F.l60 F. is preferred.
  • a suitable surface-active agent such as sodium lauryl sulfate, sodium Z-ethyl hexyl sulfate or sulfonate, octyl sulfonic acid, etc.
  • a surface-active agent such as sodium lauryl sulfate, sodium Z-ethyl hexyl sulfate or sulfonate, octyl sulfonic acid, etc.
  • sodium 2-ethyl sulfate can be used which does not foam excessively, or otherwise a more powerful surface-active agent such as sodium lauryl sulfate can be used in conjunction with an anti-foam such as a silicone oil or a tallow alcohol.
  • the compounds of Table II can be used in amounts between about 0.1 gram/liter and saturation and the preferred organic sultan-compounds to be used with the compounds of Table I are the benzene sulfonamides and sulfonimides (0.1 gram/liter to saturation) especially when used in conjunction with allyl sulfonic acid (0.6-2 grams/liter) or Z-butyne disulfonic acid (3-10 grams/ liter).
  • the preferred compound of Table I is Example 2, which is 3,9-divinyl spirobi (m-dioxane), in a concentration of 0.01 to 0.05 gram/liter.
  • the baths containing compounds of Table I and Table II are not very sensitive to giving poor adhesion due to broken electrical contacts or to small excesses of these compounds, and therefore these compounds do not readily cause double or laminated plates.
  • the compounds of Table I in conjunction with those of Table II give excellent results in bulk, tumble or barrel plating, as well as in the rack plating of steel, zinc diecast, aluminum and brass articles. Especially superior results (brightness and ductility) are obtained with rapid agitation (air agitation or hydraulic agitation).
  • the conjunctive use of the compounds of Table I with the compounds of Table II does not greatly reduce the excellent properties which are characteristic of all of the organic sulfon-compounds of Table II with respect to the low sensitivity of nickel baths containing the latter organic sulfon-compounds to poor adhesion from broken electrical contacts or delayed electrical contacts or from reverse or anodic currents as in periodic current reversals, or in anodic activation of the nickel plate for re-plate. Delays of as long as one minute before electrical contact is made, or anodic currents for as long as one minute in many cases, do not cause poor adhesion.
  • Zinc ions or cadmium ions can be present in most of the nickel baths, especially in high chloride baths, in concentrations of at least 0.05 to 0.1 gram per liter and also not aifect the adhesion during delayed electrical contacts or periodic current reversals.
  • the zinc or cadmium present in the nickel plate causes a more shallow type of corrosion pit to occur in the nickel when chromium plated and exposed to a corrosive atmosphere (for example the atmosphere in industrial areas).
  • the relative insensitivity of such baths to passivity from anodic current makes possible the use of periodic current reversal in its sacrificial form which tends to promote leveling and to improve the corrosion protection afiorded to the underlying metal.
  • a sacrificial periodic current reversal cycle of ten or more seconds anodic current preferably at low anodic current (5 to 10 amps/sq. ft.) with about 1 to 5 seconds cathodic current can be used for periods of about 1 to 2 or more minutes and then the procedure repeated until the desired thickness of plate is obtained.
  • the benzene sulfonamides and sulfonimides and o-benzoyl sulfimide together with small concentrations of the compounds of Table I represent preferred combinations of the compounds of this invention for the periodic current reversal treatments.
  • Example I NiSO .6H O "grams/liter" 200-300 NiCl .6H O do 30-80 H3803 d0 N-aBF do 0-0.S
  • Example 2 of Table I (3,9-divinyl spirobi (m-dioxane) grams/liter 0.01-0.04 Sodium allyl sulfonate do 0.6-2 Benbene sulfonamide do 1-2 o-Benzoyl sulfimide do 0-2 Temperature F 120-160 pH 3.2-4.8
  • Example II NiCl .6H- O grarns/liter -200 -d0 H 30 do 30-50
  • Example 2 of Table I (3,9-divinyl spirobi (m-dioxane) grams/liter- 0.01-0.04 Sodium allyl sulfonate do 0.6-2 o-Benzoyl sulfimide do 1-2 Benzene sulfonamide do 1-2 Temperature F -160 pH 3.2-4.8
  • Example III NiSO .6H O grams/liter 200-300 NiC1 .6H O do 30-100 H3B03 ..d0
  • Example I of Table I (vinyl-m-dioxane) grams/liter 0.01-0.05 o-Benzoyl sulfimide do 0.1-2 Temperature F 120-160 pH 3.2-4.8
  • Example IV NiS0 .6H O grams/liter 200-300 NiCl .6H O do 30-80 H BO do 30-50 NaBF o 0-0.5
  • Example 2 of Table I (3,9-divinyl spirobi (m-dioxane) grams/1iter 0.01-0.04 2-Butyne 1,4-disulfonic acid Na, K, or Ni salt) grams/liter- 3-10 Benzene sultonamide do 1-2 o-Benzoyl sulfimide do 0-2 Temperature F 120-160 pH 3.2-4.8
  • a bath for electrodepositing bright, ductile nickel plate which comprises an aqueous acidic solution containing at least one electrolyte selected from the group consisting of nickel sulfate, nickel chloride, nickel fluoborate and nickel sulfamate, and having dissolved therein about 0.1 gram/ liter to saturation of at least one organic sulfon- .compound selected from the class consisting of benzene, biphenyl and naphthalene sulfonic acids, sulfonamides and sulfonimides and the mixed phenyl, biphenyl and naphthyl sulfonamides and the mono-, di-, tri-, and tetrasulfonimides thereof, and dibenzene sulfonimides and the halogen, methyl, and aldehydo derivatives of said sulfonic acids, sulfonamides and sulfonimides, and beta unsaturated alkene and al
  • a bath in accordance with claim 1 wherein said vinyl substituted m-dioxane compound is 3,9-divinyl spirobi (m-dioxane) and is present in a concentration in the bath of 0.005 to about 0.2 gram/liter.
  • a bath in accordance with claim 1 wherein the vinyl substituted m-dioxane is 3-viny1' m-dioxane and is dissolved in the said nickel bath in a concentration of 0.005 to about 0.2 gram/ liter.
  • a bath in accordance with claim 1 wherein said organic sulfon-compound is allyl sulfonate.
  • a bath in accordance with claim 1 wherein said organic sulfon-compound is 2-butyne-1,4-disulfonate.
  • a method of electrodepositing bright, ductile nickel plate which comprises electrolyzing an aqueous acidic solution comprising at least one nickel salt selected from the group consisting of nickel sulfate, nickel .chloride, nickel fluoborate and nickel sulfamate, said bath containing dissolved therein about 0.1 gram/liter to saturation of at least one organic sulfon-compound selected from the group consisting of benzene, biphenyl and naphthalene sulfonic acids, sulfonamides and sulfonim-ides and the mixed phenyl, biphenyl and naphthyl sulfonamides and the mono-, di-, tri-, and tetrasulfonimides thereof, and dibenzene sulfonimides and the halogen, methyl, and aldehydo derivatives of said sulfonic acids, sulfonamides and sulfonimides, and beta unsaturated al
  • said vinyl Substituted m-dioxane compound is 3,9-divinyl spirobi (m-dioxane) and is present in a concentration in the bath of 0.005 to about 0.2 gram/liter.

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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)

Description

- United States Patent ELECTRODEPOSITION OF NICKEL Donald H. Becking, Birmingham, and Henry Brown, Huntington Woods, Mich., assignors to The Udylite Research Corporation, Detroit, Mich., a corporation of Michigan No Drawing. Application September 13, 1957 Serial No. 683,721
Claims. (Cl. 204-49) This invention relates to the electrodeposition of nickel and more particularly it relates to the electrodeposition of bright ductile nickel from aqueous acidic nickel electroplating baths.
In accordance with this invention, it has been found that certain vinyl substituted m-dioxane compounds, such as those illustrated in Table I, containing the O. CHFCH-Cfi grouping I when used in very small concentrations in aqueous acidic nickel baths in conjunction with the well-known organic sulfon-compounds (as illustrated in Table II) make possible the production of brilliant ductile nickel plate.
While numerous unsaturated compounds have been used in the art in conjunction with sulfon-compounds to obtain bright ductile nickel plate, the number of highly satisfactory unsaturated vinyl substituted compounds have been very few. For example, 2-vinyl pyridine is actually far inferior to pyridine as a nickel brightener when used in conjunction with an aryl sulfoncompound and vinyl benzene is insoluble in a Watts-type nickel bath.
The vinyl substituted saturated ring, m-dioxane, compounds of Table I give far superior brightening results than when the vinyl group is attached to an aromatictype ring such as benzene or pyridine. This is thought to be due to the fact that in the compounds of Table I the vinyl group is, in fact, an allylic group with the terminal, i. e. farthest from thedouble bond carbon atom of the allylic group as part of the dioxane ring.
TABLE I..-Continued Optimum Oonc., Grams/liter CHz=CH-C CHOCHax' 0.01 to 0.06
OCz
7. OCH2 CH2=CHC /CHOC2H5 0. 01 to 0.06
O-CHg 8. O C H: g CHz=OH-C\ CHO(C2H4O),.H 0.01 to 0.06
The compounds of Table I are efiective in very low concentrations, and when fast agitation is used (air or mechanical, or hydraulic), concentrations as low as about two or three milligrams per liter show beneficial brightening effects. In general, however, concentrations of about 0.01 to 0.06 gram/liter are preferred, though much higher concentrations can be used, for example, up to about 0.2 gram/liter and in some cases as high as 0.5 gram/liter.
TABLE II Optimum Sulfur-Containing Brighteners Cone, grams/ liter 1. Benzene sulfonamide 0.1-3 2. Toluene sulionamides (oand p-) 0. 1-2 3. o-Benzoyl sulfimide 0. 1-2 4. N-Benzoyl benzene sultonimide. 0.1-1 5. p-Toluene sultonchloramide. 0. 1-1 6. p-Brom benzene sulonamide 0. 1-1 7. G-Chlor o-benzoyl sulfirnide. 0, 1-1 8. m-Aldebydo benzene snlfonami 0.1-1 9. Sulfomethyl benzene sulfonamide 0, 1-6 10. Benzene sultonamide m-carboxylic 0. 1-3 11. 7-Aldehydo o-benzoyl sulfilnide 0.1-3 12. N-acetyl benzene sulfonimide. 0.1-2 18. Methoxy benzene sulionamides 0.1-1 14. Hydroxymethyl benzene sulf0namide 0. 1-2 15. Allyl sulfonamide 0. 4-12 16. Benzene sulionie acids (mono-, di-, and tri 1-15 17. p-Brom benzene sulfonic acid 3-6 18. Benzaldehyde sultonie acids (0, m, p) 2-6 19. Diphenyl sulfone sulfonic acid 1-8 20. Naphthalene sulfonic acids (mono-, di-, and tr) 1-8 21. Benzene snliohydroxamic acid 1-5 22. p-Chlor benzene sultonic acid- 1-15 23. Diphenyl sulfonic acid 1-5 24. m-Diphenyl benzene sulfonic acid. 1-4 25. 2-0hloro-5-sulfobenzaldehyde 1-5 26. m-Benzene disulfonamide. 0. 5-1 27. Ally] sulionic acid 0. 4-12 28. DichlOrOb'enzene sulfonic a 0. 5-8 29. Di-benzene sulfonimide- 0. 1-3 30. Di-toluene sulf0nimide 0.1-3 31. Z-Butyne- 1,4-disulionie acid. 5-20 32. 4-Hydr0xy-2-butyne-1-su1fonic acid 0.2-2 33. z-Butyne-i-sultonic acid 0. 05-1. 5 34. 3Cl1lor0-2-pr0pyne-1-sulf0nic acid. 0. 05-1. 5 35. 2-butene-1A-disulfonic acid .03-5 36. 2-cl1l0ro butene-4-su1fonic acid- 0. 3-5 37. 2-cl1l0ro propene sulfonic acid 0.1-1. 5 38. Cinnamyl sulionic acid; 0. 1-3. 0 39. 3-Phenyl-2-propyne-1-sulf0nic acid. 0.3-3.0 40. 4-Methoxy-2-butyne-1-sult0nic acid 0.2-2
The combination of the compounds of Table I with those of Table II can be used in all types of acidic nickel baths that give good ductile gray nickel deposits without the additives, such as Watts nickel baths, high chloride,
fluoborate, and sulfamate baths and mixtures of these various nickel salts. Sodium, potassium, and lithium ions may be present, also ammonium ions, though the latter should preferably be kept below about 7 grams per liter for maximum ductility and brightness. Boric acid is the preferred buffer.
The best pH range is from about 2.8 to 4.5, though pH values of 2 to 6 may be used. The temperature of' 3 the bath may be from room to 190 F., though in general 120 F.l60 F. is preferred.
When no air agitation or strong mechanical or hydraulic agitation is used, it is preferred to use a suitable surface-active agent such as sodium lauryl sulfate, sodium Z-ethyl hexyl sulfate or sulfonate, octyl sulfonic acid, etc., to prevent gas-pitting. With air agitation, it is usually not necessary to use a surface-active agent but if desired, sodium 2-ethyl sulfate can be used which does not foam excessively, or otherwise a more powerful surface-active agent such as sodium lauryl sulfate can be used in conjunction with an anti-foam such as a silicone oil or a tallow alcohol.
The compounds of Table II can be used in amounts between about 0.1 gram/liter and saturation and the preferred organic sultan-compounds to be used with the compounds of Table I are the benzene sulfonamides and sulfonimides (0.1 gram/liter to saturation) especially when used in conjunction with allyl sulfonic acid (0.6-2 grams/liter) or Z-butyne disulfonic acid (3-10 grams/ liter). The preferred compound of Table I is Example 2, which is 3,9-divinyl spirobi (m-dioxane), in a concentration of 0.01 to 0.05 gram/liter.
The baths containing compounds of Table I and Table II are not very sensitive to giving poor adhesion due to broken electrical contacts or to small excesses of these compounds, and therefore these compounds do not readily cause double or laminated plates. For these reasons, the compounds of Table I in conjunction with those of Table II give excellent results in bulk, tumble or barrel plating, as well as in the rack plating of steel, zinc diecast, aluminum and brass articles. Especially superior results (brightness and ductility) are obtained with rapid agitation (air agitation or hydraulic agitation).
In the following examples typical bath compositions and conditions are illustrated for obtaining the bright nickel deposits in accordance with this invention, but it is to be understood that they are representative only, and that the compounds of Table I can be used in such bath compositions with each compound or combinations of the compounds of Table II or other organic sulfoncompounds similar to those of Table II such as those carrying di-, tri-, or tetra-sulfonimide groups of phenyl, biphenyl, naphthyl, or mixed phenyl, biphenyl etc., di-, tri-, and tetra-sulfonimides, such as in the approximate proportions indicated in Table II. Furthermore, the conjunctive use of the compounds of Table I with the compounds of Table II does not greatly reduce the excellent properties which are characteristic of all of the organic sulfon-compounds of Table II with respect to the low sensitivity of nickel baths containing the latter organic sulfon-compounds to poor adhesion from broken electrical contacts or delayed electrical contacts or from reverse or anodic currents as in periodic current reversals, or in anodic activation of the nickel plate for re-plate. Delays of as long as one minute before electrical contact is made, or anodic currents for as long as one minute in many cases, do not cause poor adhesion. Zinc ions or cadmium ions can be present in most of the nickel baths, especially in high chloride baths, in concentrations of at least 0.05 to 0.1 gram per liter and also not aifect the adhesion during delayed electrical contacts or periodic current reversals. As a matter of fact, the zinc or cadmium present in the nickel plate causes a more shallow type of corrosion pit to occur in the nickel when chromium plated and exposed to a corrosive atmosphere (for example the atmosphere in industrial areas). The relative insensitivity of such baths to passivity from anodic current, makes possible the use of periodic current reversal in its sacrificial form which tends to promote leveling and to improve the corrosion protection afiorded to the underlying metal. For
example, after the initial deposition of a thin nickel plate (0.1 to 0.2 mil), a sacrificial periodic current reversal cycle of ten or more seconds anodic current preferably at low anodic current (5 to 10 amps/sq. ft.) with about 1 to 5 seconds cathodic current can be used for periods of about 1 to 2 or more minutes and then the procedure repeated until the desired thickness of plate is obtained. The benzene sulfonamides and sulfonimides and o-benzoyl sulfimide together with small concentrations of the compounds of Table I represent preferred combinations of the compounds of this invention for the periodic current reversal treatments.
Example I NiSO .6H O "grams/liter" 200-300 NiCl .6H O do 30-80 H3803 d0 N-aBF do 0-0.S Example 2 of Table I (3,9-divinyl spirobi (m-dioxane) grams/liter 0.01-0.04 Sodium allyl sulfonate do 0.6-2 Benbene sulfonamide do 1-2 o-Benzoyl sulfimide do 0-2 Temperature F 120-160 pH 3.2-4.8
Example II NiCl .6H- O grarns/liter -200 -d0 H 30 do 30-50 Example 2 of Table I (3,9-divinyl spirobi (m-dioxane) grams/liter- 0.01-0.04 Sodium allyl sulfonate do 0.6-2 o-Benzoyl sulfimide do 1-2 Benzene sulfonamide do 1-2 Temperature F -160 pH 3.2-4.8
Example III NiSO .6H O grams/liter 200-300 NiC1 .6H O do 30-100 H3B03 ..d0 Example I of Table I (vinyl-m-dioxane) grams/liter 0.01-0.05 o-Benzoyl sulfimide do 0.1-2 Temperature F 120-160 pH 3.2-4.8
Example IV NiS0 .6H O grams/liter 200-300 NiCl .6H O do 30-80 H BO do 30-50 NaBF o 0-0.5 Example 2 of Table I (3,9-divinyl spirobi (m-dioxane) grams/1iter 0.01-0.04 2-Butyne 1,4-disulfonic acid Na, K, or Ni salt) grams/liter- 3-10 Benzene sultonamide do 1-2 o-Benzoyl sulfimide do 0-2 Temperature F 120-160 pH 3.2-4.8
The above baths gave brilliant ductile nickel deposits that were remarkably adherent even when electrical contact was not instantly made. Exceptionally good results Were obtained with air agitation, especially in baths of Examples I, II and IV.
What is claimed is:
1. A bath for electrodepositing bright, ductile nickel plate which comprises an aqueous acidic solution containing at least one electrolyte selected from the group consisting of nickel sulfate, nickel chloride, nickel fluoborate and nickel sulfamate, and having dissolved therein about 0.1 gram/ liter to saturation of at least one organic sulfon- .compound selected from the class consisting of benzene, biphenyl and naphthalene sulfonic acids, sulfonamides and sulfonimides and the mixed phenyl, biphenyl and naphthyl sulfonamides and the mono-, di-, tri-, and tetrasulfonimides thereof, and dibenzene sulfonimides and the halogen, methyl, and aldehydo derivatives of said sulfonic acids, sulfonamides and sulfonimides, and beta unsaturated alkene and alkyne sulfonic acids having 4-2 carbon atoms, and about 0.002 to about 0.5 gram/ liter of a compound selected from the group consisting of vinyl substituted m-dioxane, and di-vinyl substituted bi(m-dioxane), and derivatives thereof, in which derivatives the m-dioxane ring is substituted with a radical selected from the group consisting of chloro, bromo, hydroxy, methoxy, ethoxy and hydroxy-ethoxy radicals.
2. A bath in accordance with claim 1 wherein said vinyl substituted m-dioxane compound is 3,9-divinyl spirobi (m-dioxane) and is present in a concentration in the bath of 0.005 to about 0.2 gram/liter.
3. A bath in accordance with claim 1 wherein the vinyl substituted m-dioxane is 3-viny1' m-dioxane and is dissolved in the said nickel bath in a concentration of 0.005 to about 0.2 gram/ liter.
4. A bath in accordance with claim 1 wherein said organic sulfon-compound is allyl sulfonate.
5. A bath in accordance with claim 1 wherein said organic sulfon-compound is 2-butyne-1,4-disulfonate.
6. A method of electrodepositing bright, ductile nickel plate which comprises electrolyzing an aqueous acidic solution comprising at least one nickel salt selected from the group consisting of nickel sulfate, nickel .chloride, nickel fluoborate and nickel sulfamate, said bath containing dissolved therein about 0.1 gram/liter to saturation of at least one organic sulfon-compound selected from the group consisting of benzene, biphenyl and naphthalene sulfonic acids, sulfonamides and sulfonim-ides and the mixed phenyl, biphenyl and naphthyl sulfonamides and the mono-, di-, tri-, and tetrasulfonimides thereof, and dibenzene sulfonimides and the halogen, methyl, and aldehydo derivatives of said sulfonic acids, sulfonamides and sulfonimides, and beta unsaturated alkene and alkyne sulfonic acids having 4-2 carbon atoms, and about 0.002 to about 0.5 gram/ liter of a compound selected from the group consisting of vinyl substituted m-dioxane, and divinyl substituted bi(m-dioxane), and derivatives thereof, in which derivatives the m-dioxane ring is substituted with a radical selected from the group consisting of chloro, bromo, hydroxy, methoxy, ethoxy and hydroxy-ethoxy radicals.
7. A method in accordance with claim 6 wherein said vinyl Substituted m-dioxane compound is 3,9-divinyl spirobi (m-dioxane) and is present in a concentration in the bath of 0.005 to about 0.2 gram/liter.
8. A method in accordance with claim 6 wherein the vinyl substituted m-dioxane is 3-vinyl m-dioxane and is dissolved in the said nickel bath in a concentration of 0.005 to about 0.2 gram/liter.
9. A method in accordance with claim 6 wherein said organic sulfon-compound is allyl sulfonate.
10. A method in accordance with claim 6 wherein said organic sulfon-compound is Z-butyne-l,4-disulfonate.
No references cited.

Claims (1)

1. A BATH FOR ELECTRODEPOSITING BRIGHT, DUCTILE NICKEL PLATE WHICH COMPRISES AN AQUEOUS ACIDIC SOLUTION CONTAINING AT LEAST ONE ELECTROCLYTE SELECTED FROM THE GROUP CONSISTING OF NICKEL SULFATE, NICKEL CHLORIDE, NICKEL FLUOBORATE AND NICKEL SULFAMATE, AND HAVING DISSOLVED THEREIN ABOUT 0.1 GRAM/LITER TO SATURATION OF AT LEAST ONE ORGANIC SULFONCOMPOUND SELECTED FROM THE CLASS CONSISTING OF BENZENE, BIPHENYL AND NAPHTHALENE SULFONIC ACIDS, SULFONOMIDES AND SULFONIMIDES AND THE MIXED PHENYL, BIPHENYL AND NAPHTHYL SULFONIMIDES AND THE MONO-, DI-, TRI, AND TETRASULFONIMIDES THEREOF, AND DIBENZENE SULFONIMIDES AND THE HALOGEN, MEYTHYL, AND ALDEHYDO DERIVATIVES OF SAID SULFONIC ACIDS, SULFONAMIDES AND SULFONIMIDES, AND BETA UNSATURATED ALKENE AND ALKYNE SULFONIC ACIDS HAVING 4-2 CARBON ATOMS, AND ABOUT 0.002 TO ABOUT 0.5 GRAM/ITER OF A COMPOUND SELECTED FROM THE GROUP CONSISTING OF VINYL SUBSTITUTED M-DIOXANE, AND D-VINYL SUBSTITUTED BI(M-DIOXANE), AND DERIVATIVES THEREOF, IN WHICH DERIVATIVES THE M-DIOXANE RING IS SUBSTITUTED WITH A RADICAL SELECTED FROM THE GROUP CONSISTING OF CHLORO, BROMO, HYDROXY, METHOXY, ETHOXY AND HYDROXY-ETHOXY RADICALS.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2986500A (en) * 1959-04-21 1961-05-30 Metal & Thermit Corp Electrodeposition of bright nickel
US3075898A (en) * 1961-05-29 1963-01-29 Udylite Res Corp Electrodeposition of nickel
US3305462A (en) * 1965-09-02 1967-02-21 Barnet D Ostrow Acid nickel electroplating bath
US4764262A (en) * 1979-09-13 1988-08-16 M&T Chemicals Inc. High quality, bright nickel plating
US6045682A (en) * 1998-03-24 2000-04-04 Enthone-Omi, Inc. Ductility agents for nickel-tungsten alloys

Non-Patent Citations (1)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2986500A (en) * 1959-04-21 1961-05-30 Metal & Thermit Corp Electrodeposition of bright nickel
US3075898A (en) * 1961-05-29 1963-01-29 Udylite Res Corp Electrodeposition of nickel
US3305462A (en) * 1965-09-02 1967-02-21 Barnet D Ostrow Acid nickel electroplating bath
US4764262A (en) * 1979-09-13 1988-08-16 M&T Chemicals Inc. High quality, bright nickel plating
US6045682A (en) * 1998-03-24 2000-04-04 Enthone-Omi, Inc. Ductility agents for nickel-tungsten alloys

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