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
• • 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
  • C25D3/38—Electroplating: Baths therefor from solutions of copper

Definitions

• This invention relates to a process for producing metal Patent F 2,986,498 Patented May .30, 1961 4 if tached either on the X or R groups, and may be provided,
• N-ethyl-N-fi-aminoethyl-aminoethane-sulfonic acid electrodeposits and more particularly to additives for electroplating baths which are capable of eliminating the adverse efiects of impurities in such baths upon the quality of the metal deposits produced by means of such baths.
• Impurities which adversely affect the qualities of metal electrodeposits include those which cause the 1 hardness of tap water as well as those contained in technically pure metal salts usually employed to make up the electroplating solution. The adverse effect of these impurities is particularly noticeable in electroplating processes for depositiing copper on metal objects, and
• drocarbon radicals may also have substituen'ts 'containiug Oxygen, sulfur or nitrogen atoms.
• electrodeposits produced thereby are bright and lustrous despite the fact that the bath contains impurities of the type described above, such as impurities which cause hardness, etc. Such bright deposits are ob tained over the entire effective range of current densities.
• these additives have the further advantage that they increase the ductility of the electrodeposits.
• the above-mentioned additives are entrained with the metal electroplates to a substantially lesser degree than the corresponding compounds vof the principal patent, which results in a much more economical consumption.
• the amounts in which the additives in accordance with our invention can be added to produce the desired eifect range from about-0.01 gn1./liter of bath to about 15 gm./ liter of bath, but the preferred amount is from 3 to 12 gnu/liter of bath.
• the precise amounts required vary from one additive to the other and are also dependent upon the type of brightening agent employed and the amount and kind of inorganic impurities present in the bath.
• objects can be electroplated in such baths at temperatures ranging from 20 C. to 60 C., and
• the use of the additives in accordance with our invention does not require any change in the composition of the electroplating baths commonly use, nor does it require any change in the conditions under which objects are usually electroplated, particularly with respect to the temperature of the plating bath and the current densities usually employed.
• the additives we use are soluble in the usual acid metal salt baths, and particularly in copper-plating baths containing the usual copper salts in an acid aqueous solution. The additives are not decomposed during the electroplating-process.
• additives for electroplating baths in accordance with our invention can be used in conjunction with any electroplating bath containing a brightening agent and in which the quality of the metal electrodeposits produced therefrom are adversely afiected by impurities of the type described, such as, for example, in zinc-, chromiurn-, precious metal-, and particularly copperplating baths which contain brightening agents, and in particular sulfonic acid brightening agents.
• Brightening agents usable for the process according to the above noted invention are listed in the following table:
• Example 11 When 1.5 gm./liter N,N,N,N' tetra n butyl 1,3- diaminopropanol-2-mono-sulfonic acid ester are added to an acid copper-plating bath containing 250 gm./liter technical-grade copper sulfate, 70 gm./liter concentrated sulfuric acid and 0.3 gm./liter N,N-diethyl-dithiocarbamic acid-ethylester-w-sodium sulfonate, as brightening agent, electroplating of sheet iron preplated in a cyanide bath is provided with a full bright copper electroplate. The best copper electroplates are obtained when the electroplating step is carried out at C.
• Example 111 sodium sulfonate, as brightening agents, and 1 gm./liter,
• ZQS-diarnino-benzene-1,4-disulfonic acid At temperatures between 20 and 45 C., objects may be electroplated at current densities up to 13 amp./dm. Without the addition of 2,5-diaminobenzene-1,4-disulfonic acid the copper electroplates are much less bright.
• Examples 1 V-XX V1 In the table some compositions for copper plating baths are listed.
• the copper baths contain 100-240 gmJliter CuSO .5H O, 20-120 gm./liter concentrated sulfuric acid and the following amounts of brightening agents according to the above noted list and the following amounts of sulfonic acid or sulfuric acid ester derivatives respectively of the diamino compounds free from carboxyl groups according to the above noted list:
• a process of producing bright metal electrodeposits said metal being selected from the group consisting of copper, Zinc, chromium and precious metals, from electroplating baths containing impurities found in hard water and in technical grade metal salts; and containing a brightening agent, the step which comprises adding to such electroplating baths 0.01 to -15 gm./liter of an amino compound free from carboxyl groups having the general structural formula wherein X is an organic radical selected from the group consisting of bivalent acyclic'hydrocarbon radicals, bivalent cyclic hydrocarbon radicals, and heterocyclic hydrocarbon radicals which include at least one of the nitrogen atoms, and R R R R and R are selected from the group consisting of hydrogen, substituted hydrocarbon radicals and unsubstituted hydrocarbon radicals, wherein at least one of the radicals selected from the group consisting of R R R R and X is substituted with a sulfonic acid group, X being free of said substituent when said substituent is on one of said radical
• step 4 which comprises adding to such electroplating baths 0.01 to 15 gm./liter of piperazine-N,N-bis-(Z-hydroxypropane-sulfonic acid) whereby said impurities are prevented from interfering with the production of bright copper electrodeposits.
• step 5 which comprises adding to such electroplating baths 0.01 to 15 gm./liter of piperazine-N,N-bis(2-hydroxypropane-sulfonic acid), whereby said impurities are prevented from interfering with the production of bright copper electrodeposits.
• step 6 which comprises adding to such electroplating baths 0.01 to 15 gut/liter of N,N,N'N'-tetra-n-butyl-1,3-diaminopropanol- 8 Z-mOno-suifuricacid ester, whereby said impurities are prevented from interfering with the production of bright copper electrodeposits.
• step 7 which comprises adding 0.01 to 15 gm.-/liter of N, N,N"N'- tetra-n-b'utyl-1,3-diaminopropanol-2-monosulfuric acid ester to such electroplating baths, whereby said impurities are prevented from interfering with the production .of bright copper electrodeposits.
• an acid copper electroplating bath comprising technical grade copper salts and hard tap water
• the improvement which comprises a component for rendering impurities in said bath harmless, comprising 0.01 to 15 gm./liter of an organic amino compound free from carboxyl groups having the general structural formula wherein X is an organic radical selectedfrom the group consisting of bivalent acyclic hydrocarbon radicais, bivalent cyclic hydrocarbon radicals and heterocyclic hydrocarbon radicals which include at least one of the nitrogen atoms, and R R R and R are radicals selected from the group consisting of hydrogen, substituted hydrocarbon radicals and unsubstituted hydrocarbon radicals, wherein at least one of the radicals selected from the group consisting of R R R R and X is substituted with a substituent selected from the group consisting of sulfonic and sulfuric acid ester groups, X being free of said substituent when said substituent is on one of said radicals selected from the group consisting of R R R and R whereby said impurities are prevented from interfering with the

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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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• 0
  • BE BE563647D patent/BE563647A/xx unknown
  • BE BE534101D patent/BE534101A/xx unknown
• 1954
  • 1954-12-28 CH CH340395D patent/CH340395A/de unknown
• 1955
  • 1955-01-20 FR FR1118019D patent/FR1118019A/fr not_active Expired
  • 1955-03-11 GB GB7161/55A patent/GB807574A/en not_active Expired
• 1957
  • 1957-02-13 DE DED24913A patent/DE1030133B/de active Pending
• 1958
  • 1958-01-07 CH CH5441958A patent/CH370612A/de unknown
  • 1958-02-12 US US714687A patent/US2986498A/en not_active Expired - Lifetime
  • 1958-02-12 GB GB4550/58A patent/GB884035A/en not_active Expired
  • 1958-05-15 US US735360A patent/US3030283A/en not_active Expired - Lifetime

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