US3661783A - Composition for metal plating of plastics - Google Patents
Composition for metal plating of plastics Download PDFInfo
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- US3661783A US3661783A US6947A US3661783DA US3661783A US 3661783 A US3661783 A US 3661783A US 6947 A US6947 A US 6947A US 3661783D A US3661783D A US 3661783DA US 3661783 A US3661783 A US 3661783A
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- Prior art keywords
- solution
- borane
- plating
- bath
- plastic
- 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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- 238000007747 plating Methods 0.000 title abstract description 32
- 239000004033 plastic Substances 0.000 title abstract description 21
- 229920003023 plastic Polymers 0.000 title abstract description 21
- 229910052751 metal Inorganic materials 0.000 title description 9
- 239000002184 metal Substances 0.000 title description 9
- 239000000203 mixture Substances 0.000 title description 6
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 abstract description 28
- 229910000085 borane Inorganic materials 0.000 abstract description 21
- 239000000126 substance Substances 0.000 abstract description 15
- 150000003839 salts Chemical class 0.000 abstract description 12
- 239000002253 acid Substances 0.000 abstract description 11
- 238000011282 treatment Methods 0.000 abstract description 10
- 150000001412 amines Chemical class 0.000 abstract description 9
- JBANFLSTOJPTFW-UHFFFAOYSA-N azane;boron Chemical compound [B].N JBANFLSTOJPTFW-UHFFFAOYSA-N 0.000 abstract description 9
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 26
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 15
- 239000012190 activator Substances 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 229910052759 nickel Inorganic materials 0.000 description 8
- 229910000510 noble metal Inorganic materials 0.000 description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 7
- -1 amine boranes Chemical class 0.000 description 6
- 238000007772 electroless plating Methods 0.000 description 6
- 229910021645 metal ion Inorganic materials 0.000 description 6
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 6
- 239000003638 chemical reducing agent Substances 0.000 description 5
- 101150003085 Pdcl gene Proteins 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000001464 adherent effect Effects 0.000 description 3
- RJTANRZEWTUVMA-UHFFFAOYSA-N boron;n-methylmethanamine Chemical group [B].CNC RJTANRZEWTUVMA-UHFFFAOYSA-N 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 2
- LRZSAGKIMYFLHY-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;dihydrate Chemical compound O.O.OC(=O)CC(O)(C(O)=O)CC(O)=O LRZSAGKIMYFLHY-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 241001602742 Gegenes niso Species 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 150000003141 primary amines Chemical class 0.000 description 2
- PXIHYUSUNVOWGQ-UHFFFAOYSA-N B.CCCCN(CCCC)CCCC Chemical compound B.CCCCN(CCCC)CCCC PXIHYUSUNVOWGQ-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical class OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- QFLVHLKRNQNMGT-UHFFFAOYSA-N boron;methanamine Chemical compound [B].NC QFLVHLKRNQNMGT-UHFFFAOYSA-N 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 150000001860 citric acid derivatives Chemical class 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 229940083124 ganglion-blocking antiadrenergic secondary and tertiary amines Drugs 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012442 inert solvent Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000003893 lactate salts Chemical class 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical class O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000001119 stannous chloride Substances 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/22—Roughening, e.g. by etching
- C23C18/24—Roughening, e.g. by etching using acid aqueous solutions
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
Abstract
PLASTIC SURFACES ARE PREPARED TO MAKE THEM SUSCEPTIBLE TO BEING PLATED BY CHEMICAL PLATING SOLUTIONS BY TREATMENT WITH A SOLUTION OF A NOBLE METAL SALT, FOR EXAMPLE, PALLADIUM CHLORIDE, IN AN ACID ETCHANT FOR THE PLASTIC, FOLLOWED BY TREATMENT WITH A SOLUTION CONTAINING AMINE BORANES OR AMMONIA BORANE. THE BORANE SOLUTION MAY BE A CHEMICAL PLATING SOLUTION, IN WHICH CASE, THE SECOND STEP OF THE SURFACE PREPARATION AND THE PLATING OCCURS SIMULTANEOUSLY.
Description
United States Patent Office 3,661,783 Patented May 9, 1972 U.S. Cl. 252-792 3 Claims ABSTRACT OF THE DISCLOSURE Plastic surfaces are prepared to make them susceptible to being plated by chemical plating solutions by treatment with a solution of a noble metal salt, for example, palladium chloride, in an acid etchant for the plastic, followed by treatment with a solution containing amine boranes or ammonia borane. The borane solution may be a chemical plating solution, in which case, the second step of the surface preparation and the plating occurs simultaneously.
I This application is a division of my application Ser. No.
643,053, filed June 2 1967, now U.S. Pat. No. 3,507,681.
This invention relates to the electroless plating of metals on plastics and more particularly to such plating in which the plastic surfacev to be plated is pretreated to make it susceptible to being plated by a chemical plating bath.
The conventional method of forming a metal plate on plastics by electroless or chemical plating, which plate can then be a base for further electroless plating or for electroplating, utilizes, after cleaning to remove soil and grease, a series of sequential surface conditioning treatments: (1) the surface is etched by dipping in an etchant for the particular plastic to roughen or modify the plastic surface to make it receptive to subsequent treatment, (2) the etched surface is sensitized by dipping in an acid solution of stannous chloride, (3) the sensitized surface is activated by dipping in an acid solution of a noble metal chloride, such as palladium chloride. The thus pretreated plastic is then dipped in a chemical plating bath containing metal ions and a reducing material such as hypophosphites or amine boranes. It is conventional to water rinse the surface between each treatment step.
aqueous solution of amine boranes or ammonia borane, in
which case the plastic surface is activated so that it is susceptible to plating with any chemical plating bath. In the now' preferred embodiment the boraue solution is itself an electroless chemical plating bath containing metal ions as well as the borane, in which case, the plastic is directly i plated with the metal corersponding to the metal ion or ions in the bath.
The etchactivator bath of this invention is a solution of a noble metal salt, particularly chlorides such as gold chloride, platinum chloride, or preferably palladium chloride in an etchant for the particular plastic to be treated The etch-activator solution should contain at least about 0.001 weight percent noble metal salt and preferably to obtain high plating rates between about 0.005 and 0.010 weight'percent. The bath may contain higher amounts of noble metal salts, but is generally undesirable because no substantial benefit is realized and the salts are quiteexpensiye. The etchant used, is of course, selected to be effective with the particular plastic to be used and any acid etchant in which the noble metal salts are soluble is satisfactory for use in the etch-activator solutions. Generally, acid etchants are mixtures of oxidizing acid, such as chro mic acid and sulfuric acid mixtures formed by dissolving chromic oxide or alkali metal chromates in sulfuric acid. Phosphoric acids are also commonly used as etchants in admixture with chromic acid and sulfuric acid. The echants may also contain adidtives such as, for example. wetting agents. In addition, there are a number of acid proprietary etchants which may also be used in making the pretreatment bath of this invention, provided, of course, that the noble metal salt can be dissolved therein. Any plastic that is etched by acid etchants, such as ABS (acrylonitrile-butadieneastyrene copolymers) and polystyrene, and acetates and polyolefins that are etchable with acid etchants after pretreatment with organic solvents.
The conditions of treatment with the etch-activator solution such as temperature and time of contact, may be varied widely depending on the particular etchant and plastic used. Conditions at which the etchant alone will satisfactorily etch the plastic are suitable conditions for use of the etch-activator bath. Generally, a slightly elevated temperature, between about 40 and C., and a contact time of about 1 to 10 minutes are used.
Following treatment with the etch-activator, the plastic surface is contacted with a solution containing an amine boraue or ammonia borane. This may suitably be essentially a solution of the boraue in an inert solvent, suitably water, preferably containing between about 0.01 and 1 moles/liter of amine borane or ammonia borane. Higher concentrations of boranes may be used if desirable without detriment or benefit. The amine borane may be any of the wide variety of amine boranes used in electroless plating baths, such as boranes of primary, secondary and tertiary amines. In such instances the surface is activated so that any metal or alloy electroless plating solution will form an adherent plate on the surface by conventional methods, regardless of the reductant used in the plating baths. For example, nickel plates may be laid down from conventional hypophosphitenickel plating solutions and copper from conventional formaldehydecopper plating solutions.
Preferably the boraue-containing solution is 'itself an electroless plating bath. Bol'ane chemical plating baths contain an amine boraue or ammonia borane and a soluble metal salt, such as nickel, cobalt, iron or zinc salts, and, if desired, additional solubilizing agents, chelating agents, stabilizers, buffering materials or other additives. A large number of such plating baths are well known, such as those disclosed by Hoke in U.S. Pat. 2,990,296, by Zirngiebl and Klein in U.S. Pats. 3,140,188 and 3,234,031, by McLeod in U.S. Pat. 3,062,666, and by E. I. du Pont de Nemours and Comany in British Pat. 842,826. Any of the electroless plating baths with an amine borane reductant, such as boranes of primary, secondary or tertiary amines, as well as ammonia borane, may be used in the practice of this invention. The preferred reductant is dimethylamine borane, as baths having this reductant give complete coverage of the surface at a somewhat faster rate than those containing only other amine boranes. Generally, the concentration of amine borane in such plating baths is between about 0.01 mol and 0.1 mol per liter, the concentration of metal ion is between about 0.02 mol and 0.3 mol per liter, and the pH is maintained above about 3.5. When borane plating solutions are so used an adherent continuous metal plate, corresponding to the metal ion in the solution, is
the plating bath is ordinarilyuseable.
The borane solution may' be a plating solution having primarily another chemical reductant and only. a small catalytioamountiofamine borane or ammonia borane.
For example, avnickel plate is formed when a plastic surface pretreated withetch-activatoris contacted with a conventionalhypophosphite-nickel 7 (bath containing as little as 0.001 mol/liter of amine borane or ammonia borane. I It should be recognized that the metal plates may be single metals or alloys, depending on the plating bath and conditions used, and frequently will contain minor amounts of boron or phosphorous. This invention is applicable for use with any of the well-known chemical plating baths and such bath compositions or plates produced therefrom constitute no part of my discovery.
The following examples are illustrative of this invention.
EXAMPLE I A placque of ABS plastic Cycolac EP-3510 (Marbon Chemical Company) was cleaned by a dip in an alkaline cleaning solution to remove extraneous dirt and grease. The placque was then immersed for two minutes at 50 C. in an etch-activator bath containing 100 g. Cr O 50 ml. of concentrated H 80 0.0221 g. of PdCl and sufiicient water to bring the solution volume to 400 ml. The placque was then rinsed with water and immersed for 2 minutes at 50 C. in a chemical plating bath having the following composition: NiS'O '6H O, 0.13 mol/liter; C H -H O, 0.07 mol/liter, (CH NBH 0.04 mol/ liter; and NH OH to pH 7.0-7.5. At the end of the treatment, the placque was covered with a continuous adherent, bright nickel plate.
EXAMPLE II Example I was repeated, except the etch-activator was (a) diluted to /2 the original concentration, (b) 25 ml. of concentrated H 80 was added to the etch-activator, and (c) 250 ml. of 72 wt. percent H 80 was added to the etch-activator, with substantially the same results.
EXAMPLE III A clear placque of Cycolac EP-35 10 was immersed for 4 minutes at 60 C. in an etch-activator bath containing 30 g. of Kzcl'goq, 200 ml. of concentrated H 80 0.1096 g. 'PdCl and 200 ml. of water. After rinsing with water, the placque was plated with nickel as in Example 1.
EXAMPLE IV Example I was repeated with the same results, except that the etch-activator contained 0.0067 g. of PdCl EXAMPLE V Example HI was repeated using etch-activator solution to which 10, 20, 30 and 40 ml., respectively, of 85% H PO was added. The plating rate was slightly faster than Example 1V in the first three'runs and somewhat slower in the fourth run.
EXAMPLE VI A placque of Cyclolac-EP-35'10 was immersed for two minutes at 60 C. inan etch-activator bath containing 200 ml. concentrated H 80 25 ml. concentrated HCl, 0.1255
then each was nickel plated with various amine borane.
chemical plating baths. A number of placques were satissformedontheplastic surface under..the conditions which factorilyplated. with baths. containing dimethylamine borane and nickel sulfate, the concentration of dimethylamine borane ranging from 2.0 g./l. to 3.5 g./l., the pH ranging from 5.0 to 9.0, and with various nickel complexing agents, including'citrates, lact-ates, glycolates and ammonia,1iat temperatures between "about 30fl C. and 65 C. p
A pretreated placque was satisfactorilyrplated- 1at-=-50 C. with a bathcontaining 7.5 g. of NiSO4-6H O, 5 g. of citric acid dihydrate, 0.3 g; Nl-l B-Hgfwaterto"'25 0 ml: total volume, and NH OH to a"pH of"6.5. I v
Another pretreated placque was sa" factorily plated at 65 C. with a bath containing 15 g. NiSO;-6H O', 10 g. of citric acid dihydrate, 5 g. tributylamine borane, water to 400 ml. total volume, and NH OH to a pH of EXAMPLE VIII To illustrate the unsuitability of plating baths containing only hypophosphite reductan-ts, a, placque pre treated as in Example IV was immersed at 65 C. in a hypophosphite bath containing 8.1 g. NiSO -6H O, 12.8 g. of lactic acid, 4.0 g. succinic acid, 9.6; g. NaH PO water to 400 ml. total volume, and NaOH to a pH of 5.5. Therewas negligiblenickel deposition, even when placques had been immersed as-long as 60 minutes in the etch-activator bath and in the hypophos phite plating bath. The hypophosphite bath is a typical bath that produced good plates on plastics pr'etreated by the prior art procedures outlined hereinbefore. i EXAMPLE IX Example VIII was repeated except that 0.12 g. of di-, methylamine borane was added to the. hypophosphite. bath and a good nickelplate was produced with an immersion time of two minutes in the etch-activator;
5-10 minutes in the plating bath. I .7
EXAMPLE X A placque pretreated as in Example IV was imf mersed in a 1 wt. percent aqueous dimethyla minebor; ane solution and rinsed with water. A good nickel plate was formed when the placque was immersed in the hypo phosphite bath of Example VIII.
EXAMPLE XI I about 0.001 and 0.01 wt. percent of a noble metal salt in an etchant selected from the group co'nsistingof -mix-- tures of chromic and sulfuric acids andmixtures thereof withphosphoric acid'w' r 7 2. A bath according to claimnl in which the salt is palladium chloride.
3. A bath according-to claim. 2 containing between about 0.005 and 0.10 wt. percent salt.
References Cited s I, UNITED STATES; PATENTS 3,445,350 5/1969 Klinger a 'ai t 2 04536 JACOB H. SDEINBERG, Primary Examiner US. :1. X.R. e 101-1; 117-47 R; 148--6.14; 1562; 204--38'
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US64305367A | 1967-06-02 | 1967-06-02 | |
US694770A | 1970-01-29 | 1970-01-29 |
Publications (1)
Publication Number | Publication Date |
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US3661783A true US3661783A (en) | 1972-05-09 |
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ID=26676278
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US6947A Expired - Lifetime US3661783A (en) | 1967-06-02 | 1970-01-29 | Composition for metal plating of plastics |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4017265A (en) * | 1972-02-15 | 1977-04-12 | Taylor David W | Ferromagnetic memory layer, methods of making and adhering it to substrates, magnetic tapes, and other products |
US5160600A (en) * | 1990-03-05 | 1992-11-03 | Patel Gordhanbai N | Chromic acid free etching of polymers for electroless plating |
US20040132300A1 (en) * | 2002-12-18 | 2004-07-08 | Enthone Inc. | Procedure for activation of substrates for plastic galvanizing |
-
1970
- 1970-01-29 US US6947A patent/US3661783A/en not_active Expired - Lifetime
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4017265A (en) * | 1972-02-15 | 1977-04-12 | Taylor David W | Ferromagnetic memory layer, methods of making and adhering it to substrates, magnetic tapes, and other products |
US5160600A (en) * | 1990-03-05 | 1992-11-03 | Patel Gordhanbai N | Chromic acid free etching of polymers for electroless plating |
US20040132300A1 (en) * | 2002-12-18 | 2004-07-08 | Enthone Inc. | Procedure for activation of substrates for plastic galvanizing |
EP1441045A2 (en) | 2002-12-18 | 2004-07-28 | Enthone Inc. | Process for activating a plastic substrate to be electroplated |
EP1441045A3 (en) * | 2002-12-18 | 2006-01-04 | Enthone Inc. | Process for activating a plastic substrate to be electroplated |
CN1328412C (en) * | 2002-12-18 | 2007-07-25 | 恩通公司 | Method for activating substrate for plating on plastic |
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