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
  • C23C18/18—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

Definitions

• the invention relates to a gentle method for activating non-conductive or semiconductive substrate surfaces for chemogalvanic metal deposition.
• the object of the present invention was therefore to avoid these disadvantages as far as possible, i.e.
• Preferred complexing agents for dissolving the sparingly soluble silver compounds are nitrogen-containing compounds which, by the action of heat and / or acids, provide complexes which can be readily split.
• Aqueous ammonia is particularly preferred.
• Amines can also be used, but their boiling point should preferably be below 100.degree.
• other complexing agents can also be used, e.g. Cyanide ions or thiosulfate ions.
• Germination - as already mentioned - is preferably carried out from an aqueous solution.
• aqueous solution water-like compounds, e.g. aliphatic alcohols or blends of organic solvents with water or alcohols are used.
• wetting agents e.g. Mersolate to add Texapon.
• the wetting is carried out at temperatures between 0 ° C and 90 ° C. In special cases, the temperature can also be below or above. It is very particularly preferred to work at 15-40 ° C.
• Another variant of the method is that the poorly soluble silver salt is precipitated on the moistened surface by a chemical reaction.
• An example is the acidification of a silver amine chloride solution with mineral acid, which leads to the precipitation of silver chloride. In these cases, removal of the complexing agent is no longer necessary.
• the surfaces germinated according to one of the process variants described must then be activated by reduction.
• the reducing agents customary in electroplating such as hydrazine hydrate, formaldehyde, hypophosphite, boranes or borohydrides, can preferably be used.
• the reduction is preferably carried out in aqueous solution.
• solvents such as alcohols, ethers, hydrocarbons can also be used.
• Suitable substrates for the process according to the invention are: glass, quartz, ceramic, carbon, paper, polyethylene, polypropylene, ABS plastics, epoxy resins, polyesters, polycarbonates, polyamides, polyethylene fluoride and textile fabrics, threads and fibers made of polyamide. Polyester, polyalkylene, polyacrylonitrile, polyvinyl halide, cotton and wool as well as their blends or copolymers, graphite fibers, flock and whiskers made of aluminum oxide etc. Textile materials are preferred.
• the surfaces activated according to the invention can be used directly for electroless metallization.
• a very particularly preferred embodiment of the method according to the invention consists in that the reduction in the metallization bath is carried out immediately with the reducing agent of the electroless metallization.
• This variant only consists of three work steps, for example: immersing the substrate in the solution of the silver compound, drying the substrate surfaces and immersing the surfaces activated in this way in the metallization bath.
• This embodiment is particularly suitable for nickel baths containing amine borane or copper baths containing formalin.
• Metallization baths which can be used in the process according to the invention are preferably baths with nickel salts, cobalt salts, copper salts or their mixtures with iron salts, gold and silver salts. Such metallization baths are known in the electroless metallization art.
• the silver salts according to the invention only detach from the germinated substrate surfaces to such an extent that the surfaces are metallized without the metallization baths being destroyed by noble metal nuclei.
• a 15 cm x 15 cm square of a cotton fabric (satin) is immersed in a solution of 0.7 g of silver chloride in one liter of aqueous ammonia for 10 seconds, then dried at 90 ° C. and then in an alkaline nickel-plating bath containing 30 g / 1 contains nickel chloride, 10 g / l dimethylamine borane and 10 g / l citric acid and was adjusted to pH 8 with ammonia, nickel-plated.
• a shiny metallic piece of fabric with a metal coating of 44 g nickel / m 2 is obtained .
• the electrical resistance of a 10 cm x 10 cm square area is 2 ohms in the warp direction and 3 ohms in the weft direction.
• a 15 cm x 15 cm square of a polyamide fabric (polyamide-6) is immersed in a solution of 1.3 g of silver chloride in one liter of aqueous ammonia for 1 minute.
• the fabric is then dried at 80 ° C. and then nickel-plated for 30 minutes in an alkaline nickel-plating bath in accordance with Example 1.
• a shiny metallic piece of fabric with a metal coating of 37 g nickel / m 2 is obtained .
• the resistance measured on a 10 cm x 10 cm square area is 0.2 ohms in the warp direction and 0.4 ohms in the weft direction.
• a 15 cm x 15 cm square of carbon fabric (plain weave) is immersed for 1 minute in an activation solution containing 0.5 g silver chloride / l aqueous ammonia.
• the fabric is dried at 120 ° C. and then metallized in an alkaline nickel plating bath according to Example 1 for one hour.
• a shiny metallic fabric with a metal coating of 55 g nickel / m 2 is obtained .
• the resistance of a 10 cm x 10 cm square area is 0.2 ohms in the warp direction and 0.3 ohms in the weft direction.
• a 15 cm x 15 cm network of aromatic polyamide is immersed in an activation solution containing 7 g / 1 ammoniacal aqueous solution of silver chloride for 30 seconds.
• the fabric is then dried at 100 ° C.
• a shiny metallic mesh with a metal coating of 10 g / m 2 is obtained .
• the resistance of a square area of 10 cm x 10 cm is 16 ohms or 18 ohms.
• a knitted fabric made of a polyester fiber yarn (Nm 40) (100% polyethylene terephthalate) is used at room temperature rature immersed in an activation solution according to Example 4 for 1 minute.
• the knitted fabric is dried at 100 ° C. and then nickel-plated in an alkaline nickel-plating bath according to Example 1 for 45 minutes.
• a shiny metallic knitted fabric with a metal coating of 76 g nickel / m 2 is obtained .
• a glass plate of 20 cm x 8 cm is sprayed uniformly with an activation solution according to Example 4, dried and then metallized in an alkaline nickel plating bath according to Example 1 for 5 minutes. After 1 minute the surface turns dark and after 5 minutes a shiny metallic layer is observed. The glass pane washed and dried after metallization is covered with a reflective metal layer.
• a 30 cm x 8 cm polyester film is degreased with 20% sodium hydroxide solution at 70 ° C. (10 minutes) and then sprayed on one side with an activation solution containing 3.5 g of silver chloride / 1 ammoniacal water.
• the film is dried at 120 ° C. and then immersed in a solution of 1 g of sodium borohydride in one liter of water for 2 minutes.
• the film is then rinsed with water and then in an alkaline cobalt bath containing 35 g / 1 cobalt sulfate, 140 g / 1 potassium sodium tartate and 20 g / 1 sodium hypo contains phosphite, metallized at 70 ° C.
• a cobalt-coated film with a cobalt content of 8.3 g / m 2 is obtained on one side.
• a cotton fabric according to Example 1 is immersed for 30 seconds in an activation solution which contains 1.5 g of silver rhodanide / 1 aqueous ammonia. The sample is dried at 120 ° C. and then nickel-plated in an alkaline nickel bath according to Example 1 for 40 minutes. A shiny metallic piece of fabric with a nickel coating of 88 g / m 2 is obtained .
• a polyamide fabric according to Example 2 is immersed for 1 minute in a solution of 1 g of silver bromide in one liter of aqueous ammonia, then dried at 80 ° C. and then nickel-plated in an alkaline nickel bath according to Example 1 for 80 minutes. A shiny metallic piece of fabric with a nickel coating of 60 g / m 2 is obtained .
• the resistance of a 10 cm x 10 cm area is 0.1 ohm in the warp direction and 0.2 ohm in the weft direction.
• a piece of paper of 15 cm x 15 cm is immersed in an activation solution according to Example 1, dried according to Example 1 and then in a 2% aqueous dimethylamine borane solution reduced. After rinsing with water, the activated piece of paper is nickel-plated for 25 minutes at room temperature in an alkaline nickel plating bath containing 30 g / 1 nickel chloride, 20 g / 1 citric acid and 8 g / 1 sodium hypophosphite and adjusted to pH 9 with ammonia. A shiny metallic piece of paper with a metal coating of 41 g / m 2 is obtained . The resistance of a 10 cm x 10 cm square area is 2 ohms in both directions.
• a 15 cm x 15 cm square of a cotton fabric (satin) is immersed in a solution of 1.6 g of silver chloride in one liter of aqueous ammonia for 30 seconds. The piece of fabric is then immersed in a 3% hydrochloric acid solution for one minute, washed and then nickel-plated in an alkaline nickel-plating bath according to Example 1 for 15 minutes. A shiny metallic piece of fabric with a nickel coating of 48 g / m 2 is obtained .
• the electrical resistance of a 10 cm x 10 cm square area is 0.9 ohms in the chain direction and 1.3 ohms in the weft direction.
• ABS piece preheated with chromic acid is immersed in a solution of 3 g of silver chloride in one liter of aqueous ammonia, then dried at 80 ° C. and then in an alkaline nickel plating bath
• Example 1 Metallized for 10 minutes. After 30 seconds the surface begins to turn dark and after 10 minutes a well adhering, shiny metallic nickel layer had been deposited.
• a 15 cm x 15 cm piece of fabric made of polyamide 6 is immersed for one minute in an ammoniacal aqueous solution of 2.5 g of silver chloride / 1, then dried at 130 ° C. and then in an alkaline copper bath made of 10 g / 1 copper sulfate, 14 g / 1 Seignette salt and 20 ml / 1 35 wt .-% formaldehyde solution brought, which was adjusted to pH 12.5 to 13 with sodium hydroxide solution. After one minute, the surface of the fabric begins to discolor and after 20 minutes a shiny metallic, copper-colored fabric with 12 g / m 2 copper is obtained.
• the resistance of a 10 cm x 10 cm square area is 3.5 ohms in the warp direction and 5 ohms in the weft direction.

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• Chemical & Material Sciences (AREA)
• General Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Materials Engineering (AREA)
• Mechanical Engineering (AREA)
• Metallurgy (AREA)
• Organic Chemistry (AREA)
• Chemically Coating (AREA)
• Chemical Or Physical Treatment Of Fibers (AREA)

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• 1983
  • 1983-10-18 DE DE19833337856 patent/DE3337856A1/de not_active Withdrawn
• 1984
  • 1984-10-08 EP EP84112030A patent/EP0142691B1/fr not_active Expired
  • 1984-10-08 DE DE8484112030T patent/DE3474165D1/de not_active Expired
  • 1984-10-15 JP JP59214465A patent/JPS6096766A/ja active Pending
  • 1984-10-15 US US06/661,007 patent/US4568570A/en not_active Expired - Fee Related
  • 1984-10-16 CA CA000465497A patent/CA1232498A/fr not_active Expired

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