US3847649A - Process for depositing a metal layer upon a plastic - Google Patents

Process for depositing a metal layer upon a plastic Download PDF

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Publication number
US3847649A
US3847649A US33993573A US3847649A US 3847649 A US3847649 A US 3847649A US 33993573 A US33993573 A US 33993573A US 3847649 A US3847649 A US 3847649A
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United States
Prior art keywords
metal
process according
filler
plastic
metal salt
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Expired - Lifetime
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English (en)
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V Sova
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BBC Brown Boveri AG Switzerland
BBC Brown Boveri France SA
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BBC Brown Boveri France SA
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    • 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
    • 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
    • C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
    • C23C18/2046—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment
    • C23C18/2073—Multistep pretreatment
    • C23C18/208—Multistep pretreatment with use of metal first
    • 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
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
    • H05K2203/07—Treatments involving liquids, e.g. plating, rinsing
    • H05K2203/0756—Uses of liquids, e.g. rinsing, coating, dissolving
    • H05K2203/0773—Dissolving the filler without dissolving the matrix material; Dissolving the matrix material without dissolving the filler
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31511—Of epoxy ether
    • Y10T428/31529—Next to metal
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31678—Of metal
    • Y10T428/31681—Next to polyester, polyamide or polyimide [e.g., alkyd, glue, or nylon, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31678—Of metal
    • Y10T428/31688—Next to aldehyde or ketone condensation product
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31678—Of metal
    • Y10T428/31692—Next to addition polymer from unsaturated monomers

Definitions

  • ABSTRACT A metal layer is deposited onto a plastic body by admixing a soluble particulate filler and a metal which is reduceable to a catalytically active metal into a heat hardenable polymeric resin composition, applying heat to simultaneously harden the resin composition and to reduce the metal salt, removing at least one surface layer of the hardened polymeric composition to expose portions of the catalytically active metal particles and the soluble filler particles, which exposed filler particles are removed, and subjecting the treated surface to a metal plating bath for the electroless deposition of metal on the hardened polymeric surface by the catalytic activity of the metal particles.
  • the thickness of the metal layer which can be adherently formed in this manner is substantially limited. If the metal layerbecomes too thick, there is a tendency for local chipping and peeling of the layer from the substrate, and there is atendency for mechanical strains and bubbles to develop in the deposited metal. In general, the maximum thickness which was obtainable by that prior art method, with any degree of reliability, has been about 30 microns.
  • the particular polymeric resin composition which is treated in the present invention is not critical and any thermosetting or thermoplastic resin may be used.
  • the only limitation is that the resin must be sufficiently fluid in the unhardened condition to permit admixing of the metallic salt and particulate filler therewith.
  • the composition may contain a curing or hardening agent, or may be formed from a monomeric composition which is heat polymerizable into a hardened composition. Any of the widely used epoxy resin compositions, olefin resin compositions, carbonate resin compositions, acrylic resin compositions, formaldehyde resins, polyester resins, and the like may be used so long as they are heat hardenable.
  • the metal salt used herein is of the type which is catalytically inactive until subjected to reducing reaction.
  • the reduced state may be a reduced metal salt, but usually will be a metal in its 0 valence state.
  • Suitable metal salts in general are those of the Group VIII and Group IB elements.
  • the metals are preferably bound to organic anions.
  • suitable metal salts include silver lactate, iron citrate, gold acetate, and the like.
  • the advantage of metal-organic anion salts is that they are easily reduceable within the usual hardening temperature range of most plastics, and the anion portion will not have an adverse affect on the properties of the plastic.
  • metallic salts which can be heat reduceable to a catalytic state for electroless deposition, and the list is too numerous to mention, but would be readily apparent to one of ordinary skill in the art.
  • the metal salts need be used only in an amount sufficient such that when a surface layer of the plastic :body is removed, a sufficient quantity of the reduced metal salt will be present to catalyze an electroless metal plating from an electroless bath.
  • the metal salt may be admixed uniformly with the unhardened plastic, or it may be sprinkled on the surface of the unhardened plastic, contained in a suitable mold.
  • the metal salts can be added to the unhardened plastic in the form of a finely pulverized solid. Goodresults are obtainable by grinding both the metal salt and the filler in solid state or by grinding the solids in a disper-. sion in a volatile medium with subsequent evaporation of the latter. Another means of forming a fine particle size is by soaking a carrier with a metal salt solution and by evaportion of the solvent and pulverization of the dried mixture, a small grain particle size can be obtained.
  • the quantity of metal salt should be about 1 to 50 parts by weight of the metal salt acting as a catalyst per 99 to 50 parts by weight of the carrier.
  • the carrier may be selected such that it is soluble in the electroless deposition metal bath. Suitable carriers for the metal salt include the amino polycarbonic acids, oxycarbonic acids and the like.
  • dissolvable particulate fillers may be used, and particularly preferred are those fillers which are known to enhance the properties of the plastic body. There is no criticality in the particular filler used except it must be easily dissolvable from the plastic composition without substantial damage to the plastic body.
  • the filler may be solvent soluble or acid or base soluble depending upon the characteristics of the particular resin composition.
  • Suitable fillers have been found to be tartaric acid, citric acid, hydroxyethylene-diamine-tetra-acetic acid, and potassium tartarate. These fillers have been found to be quite suitable since they are easily dissolvable in water, sodium hydroxide and potassium hydroxide.
  • fillers as ethylene glycol-bisaminoethyl ether-tetra acetic acid, 1,2-diamino-cyclohexane-tetra acetic acid, ethylene diamine-tetra acetic acid, diethylene-triamine-tetra acetic acid, hydroxyethylene-diamine-triacetic acid and ethylene-diaminedi(0-hydroxy-phenyl)-acetic acid.
  • a finely distributed catalytic salt in its inactive state is added to the plastic in the unhardened state.
  • the plastic is then hardened and simultaneously the salt is activated during hardening of the plastic by reduction of the metal salt to its catalytically active state, usually the free metal.
  • thick metal layers may be deposited by subsequent direct metal precipitation onto the plastic without adversely affecting the physical or chemical properties of the plastic or the metal layer.
  • metal deposits of even greater than 30 microns can be adherently deposited onto the plastic surface.
  • the adhesion achieved according to this process appreciably exceeds that prescribed by the DIN 40,802 standards, i.e., pull-off of 3.2 kg. one-inch/width of sample. Adhesive values of 25 kg for corresponding sample widths have been achieved.
  • Another advantage of the present invention is that the surface of the plastic is enriched with catalyst. That is, a higher concentration of catalyst forms at the boundary areas of the plastic, than within the plastic, so that an active surface layer is obtained. This layer subsequently initiates a further chemical metal reduction during the electroless metal deposition process.
  • soluble filler may be dissolved by the medium of a copper bath. This entails the advantage that copperizing of the surface will only occur when the filler exposed at the surface is fully dissolved out so that the adhesion and the ductility of the separated metal layer will be appreciably increased.
  • the drawing shows a cross-section through a plastic body, the surface of which is coated with a metal layer 1.
  • the metal is a nickel layer which has been galvanically deposited onto a copper layer 2.
  • the copper layer 2 has been deposited onto the synthetic resin 3 so as to espouse its shape.
  • the synthetic resin 3 has been reinforced by carbon fibers 4.
  • the void spaces 5 had been formed by dissolving the filler from the exposed surface of the plastic.
  • Unexposed filler 6 is. left undissolved in the plastic body.
  • Metal particles 7 reduced from the metal salt are embedded between the grains of the filler and copper layer 2, with increasing concentration towards the latter. These metal particles 7 act as the catalyst for precipitation from an electroless deposition bath.
  • EXAMPLE 1 A plastic consisting of epoxy resin 100 gm, hardener gm, and acetone 20 gm, was mixed in the liquid state with 50 gm of powdered tartaric acid acting as the filler. Then 5 gm of silver lactate was added in finely distributed form and the synthetic substance so mixed was evenly deposited on a nonmetallic molding or shaping part X 200 X 5 mm so that a layer of about 20 microns thickness was obtained. The mold was heated to 120 C. for half an hour so as to harden the plastic layer. The silver lactate was reduced to powdered silver.
  • the surface was treated by chemical etching with chromic acid in order to dissolve out the exposed filler powder grains at the surface of the plastic boxes.
  • the form or mold was rinsed in water and introduced into a copper electroless deposition bath for the purpose of effecting electroless coppering.
  • the bath composition was as follows:
  • a nickel layer, acting as an additional protective coat was deposited onto the coppered mold in a galvanic metal bath of the following composition:
  • nickel sulfate 300.0 gm/liter nickel chloride 60.0 gm/liter boric acid 40.0 gm/liter Arbitrary thicknesses were found to be feasible after a copper layer of 30 microns thickness had been deposited within the shortest possible time in the copper bath. There was found to be no changes in the structure or in the properties of the fundamental plastic body.
  • Eolyester resin 100 gm ardener 20 gm acetone 20 gm in the liquid state was mixed with 10 gm of powdered ethylene-diamine-tetra-acetic acid and with 1 gm of gold acetate.
  • This mixed synthetic substance was deposited onto a non-metallic mold or form of glass-fiber reinforced plastic, so that a coat of about 20 microns thickness was achieved.
  • the mold was then heated to 100 C. for half an hour so as to harden the synthetic layer. Then the surface was treated with emery paper to free the powder grains of the filler and of the metal which were located in the region of the surface layer.
  • Electroless coppering as described in Example 1 was performed by inserting the mold or the plastic body into a copper bath of the following composition:
  • a nickel layer 15 mm thick was deposited from a galvanic nickel bath of the following composition:
  • a process for the deposition of a metal layer onto a plastic body which comprises:
  • olefin resins olefin resins, carbonate resins, acrylic resins, formaldehyde resins, and polyester resins;

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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)
US33993573 1972-03-16 1973-03-09 Process for depositing a metal layer upon a plastic Expired - Lifetime US3847649A (en)

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CH392972A CH578621A5 (xx) 1972-03-16 1972-03-16

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CH (1) CH578621A5 (xx)
DE (1) DE2216499A1 (xx)
FR (1) FR2176030B1 (xx)

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3998602A (en) * 1975-02-07 1976-12-21 Carl Horowitz Metal plating of polymeric substrates
US4004047A (en) * 1974-03-01 1977-01-18 General Electric Company Diffusion coating method
US4065316A (en) * 1976-07-19 1977-12-27 Western Electric Company, Incorporated Printing ink
DE2728465A1 (de) * 1977-06-24 1979-01-11 Preh Elektro Feinmechanik Verfahren zur herstellung von elektrisch leitenden und loetbaren anordnungen
US4158612A (en) * 1977-12-27 1979-06-19 The International Nickel Company, Inc. Polymeric mandrel for electroforming and method of electroforming
US4719145A (en) * 1983-09-28 1988-01-12 Rohm And Haas Company Catalytic process and systems
US4848348A (en) * 1983-11-14 1989-07-18 Minnesota Mining And Manufacturing Company Coated films
US5709586A (en) * 1995-05-08 1998-01-20 Xerox Corporation Honed mandrel
US5728433A (en) * 1997-02-28 1998-03-17 Engelhard Corporation Method for gold replenishment of electroless gold bath
GB2320728A (en) * 1996-12-30 1998-07-01 Coates Brothers Plc Depositing a metallic film involving pretreatment
US20080038453A1 (en) * 2006-08-14 2008-02-14 Hitachi Maxell, Ltd. Method for modifying surface of plastic member, method for forming metal film, and method for producing plastic member
US20110151268A1 (en) * 2008-08-22 2011-06-23 W.C. Heraeus Gmbh Material comprised of metal and lactic acid condensate and electronic component
WO2020122819A1 (en) * 2018-12-14 2020-06-18 Nanyang Technological University Metallization of three-dimensional printed structures
JPWO2019159747A1 (ja) * 2018-02-16 2021-01-28 ソニー株式会社 電極およびセンサ

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2854385C2 (de) * 1978-12-16 1982-04-15 Preh, Elektrofeinmechanische Werke, Jakob Preh, Nachf. Gmbh & Co, 8740 Bad Neustadt Gedruckte Schaltung
DE3243190A1 (de) * 1982-11-23 1984-05-24 Bayer Ag, 5090 Leverkusen Verfahren zur herstellung metallisierter textiler flaechengebilde

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3226256A (en) * 1963-01-02 1965-12-28 Jr Frederick W Schneble Method of making printed circuits
US3523824A (en) * 1966-12-29 1970-08-11 Ibm Metallization of plastic materials
US3770571A (en) * 1969-04-02 1973-11-06 Richardson Co Fabrication of printed circuit boards

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3226256A (en) * 1963-01-02 1965-12-28 Jr Frederick W Schneble Method of making printed circuits
US3523824A (en) * 1966-12-29 1970-08-11 Ibm Metallization of plastic materials
US3770571A (en) * 1969-04-02 1973-11-06 Richardson Co Fabrication of printed circuit boards

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4004047A (en) * 1974-03-01 1977-01-18 General Electric Company Diffusion coating method
US3998602A (en) * 1975-02-07 1976-12-21 Carl Horowitz Metal plating of polymeric substrates
US4065316A (en) * 1976-07-19 1977-12-27 Western Electric Company, Incorporated Printing ink
DE2728465A1 (de) * 1977-06-24 1979-01-11 Preh Elektro Feinmechanik Verfahren zur herstellung von elektrisch leitenden und loetbaren anordnungen
US4248921A (en) * 1977-06-24 1981-02-03 Steigerwald Wolf Erhard Method for the production of electrically conductive and solderable structures and resulting articles
US4158612A (en) * 1977-12-27 1979-06-19 The International Nickel Company, Inc. Polymeric mandrel for electroforming and method of electroforming
US4719145A (en) * 1983-09-28 1988-01-12 Rohm And Haas Company Catalytic process and systems
US4848348A (en) * 1983-11-14 1989-07-18 Minnesota Mining And Manufacturing Company Coated films
US5709586A (en) * 1995-05-08 1998-01-20 Xerox Corporation Honed mandrel
GB2320728A (en) * 1996-12-30 1998-07-01 Coates Brothers Plc Depositing a metallic film involving pretreatment
US5728433A (en) * 1997-02-28 1998-03-17 Engelhard Corporation Method for gold replenishment of electroless gold bath
US20080038453A1 (en) * 2006-08-14 2008-02-14 Hitachi Maxell, Ltd. Method for modifying surface of plastic member, method for forming metal film, and method for producing plastic member
US20110151268A1 (en) * 2008-08-22 2011-06-23 W.C. Heraeus Gmbh Material comprised of metal and lactic acid condensate and electronic component
JPWO2019159747A1 (ja) * 2018-02-16 2021-01-28 ソニー株式会社 電極およびセンサ
JP7283465B2 (ja) 2018-02-16 2023-05-30 ソニーグループ株式会社 電極およびセンサ
WO2020122819A1 (en) * 2018-12-14 2020-06-18 Nanyang Technological University Metallization of three-dimensional printed structures

Also Published As

Publication number Publication date
DE2216499A1 (de) 1973-09-27
FR2176030A1 (xx) 1973-10-26
FR2176030B1 (xx) 1977-04-22
CH578621A5 (xx) 1976-08-13

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