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
  • C23C18/2006—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
  • C23C18/2053—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 only one step pretreatment
  • C23C18/206—Use of metal other than noble metals and tin, e.g. activation, sensitisation with metals
• • 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
  • C23C18/2026—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by radiant energy
  • C23C18/2033—Heat
• • 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
• • 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
  • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
  • Y10S428/00—Stock material or miscellaneous articles
  • Y10S428/901—Printed circuit
• • 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
• • 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
  • Y10T428/31703—Next to cellulosic
• • 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]
  • Y10T428/31971—Of carbohydrate
• • 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
  • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
  • Y10T442/20—Coated or impregnated woven, knit, or nonwoven fabric which is not [a] associated with another preformed layer or fiber layer or, [b] with respect to woven and knit, characterized, respectively, by a particular or differential weave or knit, wherein the coating or impregnation is neither a foamed material nor a free metal or alloy layer
  • Y10T442/2475—Coating or impregnation is electrical insulation-providing, -improving, or -increasing, or conductivity-reducing

Definitions

• the present invention relates to a method for producing insulating material bodies by introducing metal salt solutions into the impregnating resin, the insulating materials thus obtained with metal salt particles finely distributed in the resin bond, and their use for producing printed circuits or printed circuit boards with completely or partially metallized surfaces, in particular with holes provided insulating material bodies, the inner walls of which have a metal covering.
• the invention therefore relates to a process for producing surfaces of insulating bodies suitable for electroless metal coating by using one or more compounds of groups VIII or IB of the Periodic Table of the Elements which can be reduced to metals, which by adding solutions of these compounds directly into the resin solution is marked.
• Such compounds which can be reduced to metals are known in large numbers and are mostly salts of the metals of the groups mentioned.
• the salts of the metals silver, cobalt, nickel, platinum and palladium which are preferred for practical reasons, palladium is very decidedly preferred, and of its salts palladium chloride is preferred.
• the metal compound should be added in amounts of 0.01 to 3, preferably 0.025 to 0.08% by weight, based on 100% by weight solids content of the resin solutions.
• the preferred solvent is water.
• Other solvents, as far as compatible with resin solutions, can also be used in exceptional cases and only in exceptional cases can be used as the sole solvent.
• ammonium chloride greatly reduces the amount of water required for the dissolution, especially when palladium chloride is used as the reducible metal compound.
• the electrical values of the insulating bodies produced are not affected by ammonium chloride, since the amount added is small and apparently the insulating bodies are removed at the high drying and curing temperatures.
• the amount of ammonium chloride used should be about 1.5 to 2.5 times the amount by weight of the metal compounds and, in particular, makes a decisive contribution to the solubility of palladium chloride in water, if appropriate also in other polar solvents. This makes it possible to add from 2 to 5% by weight of the amount of water added with the solution of the metal compounds, depending on the resin system used.
• Cresol resoles are sufficient to effect the reduction from the metal salts, in particular the palladium salts, to metallic palladium during the heat treatment.
• a small amount of a miscible formaldehyde-containing resin for example a phenol or cresol resole, can also be added to such resins.
• the object can also be achieved by adding the solution of the metal compound in water or, if appropriate, in a further compatible solvent, to the adhesive of one or more adhesive layers on or, if appropriate, in the insulating body.
• this adhesive layer forms one or both cover layers.
• the type and amount of the metal compounds here are the same as when they are added to the resin solution, so that palladium chloride is also decidedly preferred and the amounts are generally 0.01 to 3% by weight, based on the solids content of the adhesive.
• the stated amount of ammonium chloride should and can Solutions are increased, for example up to 3.5 times the amount by weight of the metal compound.
• Formalin or, if appropriate, further reducing agents can be added to the adhesive as a reducing agent, which lead to a corresponding formation of very finely divided metal particles in the subsequent heat treatment.
• the present method has the advantage of considerably simplifying the production process for the insulating material bodies, since a considerable number of process steps, namely the steps required for producing separate fillers or the subsequent steps for treating the surface with metal salt solutions, are now eliminated.
• the present method also offers advantages through a completely uniform deposition of the finest metal particles in the resin layer or the adhesive layer, the additional advantage being that during the production process of the laminate body, the metal compounds of the resin bond or the adhesive also penetrate into reinforcing layers of the insulating material body, which were not originally provided with solutions of the metal compounds during manufacture.
• the electroless metallization of the insulating material bodies in the surface layers as well as in particular in the provided or existing holes, recesses or recesses is achieved by the extraordinarily fine and evenly distributed metal parts produced according to the method. article much easier and improved. It is particularly advantageous that relatively small amounts of metal are sufficient to produce the catalyst.
• the insulating material bodies produced in accordance with the method comprise all generally flat base materials which can be used for the production of printed circuits, printed circuit boards etc. by electroless deposition of metals and further training to become metallic conductors, provided that at least one of the layers contained is used a resin solution or an adhesive layer is formed or is applied to any insulating material body and if at least part of the resins or the adhesive used has been provided with a solution of the metal compound in accordance with the process.
• the insulating material bodies comprise, in particular, insulating material bodies constructed from laminated materials, which have arisen from laminate webs and their sections after impregnation with resin solutions and their drying by pressing and pressure-hardening the resins of several such layers, as well as those insulating material bodies which additionally contain outer layers or intermediate layers made of differently produced materials .
• Insulated bodies are also to be understood to mean prepregs in the dried state, laminates produced therefrom, and any flat materials produced with at least one layer laminated on, pressed on or applied by means of an adhesive layer, insofar as metal compounds added in accordance with the process are not yet reduced or preferably in a reduced state in the form of the fine distributed metal particles are included.
• one or both surface layers or one or both layers close to the surface are generally provided with the metal salt solutions or the finely deposited metal particles, but layers lying inside the insulating material body can also be provided with metal compounds or the finely deposited metal particles. Advantages arise particularly in the case of holes or recesses which are later to be provided with metallic conductor layers.
• the invention accordingly further relates to the insulating material bodies which contain at least one insulating material layer or adhesive layer which has added dissolved metal compounds or finely distributed metal particles formed by their reduction, regardless of the materials or the processes by which the other constituents of the insulating material bodies are constructed.
• Another object of the invention is the use of the insulating material body for the production of printed circuits, printed circuit boards or the like.
• a paper web is first impregnated with a pre-impregnation resin (e.g. phenol-resol 2448 from Bakelite) and dried at 150 to 170 ° C, whereby a resin application of 20% by weight is obtained.
• a pre-impregnation resin e.g. phenol-resol 2448 from Bakelite
• This pretreated paper web is then impregnated again with the following resin solution and a total resin application of 120% is obtained after drying.
• the second resin solution is composed as follows: Diphenyl cresyl phosphate was used as the phosphate plasticizer.
• a solution of the metal compounds a solution of 100 parts of water containing 5 g of PdCl 2 and 10 g of NH 4 Cl is prepared by heating to 40 ° C. and added in proportions of 2% by weight per 100% by weight of the resin solution. This resin solution proved to be stable in storage in the required manner.
• the paper web was dried at 170 ° C., cut into prepregs in a conventional manner and stored for further processing.
• the laminates made from it can be perfectly metallized.
• Example 1 a paper web was first provided with 10% by weight of the first resin mentioned in Example 1 by means of a spraying process, and impregnated with a resin solution consisting of 75% by weight phenol-resole resin (solid resin components) without subsequent drying. and 25% by weight tricresyl phosphate consisted of which 1.5% by weight of a PdCl 2 solution consisting of 100 parts of water with contents of 2.5 parts of PdCl 2 and 6 parts of NH 4 Cl had been added. Drying took place at 160 ° C. The total resin application was 130% based on the weight of the paper web.
• an epoxy resin solution 97% epoxy resin DER 652 from DOW Chemicals and 3% dicyandiamide
• the prepregs are then processed into laminates in the heating press, onto which a uniform and flawless copper layer is deposited in a metallization bath in a comparatively short time.
• Example 1 is repeated, except that the same amount of PtCl 2 is added to the resin solution instead of PdCl 2 .
• the prepregs and laminates produced can be metallized with the corresponding result as in Example 1.

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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)
• Laminated Bodies (AREA)
• Compositions Of Macromolecular Compounds (AREA)
• Chemically Coating (AREA)

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• 1978
  • 1978-12-04 DE DE19782852375 patent/DE2852375A1/de not_active Withdrawn
• 1979
  • 1979-11-30 US US06/099,224 patent/US4317856A/en not_active Expired - Lifetime
  • 1979-12-03 EP EP19790104913 patent/EP0012333A1/de not_active Ceased
  • 1979-12-04 JP JP15643679A patent/JPS5579152A/ja active Pending

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