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CN117904611A - Composition for pretreatment of electroless plating, pretreatment method of electroless plating, and electroless plating method - Google Patents

Composition for pretreatment of electroless plating, pretreatment method of electroless plating, and electroless plating method Download PDF

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Publication number
CN117904611A
CN117904611A CN202410090911.1A CN202410090911A CN117904611A CN 117904611 A CN117904611 A CN 117904611A CN 202410090911 A CN202410090911 A CN 202410090911A CN 117904611 A CN117904611 A CN 117904611A
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CN
China
Prior art keywords
electroless plating
acid
resin material
pretreatment
manganese
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Pending
Application number
CN202410090911.1A
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Chinese (zh)
Inventor
永峰伸吾
北晃治
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Okuno Chemical Industries Co Ltd
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Okuno Chemical Industries Co Ltd
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Publication of CN117904611A publication Critical patent/CN117904611A/en
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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
    • C23C18/2006—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
    • C23C18/2046—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
    • C23C18/2066—Use of organic or inorganic compounds other than metals, e.g. activation, sensitisation with polymers
    • 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
    • C23C18/2006—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
    • C23C18/2086—Multistep pretreatment with use of organic or inorganic compounds other than metals, 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
    • 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
    • C23C18/31—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
    • C23C18/31—Coating with metals
    • C23C18/38—Coating with copper
    • C23C18/40—Coating with copper 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
    • C23C18/31—Coating with metals
    • C23C18/38—Coating with copper
    • C23C18/40—Coating with copper using reducing agents
    • C23C18/405—Formaldehyde
    • 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
    • C23C18/42—Coating with noble metals
    • C23C18/44—Coating with noble metals using reducing agents

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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)
  • Inorganic Chemistry (AREA)
  • Chemically Coating (AREA)
  • Coating With Molten Metal (AREA)

Abstract

The present invention provides a pretreatment composition for electroless plating, a pretreatment method, and an electroless plating method, which can exhibit high plating deposition without using harmful chromic acid and expensive palladium and can reduce the number of steps. The present invention provides a pretreatment composition for electroless plating, which is characterized by containing 10mg/L or more of manganese ions and 10mg/L or more of monovalent silver ions.

Description

Composition for pretreatment of electroless plating, pretreatment method of electroless plating, and electroless plating method
(The present application is a divisional application of application 202110654779.9 of the application entitled "composition for pretreatment of electroless plating, pretreatment method of electroless plating, and electroless plating method" filed on day 11 of 6 of 2021)
Technical Field
The present invention relates to a composition for pretreatment of electroless plating, a pretreatment method of electroless plating, and an electroless plating method.
Background
In recent years, resin molded articles have been used as automobile parts for the purpose of reducing the weight of automobiles. For such purposes, for example, ABS resin, PC/ABS resin, PPE resin, polyamide resin, or the like is used as a resin molded body, and plating of copper, nickel, or the like is performed in order to impart a high-grade feel and a beautiful appearance. Further, as a method for forming a conductor circuit by imparting conductivity to a resin substrate, a method for forming a plating film of copper or the like on the resin substrate is performed.
As a general method for forming a plating film on a resin material such as a resin substrate or a resin molded body, there is a method in which after roughening the surface of the resin material by etching with chromic acid, neutralization and prepreg are performed as needed, then a catalyst for electroless plating is applied using a colloidal solution containing a tin compound and a palladium compound, and then an activation treatment (accelerator treatment) for removing tin is performed to sequentially perform electroless plating and electroplating.
However, in the above method, chromic acid is used, which causes a problem of being harmful to the environment and the human body. In addition, since expensive palladium is used for the purpose of catalyst administration, there is a problem that the cost becomes high. In addition, after the etching treatment step, a catalyst application step is required, which causes a problem of an increase in the number of steps.
As a method for forming a plating film on a resin material, there is proposed a method in which an aqueous solution containing a metal activator molecular species is brought into contact with a part to be plated to perform etching, and then brought into contact with a solution of a reducing agent capable of reducing the metal activator molecular species, and the part is brought into contact with an electroless plating solution to perform metal plating (see patent document 1).
However, the method described in patent document 1 has room for research on the components of the activator molecule species, and there is a problem that the formation of the plating film is insufficient.
Accordingly, development of a pretreatment composition, a pretreatment method, and an electroless plating method for electroless plating which can exhibit high plating deposition without using harmful chromic acid and expensive palladium and can reduce the number of steps has been demanded.
Prior art literature
Patent literature
Patent document 1: japanese patent No. 4198799
Disclosure of Invention
Technical problem to be solved by the invention
The present invention has been made in view of the above-described problems, and an object of the present invention is to provide a pretreatment composition, a pretreatment method, and an electroless plating method for electroless plating that can exhibit high plating deposition without using harmful chromic acid and expensive palladium and can reduce the number of steps.
Technical scheme for solving technical problems
As a result of intensive studies to achieve the above object, the inventors of the present invention have found that the above object can be achieved by a pretreatment composition for electroless plating, a pretreatment method and an electroless plating method, each of which contains 10mg/L or more of manganese ions and 10mg/L or more of monovalent silver ions, and have completed the present invention.
That is, the present invention relates to the following composition for pretreatment of electroless plating, pretreatment method, and electroless plating method.
1. An electroless plating pretreatment composition characterized by containing 10mg/L or more of manganese ions and 10mg/L or more of monovalent silver ions.
2. The composition for pretreatment of electroless plating according to item 1, wherein the valence of manganese of the manganese ion is 3 or more.
3. The pretreatment composition according to item 1 or 2, wherein the pH is 2 or less.
4. A pretreatment method for electroless plating of a resin material, comprising a step 1 of bringing a surface to be treated of the resin material into contact with a pretreatment composition,
The pretreatment composition contains 10mg/L or more of manganese ions and 10mg/L or more of monovalent silver ions.
5. An electroless plating method of a resin material, comprising:
(1) Step 1 of bringing the surface to be treated of the resin material into contact with the pretreatment composition, and
(2) A step 2 of bringing the surface to be treated of the resin material into contact with an electroless plating solution,
The pretreatment composition contains 10mg/L or more of manganese ions and 10mg/L or more of monovalent silver ions.
6. The electroless plating method as recited in claim 5, wherein the electroless plating solution contains a reducing agent that exhibits catalytic activity for silver.
Effects of the invention
The composition for pretreatment for electroless plating according to the present invention can exhibit high plating deposition in electroless plating in a subsequent step without using harmful chromic acid and expensive palladium. In addition, according to the composition for pretreatment for electroless plating of the present invention, the etching step and the catalyst application step do not need to be performed separately, and thus the steps for electroless plating can be reduced.
In addition, according to the pretreatment method for electroless plating of the present invention, the surface to be treated of the resin material is brought into contact with the pretreatment composition, whereby the surface to be treated can be etched, and the silver catalyst can be applied to the surface to be treated, so that the surface to be treated of the resin material can be easily treated, and the pretreatment process can be reduced.
In addition, according to the electroless plating method of the present invention, in the pretreatment step, the surface to be treated of the resin material is brought into contact with the pretreatment composition, whereby the surface to be treated can be etched, and the silver catalyst can be applied to the surface to be treated, and the catalyst applying step and the accelerator treating step are not required, so that the surface to be treated of the resin material can be easily treated, and the steps for electroless plating can be reduced.
Detailed Description
The present invention will be described in detail below.
1. Composition for pretreatment of electroless plating
The electroless plating pretreatment composition of the present invention (hereinafter sometimes referred to as "pretreatment composition") contains 10mg/L or more of manganese ions and 10mg/L or more of monovalent silver ions. Since the pretreatment composition of the present invention contains a specific amount of manganese ions and a specific amount of monovalent silver ions, the decrease in etching force on the surface to be treated of the resin material is suppressed, and the catalyst is sufficiently administered.
For example, in a pretreatment composition containing manganese ions and palladium ions, the etching power of manganese ions is reduced by containing palladium ions. In addition, in the pretreatment composition containing chromic acid and silver ions, silver chromate (Ag 2CrO4) precipitate as an insoluble precipitate is formed in the composition, and the silver ions are discharged to the outside of the system, and the catalyst is insufficiently administered.
In contrast, since the pretreatment composition of the present invention contains manganese ions and monovalent silver ions, the electroless plating solution is brought into contact with the surface to be treated of the resin material after the surface to be treated is brought into contact with the surface to be treated, and a plating film having excellent adhesion can be formed on the surface to be treated.
Further, since the pretreatment composition of the present invention contains manganese ions and monovalent silver ions, etching of the surface to be treated and catalyst administration can be performed simultaneously by contacting the surface to be treated of the resin substrate, and thus the catalyst administration step can be omitted.
The pretreatment composition of the present invention does not require the use of a palladium-tin colloidal solution as in the conventional catalyst administration step, and the step of activation treatment (accelerator treatment) for removing tin can be omitted.
That is, the pretreatment composition of the present invention can exhibit high plating deposition properties in electroless plating in a subsequent step without using harmful chromic acid and expensive palladium. In addition, according to the composition for pretreatment of electroless plating of the present invention, the etching step and the catalyst application step are not required to be performed separately, and the accelerator treatment step is not required, so that the steps in the electroless plating are greatly shortened.
(Manganese ion)
The manganese ion is not particularly limited as long as it has an oxidizing power. The valence of manganese in the manganese ion is preferably 3 or more, more preferably 4 or more, and further preferably 7. For example, the manganese ion contained in the pretreatment composition may be in the form of a manganese ion of a metal ion monomer such as trivalent manganese ion or tetravalent manganese ion, or in the form of a manganese ion such as permanganate ion which is a manganese ion of seven valences. Among these, tetravalent manganese ions and permanganate ions are preferable, and permanganate ions are more preferable, in that etching ability is more excellent. The manganese ion of divalent manganese does not have an oxidizing power, and the surface of the resin material cannot be etched even when used alone, but may be used in combination with the manganese ion of manganese having a valence of 3 or more.
The manganese ion may be used singly or in combination of two or more.
The manganese salt used for imparting manganese ions to the pretreatment composition is not particularly limited, and examples thereof include manganese (II) sulfate, manganese (III) phosphate, manganese (IV) oxide, sodium (VII) permanganate, potassium (VII) permanganate, and the like. Among these, manganese (III) phosphate, manganese (IV) oxide, sodium (VII) permanganate, and potassium (VII) permanganate are preferable, and sodium (VII) permanganate and potassium (VII) permanganate are more preferable, in that they can impart more excellent etching power.
The manganese salt may be used alone or in combination of two or more.
In the pretreatment composition of the present invention, the content of manganese ions is 10mg/L or more. If the content of manganese ions is less than 10mg/L, the resin material cannot be sufficiently etched, and the adhesion of the film formed by electroless plating is lowered. The manganese ion content is preferably 10mg/L to 100g/L, more preferably 100mg/L to 50g/L, still more preferably 0.2g/L to 30g/L, particularly preferably 0.5g/L to 15g/L, and most preferably 0.5g/L to 10g/L. By setting the lower limit of the content of manganese ions to the above range, the etching power of the pretreatment composition is further improved. In addition, by setting the upper limit of the content of manganese ions to the above range, the formation of manganese dioxide precipitate in the pretreatment composition is further suppressed, and the stability is further improved.
(Silver ion)
The silver ion contained in the pretreatment composition of the present invention is monovalent silver ion. The silver salt for administering monovalent silver ions is not particularly limited as long as stable monovalent silver ions can be administered in the bath when dissolved in the pretreatment composition, and the counter ions forming the silver salt do not adversely affect manganese ions. Specifically, silver (I) sulfate, silver (I) nitrate, and silver (I) oxide are exemplified. Among these, silver (I) nitrate is preferable in that it has high solubility and is industrially easy to use. Further, silver (I) sulfate is preferable in that the plating deposition property is better than a resin material formed of a resin which is difficult to deposit by plating, such as an acrylonitrile-butadiene-styrene copolymer resin (ABS resin), an alloyed resin of a styrene resin and a Polycarbonate (PC) resin, and the adhesion of the plating film is difficult to be further reduced.
The silver salt may be used alone or in combination of two or more.
In the pretreatment composition of the present invention, the monovalent silver ion content is 10mg/L or more. If the content of monovalent silver ions is less than 10mg/L, the electroless plating cannot be sufficiently precipitated. The monovalent silver ion content is preferably 10mg/L to 20g/L, more preferably 50mg/L to 15g/L, still more preferably 100mg/L to 10g/L. By setting the lower limit of the monovalent silver ion content to the above range, a sufficient amount of the silver catalyst is adsorbed on the surface of the resin material, and the electroless plating film is more sufficiently deposited. In addition, even if the upper limit of the content of monovalent silver ions is not less than the upper limit, adverse effects are not caused, but by setting the upper limit, the amount of silver salt used can be suppressed, and the cost can be reduced.
As the silver ion, monovalent silver obtained by dissolving metallic silver in an acidic manganese bath may be used. The acid used to form the acidic manganese bath is not particularly limited, and inorganic acids and organic sulfonic acids can be used.
Examples of the inorganic acid include sulfuric acid, phosphoric acid, nitric acid, hydrochloric acid, hydrofluoric acid, and boric acid. Among these, sulfuric acid is preferable in that the drainage is more excellent.
Examples of the organic sulfonic acid include aliphatic sulfonic acids having 1 to 5 carbon atoms such as methanesulfonic acid, ethanesulfonic acid, propanesulfonic acid, and pentanesulfonic acid; aromatic sulfonic acids such as toluene sulfonic acid, pyridine sulfonic acid, and phenol sulfonic acid. Among these, aliphatic sulfonic acids having 1 to 5 carbon atoms are preferable in that the pretreatment composition has good stability.
The above-mentioned acids may be used singly or in combination of two or more.
The acid concentration in the pretreatment composition of the present invention is not particularly limited, and for example, the total acid concentration is preferably 100 to 1800g/L, more preferably 800 to 1700g/L.
(Other Components)
The pretreatment composition of the present invention may contain a polymer compound in addition to the manganese ion and the silver ion. The type of the polymer compound is not particularly limited, and a cationic polymer can be suitably used in terms of promoting plating deposition. The content of the polymer compound is preferably 0.01 to 100g/L, more preferably 0.1 to 10g/L.
(Solvent)
In the pretreatment composition of the present invention, the solvent preferably contains the manganese ion, the silver ion, and other components added as necessary. The solvent is not particularly limited, and examples thereof include water, alcohol, a mixed solvent of water and alcohol, and the like.
The solvent is preferably water in view of excellent safety, that is, the pretreatment composition of the present invention is preferably an aqueous solution.
The alcohol is not particularly limited, and conventionally known alcohols such as ethanol can be used.
In the case of using a mixed solvent of water and alcohol, the concentration of alcohol is preferably low, and specifically, the alcohol concentration is preferably about 1 to 30 mass%.
The pretreatment composition of the present invention is preferably acidic. By making the pretreatment composition acidic, the etching treatment of the resin material is more sufficient. The pH of the pretreatment composition of the present invention is preferably 2 or less, more preferably 1 or less.
2. Pretreatment method for electroless plating of resin material
The pretreatment method for electroless plating of a resin material of the present invention comprises a step 1 of bringing a surface to be treated of the resin material into contact with a pretreatment composition containing 10mg/L or more of manganese ions and 10mg/L or more of monovalent silver ions.
(Process 1)
Step 1 is a step of bringing the surface to be treated of the resin material into contact with the pretreatment composition.
As the pretreatment composition, the composition described as the above-mentioned electroless plating pretreatment composition can be used.
The method for bringing the surface to be treated of the resin material into contact with the pretreatment composition is not particularly limited, and the surface to be treated of the resin material may be brought into contact by a conventionally known method. Examples of the method include a method of immersing a resin material in a pretreatment composition and a method of spraying a pretreatment composition onto a surface to be treated of a resin material. Among these, a method of immersing the resin material in the pretreatment composition is preferable in that the contact efficiency is further excellent.
The temperature of the pretreatment composition in step 1 is not particularly limited, but is preferably 30 to 100 ℃, more preferably 40 to 90 ℃, and even more preferably 50 to 80 ℃. By setting the lower temperature limit of the pretreatment composition to the above range, the etching of the surface of the resin material and the catalyst can be more sufficiently provided. Further, by setting the upper limit of the temperature of the pretreatment composition to the above range, a coating appearance with more excellent decorative properties can be obtained.
The contact time between the pretreatment composition and the surface to be treated of the resin material in step 1 is preferably 3 to 60 minutes, more preferably 5 to 50 minutes, and even more preferably 10 to 40 minutes. By setting the lower limit of the contact time to the above range, etching of the surface of the resin material and the catalyst are more sufficiently provided. Further, by setting the upper limit of the contact time to the above range, a film appearance with more excellent decorative properties can be obtained.
In addition, in the case of using a chromic acid-sulfuric acid mixed solution of the prior art, when monovalent silver ions are added to the bath, silver cannot be stably present as ions in the composition for pretreatment because precipitation of silver chromate (Ag 2CrO4) is directly generated. Therefore, in the case of using a chromic acid-sulfuric acid mixed solution of the prior art, it is difficult to use a composition for pretreatment containing silver ions as in the present invention.
The resin for forming the resin material as the object to be treated is not particularly limited, and various resin materials which have been conventionally subjected to etching treatment with a chromic acid-sulfuric acid mixed acid can be used, and a good electroless plating film can be formed on the resin material. Examples of the resin forming the resin material include: and styrene resins such as acrylonitrile-butadiene-styrene copolymer resins (ABS resins), resins in which the butadiene rubber component of ABS resins is replaced with an acrylic rubber component (AAS resins), and resins in which the butadiene rubber component of ABS resins is replaced with an ethylene propylene rubber component (AES resins). The above-mentioned styrene resin and an alloying resin of a Polycarbonate (PC) resin (for example, an alloying resin having a mixing ratio of about 30 to 70 mass% of the PC resin) and the like can also be suitably used. Polyphenylene ether resin (ETHER RESIN), polyphenylene ether resin (polyphenylene oxide resin), polybutylene terephthalate (PBT) resin, polyphenylene sulfide (PPS) resin, polyamide resin, and the like, which are excellent in heat resistance and physical properties, can also be used.
The shape, size, etc. of the resin material are not particularly limited, and according to the pretreatment method of the present invention, a good plating film excellent in decorative properties, physical properties, etc. can be formed even for a large-sized resin material having a large surface area. Examples of such large-sized resin materials include automobile-related parts such as radiator grilles, hub caps, medium and small-sized marks, door handles, and the like; an exterior member in the electric and electronic field; faucet fittings used in water supply places and the like; game machine products such as pachinko parts, etc.
In step 1 described above, the surface to be treated of the resin material is brought into contact with the pretreatment composition, and the surface to be treated is treated.
In the pretreatment method of the present invention, degreasing may be performed before the step 1 to remove dirt on the surface to be treated of the resin material. The degreasing treatment is not particularly limited, and the degreasing treatment may be performed by a conventionally known method.
In the pretreatment method of the present invention, the surface of the resin material may be post-treated with a post-treatment liquid containing an inorganic acid in order to remove manganese adhering to the surface after the step 1.
The inorganic acid is not particularly limited, and examples thereof include: hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, hydrofluoric acid, boric acid, and the like. Among these, hydrochloric acid is preferable in that the removal of manganese is excellent.
The inorganic acid may be used alone or in combination of two or more.
The content of the inorganic acid in the post-treatment liquid is not particularly limited, and may be about 1 to 1000 g/L.
The post-treatment method is not particularly limited, and for example, the resin material subjected to the pretreatment may be immersed in a post-treatment liquid having a liquid temperature of about 15 to 50 ℃ for 1 to 10 minutes by the pretreatment method. The post-treatment can further improve the deposition property and appearance of the formed coating film.
By the above-described pretreatment method for electroless plating of a resin material, the surface to be treated of the resin material can be etched, and the silver catalyst can be applied to the surface to be treated, so that the surface can exhibit high plating deposition in electroless plating in a subsequent step.
3. Electroless plating method for resin material
The electroless plating method for a resin material of the present invention comprises (1) a step 1 of bringing a surface to be treated of the resin material into contact with a pretreatment composition containing 10mg/L or more of manganese ions and 10mg/L or more of monovalent silver ions, and (2) a step 2 of bringing the surface to be treated of the resin material into contact with an electroless plating solution.
(Process 1)
The step 1 in the electroless plating method of the resin material of the present invention is the same as the step 1 described in the step 1 in the pretreatment method of electroless plating of the resin material described above.
(Process 2)
Step 2 is a step of bringing the surface to be treated of the resin material into contact with an electroless plating solution.
The method for bringing the surface to be treated of the resin material into contact with the electroless plating solution is not particularly limited, and may be any method conventionally known. As this method, a method of immersing the surface to be treated of the resin material in an electroless plating solution is preferable in that the contact efficiency is further excellent.
The electroless plating solution is not particularly limited, and a conventionally known self-catalytic electroless plating solution can be used. Examples of the electroless plating solution include a nickel electroless plating solution, a copper electroless plating solution, a cobalt electroless plating solution, a nickel-cobalt alloy electroless plating solution, and a gold electroless plating solution.
The electroless plating solution preferably contains a reducing agent that exhibits catalytic activity for silver as a reducing agent. Examples of the reducing agent include dimethylamine borane, formaldehyde water, glyoxylic acid, tetrahydroboric acid, and hydrazine.
The condition for bringing the surface to be treated of the resin material into contact with the electroless plating solution is not particularly limited, and for example, in the case of immersing the resin material in the electroless plating solution, the solution temperature of the electroless plating solution may be about 20 to 70 ℃ and the immersion time may be about 3 to 30 minutes.
The content of the reducing agent in the electroless plating solution is not particularly limited, but is preferably about 0.01 to 100g/L, and more preferably about 0.1 to 10 g/L. By setting the lower limit of the content of the reducing agent to the above range, plating precipitation property is further improved, and by setting the upper limit of the content of the reducing agent to the above range, stability of the electroless plating bath is further improved.
In the electroless plating method of the present invention, step 2 may be repeated 2 or more times as necessary. By repeating the step 2 two or more times, an electroless plating film having two or more layers can be formed.
In the electroless plating method of the present invention, the activation treatment may be performed by using an activation treatment liquid containing a reducing agent and/or an organic acid before the step 2 in order to improve the precipitation performance of the electroless plating.
The reducing agent used for the activation treatment is not particularly limited, and examples thereof include dimethylamine borane, formaldehyde water, glyoxylic acid, tetrahydroboric acid, hydrazine, hypophosphite, isoascorbic acid, ascorbic acid, hydroxylamine sulfate, hydrogen peroxide, glucose, and the like. Among these, dimethylamine borane, formaldehyde water, glyoxylic acid, tetrahydroboric acid, and hydrazine are preferable because plating precipitation is more excellent.
The above reducing agents may be used singly or in combination of two or more.
The concentration of the reducing agent in the activation treatment liquid is not particularly limited, but is preferably 0.1 to 500g/L, more preferably about 1 to 50g/L, and further preferably 2 to 25g/L.
The organic acid used for the activation treatment is not particularly limited, and examples thereof include formic acid, oxalic acid, glycolic acid, tartaric acid, citric acid, maleic acid, acetic acid, propionic acid, malonic acid, succinic acid, lactic acid, malic acid, gluconic acid, glycine, alanine, aspartic acid, glutamic acid, iminodiacetic acid, nitrotriacetic acid, fumaric acid, and the like. Among these, formic acid, oxalic acid, glycolic acid, tartaric acid, citric acid, and maleic acid are preferable in that plating precipitation is further improved.
The organic acid may be used alone or in combination of two or more.
The concentration of the organic acid in the activation treatment liquid is not particularly limited, but is preferably 0.1 to 500g/L, more preferably about 1 to 50g/L, and further preferably 2 to 25g/L.
The activation treatment method is not particularly limited, and for example, the resin material pretreated in the step 1 may be immersed in an activation treatment liquid having a liquid temperature of about 15 to 50 ℃ for about several seconds to 10 minutes.
In the electroless plating method of a resin material of the present invention, a plating step may be provided after step 2.
The plating step is performed by performing activation treatment with an aqueous solution such as an acid or an alkali as needed after the step 2, immersing the substrate in a plating solution, and performing plating.
The plating solution is not particularly limited, and may be appropriately selected from conventionally known plating solutions according to the purpose.
The plating method is not particularly limited, and for example, the resin material having the electroless plating film formed in the step 2 is immersed in an activation treatment liquid at a liquid temperature of about 15 to 50 ℃ for about several seconds to 10 minutes under a current density of about 0.1 to 10A/dm 2.
Examples
The present invention will be specifically described below with reference to examples and comparative examples. The present invention is not limited to the examples.
(Production of electroless plating film)
A flat plate (10 cm. Times.5 cm. Times.0.3 cm, surface area: about 1dm 2) of an ABS resin (manufactured by UMG ABS Co., ltd., trade name: UMG ABS 3001M) was prepared as a resin material of the plated material, and an electroless plating film was formed by the following method.
First, the resin material was immersed in an alkali degreasing solution (ACE CLEAN A-220 bath, manufactured by Aofield pharmaceutical industries Co., ltd.) at 40℃for 5 minutes, and then washed with water.
Next, additives were added to water as a solvent in the amounts shown in tables 1 and 2, and pretreatment compositions of examples and comparative examples were prepared. The resin material after washing was immersed in the prepared pretreatment composition at an immersion temperature of 68℃for 30 minutes.
Finally, the resin material was immersed at 40℃for 10 minutes in an electroless plating solution prepared by adding additives in water as a solvent in the amounts shown in tables 1 and 2, to form an electroless plating film.
TABLE 1
TABLE 2
The coating ratio and adhesion of the coating film formed by the above method were evaluated by the following methods.
(1) Coating ratio
The ratio of the area of the resin material surface where the electrolytic plating film was formed was evaluated as a coating ratio. The coating ratio was set to 100% when the entire surface of the resin material was coated.
(2) Peel strength measurement
The resin material having the electroless plating film formed thereon was immersed in a copper sulfate plating bath, and subjected to a plating treatment at a current density of 3A/dm 2 and a temperature of 25℃for 120 minutes to form a copper plating film, thereby producing a sample. The sample was dried at 80℃for 120 minutes and allowed to stand at room temperature. Next, a 10mm wide cut was made in the plating film, and the plating film was stretched in the vertical direction on the surface of the resin material by using a tensile tester (AUTOGRAPH AGS-J1 kN, manufactured by Shimadzu corporation), and the peel strength was measured. The results are shown in Table 3.
TABLE 3
As is apparent from the results of Table 3, the coating films formed by immersing the pretreatment compositions of examples 1 to 5 containing 10mg/L or more of manganese ions and 10mg/L or more of monovalent silver ions in the electroless plating solution were high in coating ratio and excellent in adhesion.
Further, it was found that the coating film formed by immersing in the pretreatment composition of examples 1 to 5 and immersing in the electroless plating solution had a coating ratio of 100% and was sufficiently coated, and therefore, it was not necessary to add a catalyst in a separate catalyst adding step to increase the coating ratio. Therefore, it was found that by using the pretreatment composition for electroless plating of the present invention, the adhesion of the catalyst to the jig surface used in the formation of the electroless plating film can be suppressed, and plating deposition on the jig surface can be suppressed. This can prevent the plating film deposited on the surface of the jig from being peeled off in a granular shape when the electroless plating film is formed by repeatedly using the jig, and the electroless plating film on the surface of the resin material from being uneven due to the plating film being taken in the electroless plating film on the surface of the resin material in each step.
In the case where the resin material is usually subjected to pretreatment by etching treatment with chromic acid, and then a catalyst for electroless plating is given by using a colloidal solution containing a tin compound, a palladium compound, and the like, chromic acid becomes catalyst poison, inhibits the adhesion of the catalyst to the surface of the clamp, and inhibits the deposition of the plating film on the surface of the clamp. However, when chromic acid is not used in consideration of the environment or the like, there is a problem that the electroless plating film formed on the surface of the resin material is uneven due to precipitation of the plating film in the jig.
In contrast, since the coating ratio of the plating film formed by immersing in the electroless plating solution after immersing in the pretreatment composition of the present invention is 100%, the plating film is sufficiently coated, and thus, it is not necessary to add a catalyst in a separate catalyst adding step to increase the coating ratio. Therefore, the catalyst can be prevented from adhering to the surface of the jig used for forming the electroless plating film, and deposition of the plating film on the surface of the jig can be prevented, and generation of irregularities in the electroless plating film formed on the surface of the resin material can be prevented.
It was found that when the pretreatment composition of comparative example 1 containing no manganese ions and comparative example 2 having a 7-valent manganese concentration of less than 10mg/L were used, the adhesion of the plating film was low.
In addition, it was found that in the case of using the pretreatment compositions of comparative examples 3 and 4 having monovalent silver ion concentrations of less than 10mg/L, the coating film formed was poor in coating.
In addition, it was found that when the pretreatment composition of comparative example 5 containing 50mg/L of 2-valent palladium ion in addition to monovalent silver ion was used, the coating ratio of the formed coating film was not lowered, but the adhesion of the coating film was lowered. In addition, in the case of using the pretreatment composition of comparative example 6 containing 20mg/L of 2-valent palladium ion, the degree of decrease in adhesion of the plating film was smaller than that of comparative example 5, but the coating ratio of the formed plating film was lower than that of comparative example 5.
Further, as can be seen from the comparison of comparative examples 3 and 7, if silver (I) sulfate is used as the silver salt for imparting monovalent silver ions, the coating ratio of the plating film is further improved.

Claims (3)

1. An electroless plating method of a resin material, comprising:
(1) A step 1 of bringing the surface to be treated of the resin material into contact with a pretreatment composition,
(2) A post-treatment step of post-treating the surface of the resin material with a post-treatment liquid containing an inorganic acid after the step 1, and
(3) A step 2 of bringing the surface to be treated of the resin material into contact with an electroless plating solution after the post-treatment step,
The pretreatment composition contains 10mg/L to 10g/L of manganese ions and more than 10mg/L of monovalent silver ions,
The valence of manganese of the manganese ion is more than 3,
When the valence of manganese of the manganese ion is 7, the manganese salt used for imparting manganese ion to the pretreatment composition is at least one selected from sodium permanganate (VII) and potassium permanganate (VII),
The pH of the pretreatment composition is 2 or less,
The electroless plating method does not include a catalyst administration step.
2. The electroless plating method according to claim 1, wherein:
The electroless plating solution contains a reducing agent that exhibits catalytic activity for silver.
3. The electroless plating method according to claim 1 or 2, characterized in that:
The inorganic acid is at least one selected from hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, hydrofluoric acid and boric acid.
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