JP6322692B2 - プリント回路基板及びスルーホールの無電解金属化のための環境に優しい安定触媒 - Google Patents
プリント回路基板及びスルーホールの無電解金属化のための環境に優しい安定触媒 Download PDFInfo
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- JP6322692B2 JP6322692B2 JP2016238915A JP2016238915A JP6322692B2 JP 6322692 B2 JP6322692 B2 JP 6322692B2 JP 2016238915 A JP2016238915 A JP 2016238915A JP 2016238915 A JP2016238915 A JP 2016238915A JP 6322692 B2 JP6322692 B2 JP 6322692B2
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- catalyst
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- copper
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- starch
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- 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
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
- H05K3/42—Plated through-holes or plated via connections
- H05K3/422—Plated through-holes or plated via connections characterised by electroless plating method; pretreatment therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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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
- C23C18/1601—Process or apparatus
- C23C18/1633—Process of electroless plating
- C23C18/1655—Process features
- C23C18/1658—Process features with two steps starting with metal deposition followed by addition of reducing agent
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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
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1827—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment only one step pretreatment
- C23C18/1831—Use of metal, e.g. activation, sensitisation with noble metals
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- C—CHEMISTRY; METALLURGY
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- 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
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
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- C23C18/1837—Multistep pretreatment
- C23C18/1841—Multistep pretreatment with use of metal first
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- C—CHEMISTRY; METALLURGY
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- 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
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
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- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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- 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
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- C23C18/1879—Use of metal, e.g. activation, sensitisation with noble metals
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- 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
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1889—Multistep pretreatment with use of metal first
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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
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
- C23C18/1893—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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- 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
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- 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
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- 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
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- 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
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- 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
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- 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
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- C23C18/28—Sensitising or activating
- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
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- 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
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- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
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- 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
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- 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
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- C23C18/48—Coating with alloys
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- 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
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- C23C18/50—Coating with alloys with alloys based on iron, cobalt or nickel
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- 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
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
- H05K3/181—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating
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- 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
- H05K2203/0703—Plating
- H05K2203/0709—Catalytic ink or adhesive for electroless plating
Description
6g/Lのデンプンを、50℃〜55℃で加熱しながら、900mLのDI水を含むビーカー内で溶解させることによって、デンプン/銀触媒を調製した。デンプン溶液は、50g/Lで構成した。472mgの硝酸銀を50mLのDI水に添加し、完全に溶解するまで撹拌した。この混合物を溶液に添加し、連続的に加熱しながら勢いよく撹拌した。pHを9〜13に調整し、100mgのグルコースを20mLのDI水中に溶解し、溶液混合物を非常に勢いよく撹拌した。この溶液は無色から赤褐色に素早く変化し、銀イオンから銀金属への還元が示された。次いで、最終体積を1リットルに調整した。この溶液のpHを無機酸または有機酸で再調整し、合成したままの触媒は、ACCUMET AB15 pH計器を使用して測定した場合に5〜10のpHを有した。この触媒水溶液を含むビーカーを、約12時間にわたって50℃の水浴内に置いて、その安定性を試験した。約12時間後、観察可能な沈殿物は存在せず、この触媒が依然として安定であったことが示された。
実施例1で調製した触媒溶液を原液として使用し、2つのアリコートを、250ppmのナノ粒子濃度までDI水で希釈した。アリコートのpHを、アスコルビン酸で3または5のいずれかに調整した。デキストリン対還元剤の重量比は約60:1であった。
複数のスルーホールを有する6枚の異なる積層板:NP−175、370 HR、TUC−752、SY−1141、SY−1000−2、及びFR−408を提供した。NP−175はNan Yaによるものであった。370 HR及びFR4−408はIsolaによるものであった。TUC−752はTaiwan Union Technologyによるものであり、SY−1141及びSY−1000−2はShengyiによるものであった。これらの積層板のTg値は、140℃〜180℃の範囲であった。各積層板は5cm×12cmであった。各積層板のスルーホールは、次のように処理した:
1.各積層板のスルーホールを、78℃で7分間にわたり、CIRCUPOSIT(商標)MLB Conditioner 211でデスミア処理した。
2.次いで、各積層板のスルーホールを、流れる水道水で4分間濯いだ。
3.次いで、スルーホールを、10分間にわたり、78℃でpH13のCIRCUPOSIT(商標)MLB Promoter 213過マンガン酸水溶液で処理した。
4.次いで、スルーホールを、流れる水道水で4分間濯いだ。
5.次いで、スルーホールを、46℃で5分間にわたり、CIRCUPOSIT(商標)MLB Neutralizer 216−5溶液で処理した。
6.次いで、各積層板のスルーホールを、流れる水道水で4分間濯いだ。
7.次いで、スルーホールを、40℃で5分間にわたり、3%のCIRCUPOSIT(商標)Conditioner 231アルカリ性調整剤を含有する水性浴内で処理した。
8.次いで、各積層板のスルーホールを、流れる水道水で4分間濯いだ。
9.次いで、スルーホールを、室温で2分間にわたり、PREPOST(商標)748で処理した。
10.次いで、各積層板のスルーホールを、流れる水道水で4分間濯いだ。
11.次いで、これら6枚の積層板のスルーホールに、40℃で5分間にわたり、6g/Lのデンプンで安定化された硝酸銀からの300ppmの銀触媒で触媒した(触媒粒径は7〜10nmの範囲であった)。還元剤は、200ppmのグルコースであった。この触媒のpHを、アスコルビン酸で約6に調整した。
12.次いで、スルーホールを、流れる水道水で4分間濯いだ。
13.次いで、これらの積層板を、40℃でpH約13のCIRCUPOSIT(商標)880無電解銅めっき浴に浸漬し、スルーホールの壁上に銅を15分間堆積させた。
14.次いで、銅めっきされた積層板を、冷水で4分間濯いだ。
15.次いで、各銅めっき積層板を、圧縮空気で乾燥させた。
16.以下に記載されるバックライトプロセスを使用して、積層板のスルーホールの壁を、銅めっきの被覆度について検査した。
5g/Lのデンプンを、50℃〜55℃で加熱しながら、900mLのDI水を含むビーカー内で溶解させることによって、デンプン/銀触媒を調製した。472mgの硝酸銀を50mLのDI水に添加し、完全に溶解するまで撹拌した。この混合物を溶液に添加し、連続的に加熱しながら勢いよく撹拌した。pHを9〜13に調整し、300mgのスクロースを20mのDI水に溶解させた。この溶液混合物に、DI水を非常に勢いよく撹拌しながら添加した。この溶液は無色から赤褐色に素早く変化し、銀イオンから銀金属への還元が示された。次いで、最終体積を1リットルに調整した。この溶液のpHを無機酸または有機酸で再調整し、合成したままの触媒は、ACCUMET AB15 pH計器を使用して測定した場合に5〜10のpHを有した。この触媒水溶液を含むビーカーを、約12時間にわたって50℃の水浴内に置いて、その安定性を試験した。約12時間後、観察可能な沈殿物は存在せず、この触媒が依然として安定であったことが示された。
4g/Lのデンプンを、50℃〜55℃で加熱しながら、900mLのDI水を含むビーカー内で溶解させることによって、デンプン/銀触媒を調製した。472mgの硝酸銀を50mLのDI水に添加し、完全に溶解するまで撹拌した。この混合物を溶液に添加し、連続的に加熱しながら勢いよく撹拌した。pHを9〜13に調整し、300mgのガラクトースを20mLのDI水に溶解させた。この溶液混合物に、DI水を非常に勢いよく撹拌しながら添加した。この溶液は無色から赤褐色に素早く変化し、銀イオンから銀金属への還元が示された。次いで、最終体積を1リットルに調整した。この溶液のpHを無機酸または有機酸で再調整し、合成したままの触媒は、ACCUMET AB15 pH計器を使用して測定した場合に5〜10のpHを有した。この触媒水溶液を含むビーカーを、約12時間にわたって50℃の水浴内に置いて、その安定性を試験した。約12時間後、観察可能な沈殿物は存在せず、この触媒が依然として安定であったことが示された。
5g/Lのデンプンを、50℃〜55℃で加熱しながら、900mLのDI水を含むビーカー内で溶解させることによって、デンプン/銀触媒を調製した。472mgの硝酸銀を50mLのDI水と混合し、完全に溶解するまで撹拌した。pHを9〜13に調整し、20mLのDI水中に溶解した150mgのフルクトースをこの溶液に添加し、混合物を非常に勢いよく撹拌した。この溶液は無色から赤褐色に素早く変化し、銀イオンから銀金属への還元が示された。次いで、最終体積を1リットルに調整した。この溶液のpHを無機酸または有機酸で再調整し、合成したままの触媒は、ACCUMET AB15 pH計器を使用して測定した場合に5〜10のpHを有した。この触媒水溶液を含むビーカーを、約12時間にわたって50℃の水浴内に置いて、その安定性を試験した。約12時間後、観察可能な沈殿物は存在せず、この触媒が依然として安定であったことが示された。
4g/Lのデンプンを、50℃〜55℃で加熱しながら、900mLのDI水を含むビーカー内で溶解させることによって、デンプン/銀触媒を調製した。50mLのDI水中の472mgの硝酸銀を、完全に溶解するまで撹拌した。pHを9〜13に調整し、300mgのマルトースを20mのDI水に溶解させた。この溶液混合物に、DI水を非常に勢いよく撹拌しながら添加した。この溶液は無色から赤褐色に素早く変化し、銀イオンから銀金属への還元が示された。次いで、最終体積を1リットルに調整した。この溶液のpHを無機酸または有機酸で再調整し、合成したままの触媒は、ACCUMET AB15 pH計器を使用して測定した場合に5〜10のpHを有した。この触媒水溶液を含むビーカーを、約12時間にわたって50℃の水浴内に置いて、その安定性を試験した。約12時間後、観察可能な沈殿物は存在せず、この触媒が依然として安定であったことが示された。
Claims (10)
- 無電解めっきの方法であって、
a)基材を提供することと、
b)前記基材に触媒水溶液を適用することであって、前記触媒水溶液が、銀、金、パラジウム、イリジウム、銅、アルミニウム、コバルト、ニッケル、及び鉄から選択される1種以上の金属のナノ粒子と、デンプンと、グルコース、スクロース、ガラクトース、フルクトース、マルトース、及びそれらの混合物からなる群から選択される還元剤とを含み、前記デンプン対前記還元剤の重量比が150:1〜1:5であり、前記触媒水溶液がスズを含まない、適用することと、
c)前記触媒された基材を無電解金属めっき浴と接触させることと、
d)前記無電解金属めっき浴を用いて、前記触媒された基材上に金属を無電解的に堆積させることと、を含む、方法。 - 前記デンプン対前記還元剤の前記重量比が、110:1〜1:2である、請求項1に記載の方法。
- 前記デンプン対前記還元剤の前記重量比が、80:1〜1:1である、請求項2に記載の方法。
- 前記触媒水溶液が、1種以上の抗酸化剤をさらに含む、請求項1に記載の方法。
- 前記基材が、複数の開口部を備える、請求項1に記載の方法。
- 前記無電解的に堆積される金属が、銅、銅合金、ニッケル、またはニッケル合金である、請求項1に記載の方法。
- 前記ナノ粒子が、少なくとも直径1nmである、請求項1に記載の方法。
- 1種以上の安定化化合物が、250ppm〜10g/Lの量である、請求項1に記載の方法。
- 前記基材が、複数のスルーホールを備える、請求項1に記載の方法。
- 前記基材に調整剤を適用することをさらに含む、請求項1に記載の方法。
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US201562266780P | 2015-12-14 | 2015-12-14 | |
US62/266,780 | 2015-12-14 |
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US (1) | US20170171987A1 (ja) |
EP (1) | EP3181723A3 (ja) |
JP (1) | JP6322692B2 (ja) |
KR (1) | KR101898470B1 (ja) |
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US20170171988A1 (en) * | 2015-12-14 | 2017-06-15 | Rohm And Haas Electronic Materials Llc | Environmentally friendly stable catalysts for electroless metallization of printed circuit boards and through-holes |
EP3181724A3 (en) * | 2015-12-14 | 2017-08-16 | Rohm and Haas Electronic Materials LLC | Environmentally friendly stable catalysts for electroless metallization of printed circuit boards and through-holes |
JP6699378B2 (ja) * | 2016-06-14 | 2020-05-27 | Tdk株式会社 | コイル部品 |
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US3992211A (en) * | 1968-07-15 | 1976-11-16 | Trans-Metals Corporation | Electroless plating composition |
DE2257378C3 (de) * | 1972-11-23 | 1980-05-08 | Dr. Hesse & Cie, 4800 Bielefeld | Verfahren und Mittel zur Vorbehandlung von stromlos zu metallisierenden, nichtleitenden Trägeroberflächen |
JPH01319683A (ja) * | 1988-06-20 | 1989-12-25 | Electroplating Eng Of Japan Co | 白金コロイド溶液及びそれを用いた無電解白金メッキ方法ならびに白金担持体の製法 |
JP4143385B2 (ja) * | 2002-03-05 | 2008-09-03 | 株式会社大和化成研究所 | 無電解めっきの触媒付与のための前処理液、該液を使用する前処理方法、該方法を使用して製造した無電解めっき皮膜及び(又は)めっき被覆体 |
JP3881614B2 (ja) * | 2002-05-20 | 2007-02-14 | 株式会社大和化成研究所 | 回路パターン形成方法 |
US7166152B2 (en) * | 2002-08-23 | 2007-01-23 | Daiwa Fine Chemicals Co., Ltd. | Pretreatment solution for providing catalyst for electroless plating, pretreatment method using the solution, and electroless plated film and/or plated object produced by use of the method |
JP2005199267A (ja) * | 2003-12-15 | 2005-07-28 | Nippon Sheet Glass Co Ltd | 金属担持体の製造方法及び金属担持体 |
KR101215119B1 (ko) * | 2004-03-01 | 2012-12-24 | 스미토모덴키고교가부시키가이샤 | 금속콜로이드용액 및 잉크젯용 금속잉크 |
EP2222891B1 (en) * | 2007-11-23 | 2019-01-02 | The University Court Of The University Of Dundee | Nano-particle dispersions |
TWI453076B (zh) * | 2009-02-11 | 2014-09-21 | Univ Nat Cheng Kung | 可調粒徑奈米核殼材料之合成方法及其應用 |
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EP2444522B1 (en) * | 2010-10-21 | 2017-04-05 | Rohm and Haas Electronic Materials LLC | Stable nanoparticles for electroless plating |
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KR101936110B1 (ko) * | 2011-08-17 | 2019-01-08 | 롬 앤드 하스 일렉트로닉 머트어리얼즈 엘엘씨 | 인쇄회로기판의 무전해 금속화 방법 |
TWI524939B (zh) * | 2011-08-17 | 2016-03-11 | 羅門哈斯電子材料有限公司 | 用於無電金屬化之安定催化劑 |
US9138733B2 (en) * | 2011-08-17 | 2015-09-22 | Rohm And Haas Electronic Materials Llc | Stable tin free catalysts for electroless metallization |
CN102416478B (zh) * | 2011-11-24 | 2013-09-18 | 中国科学院宁波材料技术与工程研究所 | 一种制备不同形貌的银纳米粒子的绿色方法 |
US9810659B2 (en) * | 2013-02-08 | 2017-11-07 | Board Of Trustees Of Michigan State Univeristy | Nanoparticle-serialized oligonucleotide methods, compositions, and articles |
EP3181724A3 (en) * | 2015-12-14 | 2017-08-16 | Rohm and Haas Electronic Materials LLC | Environmentally friendly stable catalysts for electroless metallization of printed circuit boards and through-holes |
US20170171988A1 (en) * | 2015-12-14 | 2017-06-15 | Rohm And Haas Electronic Materials Llc | Environmentally friendly stable catalysts for electroless metallization of printed circuit boards and through-holes |
-
2016
- 2016-12-05 US US15/368,946 patent/US20170171987A1/en not_active Abandoned
- 2016-12-07 EP EP16202713.0A patent/EP3181723A3/en not_active Withdrawn
- 2016-12-08 JP JP2016238915A patent/JP6322692B2/ja active Active
- 2016-12-09 TW TW105140925A patent/TWI614372B/zh not_active IP Right Cessation
- 2016-12-12 KR KR1020160168366A patent/KR101898470B1/ko active IP Right Grant
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CN106868479A (zh) | 2017-06-20 |
KR101898470B1 (ko) | 2018-09-13 |
EP3181723A2 (en) | 2017-06-21 |
CN106868479B (zh) | 2019-09-03 |
JP2017110298A (ja) | 2017-06-22 |
EP3181723A3 (en) | 2017-08-16 |
US20170171987A1 (en) | 2017-06-15 |
KR20170074763A (ko) | 2017-06-30 |
TW201720957A (zh) | 2017-06-16 |
TWI614372B (zh) | 2018-02-11 |
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