JP2014162994A - めっき触媒および方法 - Google Patents
めっき触媒および方法 Download PDFInfo
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- JP2014162994A JP2014162994A JP2014029468A JP2014029468A JP2014162994A JP 2014162994 A JP2014162994 A JP 2014162994A JP 2014029468 A JP2014029468 A JP 2014029468A JP 2014029468 A JP2014029468 A JP 2014029468A JP 2014162994 A JP2014162994 A JP 2014162994A
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- Prior art keywords
- solution
- monomer
- noble metal
- catalyst
- polymer
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000003054 catalyst Substances 0.000 title abstract description 80
- 238000007747 plating Methods 0.000 title abstract description 22
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- 239000000178 monomer Substances 0.000 claims abstract description 66
- 229910000510 noble metal Inorganic materials 0.000 claims abstract description 61
- 229920000642 polymer Polymers 0.000 claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 claims abstract description 31
- 239000002184 metal Substances 0.000 claims abstract description 31
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 30
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- 238000007772 electroless plating Methods 0.000 claims abstract description 12
- 150000003839 salts Chemical class 0.000 claims abstract description 12
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- 239000000758 substrate Substances 0.000 claims abstract description 11
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical class C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011976 maleic acid Substances 0.000 claims abstract description 8
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims abstract description 7
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Classifications
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- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
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- 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
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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
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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
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
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- C23C18/1879—Use of metal, e.g. activation, sensitisation with noble metals
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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
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- 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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- 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
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- 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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- 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
- C23C18/20—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
- C23C18/28—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
- C23C18/38—Coating with copper
-
- 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
- H05K3/182—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 characterised by the patterning method
- H05K3/185—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 characterised by the patterning method by making a catalytic pattern by photo-imaging
-
- 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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Abstract
【解決手段】貴金属ナノ粒子と、少なくとも2種のモノマー、(1)カルボキシル基又はカルボン酸塩基を2つ以上有するモノマー及び(2)π電子有効性フィーチャを有するモノマーから重合されるポリマーと、を含む溶液。この溶液は、非導電性表面上に金属を無電解めっきするためのプロセスの触媒に有用である。前記モノマー(1)がマレイン酸又はその塩であり、前記モノマー(2)がスチレン、置換スチレンと、ブタジエンから成る群から選ばれるものである。前記貴金属ナノ粒子が二価金属であり、好ましくはパラジウムである。
【選択図】なし
Description
以下に記載するプロセスに従って無電解銅めっきによってめっきしたテストクーポンを観察することによって、触媒の特性を評価した。テストクーポンとして、Shengyi製の従来のFR−4ラミネートおよびSY−1141を使用した。表面被覆率試験では、むき出しのラミネートを使用した。バックライト試験では、内層銅を有するCuクラッドラミネートを使用した。
(1)テストクーポンを1×6cm2に切断し、その縁部にSiC#240によってサンドブラスト仕上げを施した後、RO(逆浸透)水中で数回洗浄し、温風乾燥させた。
(2)表1に示す膨潤、酸化、中和、調整およびマイクロエッチングステップにより処理した。
(3)その後、各実施例に示すように、2.9〜10.9の様々なpH値で40℃の触媒溶液にテストクーポンを10分間浸した。テストクーポンを脱イオン水で洗浄した。
(4)35℃〜40℃で15分間、無電解銅めっきを行った。
以下に定義するめっき被覆率評価尺度を用いて、テストクーポンのめっき被覆率を評価した。
完全被覆−テストクーポンの表面の95%を超える面積がめっきされていた。
高−テストクーポンの表面の75%を超えるが95%未満の面積がめっきされていた。
中−テストクーポンの表面の50%を超えるが75%未満の面積がめっきされていた。
図1参照:低−テストクーポンの表面の5%を超えるが50%未満の面積がめっきされていた。
被覆なし−テストクーポンの表面の5%未満しかめっきされていなかった。
以下のプロセスに従ってバックライト試験を行った。
透過モード下にある倍率50倍の従来の光学顕微鏡下に、各板からの厚さ1mmの断面を設置した。顕微鏡下で観測される光の量によって銅堆積物の質を決定し、欧州バックライト評価尺度0〜5と比較した。光が観測されなかった場合には、断面は完全に黒く、バックライト評価で5.0と格付けした。これは、完全な銅被覆を示していた。暗い領域なく光が断面全体を透過した場合、これは壁面上に銅金属の堆積がごく僅かであるか全くないことを示しており、断面を0と格付けした。断面の一部が暗い領域で、明るい領域も有している場合には、それら領域は基準と比較して0から5の間で格付けした。
加速老化試験を以下のように行った。
50mLの一定体積の触媒作用浴または濃縮物を調製した後、40℃に維持された浴温度下、10mL/分の速度で7日間または数週間気泡を生成することによって溶液に加速老化試験を施した。その後、これら加速老化触媒作用浴を用いることで被覆率試験およびバックライト試験を再度行って、触媒活性が失われたかどうかを確認した。その一方、紫外−可視吸収など他の対応する試験も行った。
ステップ1−ポリ(ブタジエン−マレイン酸)1:1モル(Mw=10,000〜15,000)溶液(42%)2.38gを測定し、脱イオン(DI)水25mlで溶解させ、撹拌しながら3リットルのビーカーの中で780mlのDI水と混合し、1.0gのジクロロジアミン白金(II)を溶液に撹拌しながら添加した。NaOHによってpHを3.0〜4.0に調整した。
Pd濃縮物の成分を以下に挙げる。
Pd触媒濃縮物:
Pdイオン:0.5g/L
安定化剤としてのPBDMA:1.0g/L
DMAB:7.0mM
パラジウム塩(ジクロロジアミン白金(II))を二塩化パラジウム(実施例2)、テトラクロロパラジウム(II)酸ナトリウム(実施例3)および硫酸パラジウム(実施例4)にそれぞれ変更し、pHを表2に示すように変更した以外は、実施例1と同様にPd触媒濃縮物を調製した。実施例1と同じプロセスによって無電解銅めっきを行い、その結果を表2に示す。
以下のパラジウム源および条件を使用した以外は、実施例1と同様にPd触媒濃縮物を調製した。得られたPd触媒濃縮物を、[Pd2+]として5、10、15、25、50および100ppmに希釈した後、実施例1と同じプロセスに従って無電解銅めっきを行った。
(Pd触媒濃縮物)
Pdイオン:0.5g/L(Pd源:Na2PdCl4)
安定化剤としてのPBDMA:1.0g/L
DMAB:7.0mM
(他の条件)
合成温度:20〜25℃
合成後の保存pH:8.9
触媒作用浴pH:4.0
安定化剤をポリ(4−スチレンスルホン酸−co−マレイン酸)ナトリウム塩(PSSAcoMA、実施例7)、ポリ(スチレン−alt−マレイン酸)ナトリウム塩(PSMA、実施例8)、ポリ(アクリル酸)(PAA、実施例9)に変更した以外は、実施例1と同様にPd触媒濃縮物を調製した。各安定化剤の化学構造およびMwを表5に示す。この触媒濃縮物を調製した後、上で開示した加速老化試験(AAT)を行った。
Pd触媒濃縮物:
Pdイオン:0.5g/L(Pd源:Na2PdCl4または(NH3)2PdCl2のいずれか)
安定化剤:1.0g/L
DMAB:7.0mM
安定化剤およびパラジウム源を表4および表5に示すように変更した以外は、実施例1と同様にPd触媒濃縮物を調製した。実施例1と同じプロセスによって、無電解銅めっきを行った。その結果を表4および表5に示す。
Pd源および量を1.7gの硝酸銀(AgNO3)に変更し、還元剤(DMAB)の量を20mMに変更したこと以外は、実施例1と同様にしてAg触媒濃縮物を調製した。得られたAg触媒濃縮物を以下に示す。
Ag触媒濃縮物:
Agイオン:1.08g/L
還元剤(DMAB):20mM
AgイオンおよびPBDMAの量を表6に示すように変更した以外は、実施例21と同様にAg触媒濃縮物を調製した。Ag触媒濃縮物を270ppmに希釈し、実施例1と同様のプロセスに従って無電解銅めっきを行った。
Claims (8)
- 貴金属ナノ粒子およびポリマーを含む溶液であって、前記ポリマーが、少なくとも2種のモノマー、(1)カルボキシル基またはカルボン酸塩基を2つ以上有するモノマーおよび(2)π電子有効性フィーチャを有するモノマーから重合される溶液。
- 前記モノマー(2)が、芳香族ビニルモノマーおよびアルカジエンからなる群から選択される、請求項1に記載の溶液。
- 前記モノマー(2)が、スチレン、置換スチレンおよびブタジエンからなる群から選択される、請求項1に記載の溶液。
- 前記モノマー(1)がマレイン酸またはその塩である、請求項1に記載の溶液。
- 前記貴金属ナノ粒子が二価金属である、請求項1に記載の溶液。
- 前記貴金属ナノ粒子がパラジウムである、請求項5に記載の溶液。
- 貴金属ナノ粒子と、少なくとも2種のモノマー、(1)カルボキシル基またはカルボン酸塩基を2つ以上有するモノマーおよび(2)π電子有効性フィーチャを有するモノマーから重合されるポリマーとを含む溶液を調製する方法であって、
a)貴金属イオンと、少なくとも2種のモノマー、(1)カルボキシル基またはカルボン酸塩基を2つ以上有するモノマーおよび(2)π電子有効性フィーチャを有するモノマーから重合されるポリマーとを含む溶液を調製するステップと、
b)前記溶液を撹拌しながら前記溶液に還元剤を添加するステップとを含む方法。 - 非導電性表面上に金属を無電解めっきするための方法であって、
a)請求項1の溶液に、めっきしようとする基板を浸すステップと、
b)前記基板の無電解めっきを行うステップとを含む方法。
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US13/775,208 US10066299B2 (en) | 2013-02-24 | 2013-02-24 | Plating catalyst and method |
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CN110318043A (zh) * | 2018-03-28 | 2019-10-11 | 东莞市斯坦得电子材料有限公司 | 一种高稳定性、高活性的胶体钯制作工艺 |
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