JP6180518B2 - 非導電性プラスチック表面を金属化するための方法 - Google Patents
非導電性プラスチック表面を金属化するための方法 Download PDFInfo
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- 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
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- 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
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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- 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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- C23C18/2006—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
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- 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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- C23C18/00—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
- C23C18/285—Sensitising or activating with tin based compound or composition
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- 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
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- 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
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- 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
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- 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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- C23C18/00—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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- C23C18/38—Coating with copper
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Description
本発明は、非導電性プラスチック表面の金属化前の、該表面の前処理に関するものであり、プラスチック部品の装飾コーティング又は機能性金属コーティングが必要とされる様々な産業で適用され得る。前処理は、六価クロムを含まない溶液中で行われる。
従来法の非導電性プラスチック表面の前処理法の後に、六価クロムを含有する溶液中で表面をエッチングすることからなる、無電解金属化、主として無電解ニッケルめっき又は銅めっきを行い、その後、パラジウム化合物のイオン性又はコロイド状溶液を活性化し、そして次亜リン酸ナトリウム溶液中での還元(殆どの場合)又はそれぞれ、プラスチック表面上に吸着された、パラジウムイオン又はコロイド状パラジウム粒子の酸性溶液(通常、塩酸)中での促進のいずれかを行う。
従って、本発明は、これまで、非導電性プラスチックから作られた物品の金属化を、環境的に安全な方法で、その後に適用された金属層の十分なプロセス信頼性と接着強度で達成することが出来なかった問題に基づくものである。
700mlの濃縮された硫酸を300mlの脱イオン水と混合する。溶液を冷却させる。次に、2gの塩素酸カリウム+10gの過塩素酸ナトリウムを溶液に溶解する。溶液は直ぐに使用できる。塩素酸カリウムよりも強い、第2の酸性化剤の過塩素酸ナトリウムが、任意選択である。これは組成物の寿命を延ばすが、その後にめっきされた金属層の良好な接着を得ることを必要としない。
物品の非導電性プラスチック表面を金属化する方法であって、以下の工程:
A)50〜80%v/v硫酸中で0.0016〜0.12モル/lの塩素酸イオン濃度をもたらす塩素酸イオンの源を含む上記のエッチング溶液でプラスチック表面をエッチングする工程;
B)金属コロイドの溶液又は金属の化合物の溶液を用いてプラスチック表面を処理する工程、その際、金属は、元素の周期律表の第I族遷移金属及び元素の周期律表の第VIII族遷移金属から選択される、及び
C)プラスチック表面を金属化溶液で金属化する工程
を含む、前記方法。
Ai)プラスチック表面を、アルカリ溶液を含む溶液中で処理する工程
が、工程A)と工程B)との間に実施される。
Ai)プラスチック表面を、塩素酸イオンの還元剤及び任意に第2の酸化剤を含む溶液中で処理する工程が、工程A)と工程B)の間に実施される。
Aii)プラスチック表面を水性酸性溶液中で処理する工程
を行うことができる。
Bi)水性の酸性溶液中でのプラスチック表面の処理及び
Bii)金属化溶液中でのプラスチック表面の無電解金属化
が、処理工程B)と処理工程C)との間に実施される。
Ci)金属化プラスチック表面の高められた温度での保存
が実施される。
以下に記載される実施例は、本発明を詳細に例示することを意図するものである。
ABS(アクリロニトリル−ブタジエン−スチレンコポリマー)及びPC/ABS(45%のポリカーボネートと55%のアクリロニトリルブタジエンスチレンコポリマーとの混合物)を、米国特許出願第2005/0199587A1号によって、50g/lのKMnO4を含有する45%v/vのリン酸溶液中で37℃で5分間(ABSの場合)又は15分間(PC/ABS)、又は0.5〜5.0g/lのKClO3を有する50〜80%v/vの硫酸溶液中で、エッチングし、そして酸化剤を20℃で1〜12分間添加する。エッチング時に、プラスチックを、10g/lのNaOHを含有する室温の中和溶液に1〜2分間浸漬し、その後、パラジウム化合物の実在の溶液(20℃で5分)又はコロイド溶液(35℃で2分)(コロイド溶液はDOW Chemical Company(「DOW」)の商標つきの溶液である)中での活性化を行う。実在溶液中のPdCl2濃度は0.1g/lであり、溶液のpHは2.7である。実在Pd溶液中での活性化の際に、プラスチックを、60℃で、pH9の20g/lの次亜リン酸ナトリウムを含有する溶液中で5分間保持する。商標つきのコロイド溶液中での活性化の際に、プラスチックを、DOWの商標つきの促進溶液を用いて、40℃で2分間処理する。その後、プラスチックを、DOWのNiposit−PMニッケルめっきプロセスを用いてニッケルめっきする。コーティングの品質は、完全に/不完全にめっきされたプラスチック表面、めっきされた又はめっきされていないプラスチゾル絶縁ラック、及び無電解ニッケルとプラスチックとの接着強度などの因子に基づいて評価する。付着性を評価するために、Niめっきをガルバニ銅浴中で厚くし、1cm幅をプラスチックから剥がすために必要な力を測定する(kg/cm)。ABS試験片の場合、過マンガン酸塩溶液でのエッチング時間は5分であり、PC/ABS試験片の場合、15分間であった。塩素酸塩溶液中でのエッチングの時間は、全ての試験片について5分間であった。金属化のためのプラスチック前処理の条件と金属化(無電解ニッケルめっき)の結果を以下の表2に示す。
7cmの直径を有するABSプラスチック(イネオス(Ineos)社製のNovodur P2MC)円形基板のディスクをステンレス鋼ワイヤに固定した。基板を、表4に規定された本発明による様々な前処理エッチング溶液に22℃の温度で4分間浸漬した(プロセスの順序を表3に示す)。その後、基板を約1分間流水で濯いだ。濯ぎに続いて、中和(処理工程Ai))、及び300ml/lの36%塩酸の溶液中への簡単な浸漬(処理工程Aii))の後に、基板を、パラジウムコロイドに基づくコロイド活性剤(アトテック(Atotech)社製のAdhemax Aktivator NA、100ppmのパラジウム)中で、40℃で3分間にわたり活性化した(処理工程B)。
Claims (12)
- 以下の工程:
A)プラスチック表面を、水性のエッチング溶液を用いてエッチングする工程;
B)プラスチック表面を、金属コロイドの溶液又は金属の化合物の溶液を用いて処理する工程、その際、該金属は、パラジウム、白金、イリジウム、ロジウム、金、銀及びこれらの金属のうち2種以上の混合物を含む群から選択される金属から選択される;及び
C)プラスチック表面を、金属化溶液を用いて金属化する工程
を含む、電気的に非伝導性の、物品のプラスチック表面を金属化する方法であって、エッチング溶液が、0.003〜0.08モル/lの塩素酸イオン濃度をもたらす塩素酸イオンの源と50〜80%v/vの硫酸を含み、且つエッチング溶液が、クロム(III)イオン及びクロム(VI)イオンを含有しないことを特徴とする、前記方法。 - 処理工程A)においてエッチング溶液中の塩素酸イオンの源が塩素酸ナトリウム及び塩素酸カリウムから選択されることを特徴とする、請求項1記載の方法。
- 塩素酸イオン濃度が0.01〜0.06モル/lの間の範囲であることを特徴とする、請求項1又は2に記載の方法。
- 塩素酸イオン濃度が0.004〜0.04モル/lの間の範囲であることを特徴とする、請求項1又は2に記載の方法。
- 硫酸イオン濃度が60体積%〜70体積%の間の範囲であることを特徴とする、請求項1から4までのいずれか1項に記載の方法。
- エッチング溶液がリン酸を更に含むことを特徴とする、請求項1から5までのいずれか1項に記載の方法。
- リン酸濃度が10〜30体積%の間の範囲であることを特徴とする、請求項6に記載の方法。
- 処理工程B)における金属がパラジウムであることを特徴とする、請求項1から7までのいずれか1項に記載の方法。
- プラスチック表面が、少なくとも1つの電気的に非伝導性のプラスチックから製造され、該少なくとも1つの電気的に非伝導性のプラスチックが、アクリロニトリル−ブタジエン−スチレンコポリマー、ポリアミド、ポリカーボネート、及びアクリロニトリル−ブタジエン−スチレンコポリマーと少なくとも1種の更なるポリマーとの混合物を含む群から選択されることを特徴とする、請求項1から8までのいずれか1項に記載の方法。
- 以下の更なる処理工程:
Ai)プラスチック表面を、ヒドロキシルアンモニウム硫酸塩、塩化ヒドロキシルアンモニウム及び過酸化水素を含む群から選択される還元剤を含む溶液中で処理する工程
を、処理工程A)と処理工程B)との間に実施することを特徴とする、請求項1から9までのいずれか1項に記載の方法。 - 以下の更なる処理工程:
Ai)プラスチック表面を、水酸化物イオンの源を含む中和剤を含む溶液中で処理する工程
を、処理工程A)と処理工程B)との間に実施することを特徴とする、請求項1から10までのいずれか1項に記載の方法。 - 以下の更なる処理工程:
Bi)プラスチック表面を水性の酸性溶液中で処理する工程及び
Bii)プラスチック表面を金属化溶液中で無電解金属化する工程
を、処理工程B)と処理工程C)との間に実施することを特徴とする、請求項1から11までのいずれか1項に記載の方法。
Applications Claiming Priority (3)
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LT2012042 | 2012-06-05 | ||
LT2012042A LT5997B (lt) | 2012-06-05 | 2012-06-05 | Plastikų paviršiaus paruošimo prieš jų cheminį metalizavimą būdas |
PCT/EP2013/061568 WO2013182590A1 (en) | 2012-06-05 | 2013-06-05 | Process for metallizing nonconductive plastic surfaces |
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JP2015518924A JP2015518924A (ja) | 2015-07-06 |
JP6180518B2 true JP6180518B2 (ja) | 2017-08-16 |
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JP2015515506A Active JP6180518B2 (ja) | 2012-06-05 | 2013-06-05 | 非導電性プラスチック表面を金属化するための方法 |
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US (1) | US20150129540A1 (ja) |
EP (1) | EP2855731B1 (ja) |
JP (1) | JP6180518B2 (ja) |
KR (1) | KR102130947B1 (ja) |
CN (1) | CN104364421B (ja) |
BR (1) | BR112014029353B1 (ja) |
CA (1) | CA2875323C (ja) |
ES (1) | ES2575001T3 (ja) |
LT (1) | LT5997B (ja) |
PL (1) | PL2855731T3 (ja) |
PT (1) | PT2855731E (ja) |
WO (1) | WO2013182590A1 (ja) |
Families Citing this family (7)
Publication number | Priority date | Publication date | Assignee | Title |
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LT6070B (lt) | 2012-12-07 | 2014-09-25 | Atotech Deutschland Gmbh | Plastikų paviršiaus paruošimo prieš jų cheminį metalizavimą būdas |
US10920321B2 (en) | 2014-05-30 | 2021-02-16 | Uab Rekin International | Chrome-free adhesion pre-treatment for plastics |
US9506150B2 (en) | 2014-10-13 | 2016-11-29 | Rohm And Haas Electronic Materials Llc | Metallization inhibitors for plastisol coated plating tools |
EP3181726A1 (en) * | 2015-12-18 | 2017-06-21 | ATOTECH Deutschland GmbH | Etching solution for treating nonconductive plastic surfaces and process for etching nonconductive plastic surfaces |
US20200087791A1 (en) * | 2017-06-01 | 2020-03-19 | Jcu Corporation | Multi-stage resin surface etching method, and plating method on resin using same |
FR3074808B1 (fr) | 2017-12-13 | 2020-05-29 | Maxence RENAUD | Outillage de galvanoplastie |
CN108624907A (zh) * | 2018-04-26 | 2018-10-09 | 复旦大学 | 非金属基体高效催化电极及其制备方法 |
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JPS52112668A (en) * | 1976-03-18 | 1977-09-21 | Sony Corp | Etching solution for plastics |
US4919768A (en) * | 1989-09-22 | 1990-04-24 | Shipley Company Inc. | Electroplating process |
US5160600A (en) * | 1990-03-05 | 1992-11-03 | Patel Gordhanbai N | Chromic acid free etching of polymers for electroless plating |
US6512182B2 (en) * | 2001-03-12 | 2003-01-28 | Ngk Spark Plug Co., Ltd. | Wiring circuit board and method for producing same |
DE10259187B4 (de) * | 2002-12-18 | 2008-06-19 | Enthone Inc., West Haven | Metallisierung von Kunststoffsubstraten und Lösung zum Beizen und Aktivieren |
US20050199587A1 (en) | 2004-03-12 | 2005-09-15 | Jon Bengston | Non-chrome plating on plastic |
LT2008082A (lt) * | 2008-10-28 | 2010-05-25 | Chemijos Institutas | Poliimido ir kitų plastikų ėsdinimo būdas |
JP5552269B2 (ja) * | 2009-07-02 | 2014-07-16 | トヨタ自動車株式会社 | 無電解めっき処理方法 |
CN102409320B (zh) * | 2011-11-29 | 2015-02-25 | 沈阳工业大学 | 一种abs塑料表面电镀前处理的方法 |
-
2012
- 2012-06-05 LT LT2012042A patent/LT5997B/lt unknown
-
2013
- 2013-06-05 CA CA2875323A patent/CA2875323C/en active Active
- 2013-06-05 US US14/399,987 patent/US20150129540A1/en not_active Abandoned
- 2013-06-05 KR KR1020147034195A patent/KR102130947B1/ko active IP Right Grant
- 2013-06-05 EP EP13727595.4A patent/EP2855731B1/en active Active
- 2013-06-05 JP JP2015515506A patent/JP6180518B2/ja active Active
- 2013-06-05 CN CN201380029727.6A patent/CN104364421B/zh active Active
- 2013-06-05 PT PT137275954T patent/PT2855731E/pt unknown
- 2013-06-05 WO PCT/EP2013/061568 patent/WO2013182590A1/en active Application Filing
- 2013-06-05 ES ES13727595.4T patent/ES2575001T3/es active Active
- 2013-06-05 PL PL13727595.4T patent/PL2855731T3/pl unknown
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Also Published As
Publication number | Publication date |
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JP2015518924A (ja) | 2015-07-06 |
ES2575001T3 (es) | 2016-06-23 |
CA2875323A1 (en) | 2013-12-12 |
PT2855731E (pt) | 2016-06-15 |
LT5997B (lt) | 2014-02-25 |
EP2855731A1 (en) | 2015-04-08 |
WO2013182590A1 (en) | 2013-12-12 |
CN104364421A (zh) | 2015-02-18 |
BR112014029353A2 (pt) | 2017-06-27 |
KR102130947B1 (ko) | 2020-07-08 |
US20150129540A1 (en) | 2015-05-14 |
CA2875323C (en) | 2020-08-25 |
LT2012042A (lt) | 2013-12-27 |
CN104364421B (zh) | 2017-07-21 |
PL2855731T3 (pl) | 2016-09-30 |
KR20150024327A (ko) | 2015-03-06 |
EP2855731B1 (en) | 2016-03-23 |
BR112014029353B1 (pt) | 2021-04-20 |
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