JP2008523253A - 自己触媒無電解法の改善された安定化及び性能 - Google Patents
自己触媒無電解法の改善された安定化及び性能 Download PDFInfo
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Abstract
Description
本発明は,自己触媒無電解めっき浴を用いて基板に金属めっきする方法であって,前記めっき浴は表面活性剤,好ましくは置換アルキレンオキシド化合物を含み,前記方法は前記基板を前記めっき浴に接触させる工程を含み,前記めっき浴において少なくとも2つの相が存在するよう,前記めっき浴の曇り点よりも高い温度で前記めっき浴を作用させることを特徴とする方法を提供する。
(i)前記シリコン表面をエッチングする工程と,
(ii)前記シリコン表面を上記めっき浴に浸漬する工程と,
(iii)前記シリコン表面を銀金属で被覆する工程と,
(iiii)前記銀被覆されたシリコン表面を前記めっき浴から取り出す工程とを含む方法に関する。
本発明のめっき浴は通常以下の組成を有する:
めっき浴の曇り点よりも高い温度20℃〜100℃,好ましくは23℃〜85℃,より好ましくは50℃〜80℃にし,めっき浴のpHを9.5〜13にしてめっきを行う。
以下の組成/条件のめっき浴を用いて,Pd活性ポリマー成分に無電解銅めっきを施した:
曇り点よりも高い温度及び1ミクロン/時間のめっき速度でめっきを行った。ポリマー成分は平滑かつ非多孔質の銅表面により完全に被覆された。
1970年代にパールスタイン(Pearlstein)及びウェイトマン(Weightman)*により調製され自然浴分解としてよく知られるような,標準的な有機ボラン浴に,さらにポリアルキレンオキシド化合物を添加した:
*参考文献:F.パールスタイン及びR.Fウェイトマン(F. Pearlstein and R.F. Weightman)「ジメチルアミンボランを用いた銀の無電解析出(Electroless Deposition of Silver Using Dimethylamine Boran)」,めっき(Plating),61号,1974年2月,154〜157頁
導電性の測定には様々な方法がある。例えば,渦電流計(eddy current instrument)を用いて導電性を直接測定することができる。又は,めっきされたマイクロ波空洞の測定された反射係数から導電性を計算することができる。本実施例においては,測定された反射係数から導電性を計算した。
Claims (38)
- 自己触媒無電解めっき浴を用いて基板に金属めっきする方法であって,前記めっき浴は表面活性剤を含み,前記方法は前記基板を前記めっき浴に接触させる工程を含み,前記めっき浴中に少なくとも2つの相が存在するよう,前記めっき浴中の溶液の曇り点よりも高い温度で前記めっき浴を作用させることを特徴とする方法。
- 前記めっき浴中に2つの相が存在する請求項1記載の方法。
- 前記金属が,Ag,Cu,Pd及びCoから成る群より選択される請求項1又は2記載の方法。
- 前記金属がAg及びCuから成る群より選択される請求項3記載の方法。
- 前記金属がAgである請求項4記載の方法。
- 前記自己触媒無電解めっき浴を,20℃〜100℃,好ましくは23℃〜85℃,より好ましくは50℃〜80℃の温度で作用させる請求項1〜5いずれか1項記載の方法。
- 前記表面活性剤が,0.01g/l〜10g/l,好ましくは0.1g/l〜1.0g/l,より好ましくは0.1g/l〜0.3g/lの濃度で存在する請求項1〜6いずれか1項記載の方法。
- 前記表面活性剤が非イオン性である請求項1〜7いずれか1項記載の方法。
- 前記表面活性剤が置換アルキレンオキシド化合物である請求項8記載の方法。
- 前記表面活性剤がエチレングリコールモノマー単位を含む請求項9記載の方法。
- 前記表面活性剤がノニルフェノールエトキシレートである請求項10記載の方法。
- 前記自己触媒無電解めっき浴がさらに,分子量が100〜4000のポリエチレングリコールを含み,前記ポリマーの一部が前記水溶液に対して可溶性である請求項1〜11いずれか1項記載の方法。
- 前記自己触媒無電解めっき浴がpH上昇剤をさらに含む請求項1〜12いずれか1項記載の方法。
- 前記pH上昇剤が,例えば金属水酸化物塩などの塩基である請求項13記載の方法。
- 前記めっき浴のpHが9.5〜13の間,好ましくは10〜12の間である請求項1〜14いずれか1項記載の方法。
- 前記自己触媒無電解めっき浴が酸をさらに含む請求項1〜15いずれか1項記載の方法。
- 前記酸がホウ素酸である請求項16記載の方法。
- 前記自己触媒無電解めっき浴が還元剤をさらに含む請求項1〜17いずれか1項記載の方法。
- 前記還元剤が,ホウ素及びアルミニウムの水素化物及び金属水素化物塩,グルカミン,デキストロース,グリオキサール,ロッシェル塩,ロッシェル塩と結晶糖との混合物,転化糖,コバルトイオン,水素化物,金属水素化物塩,ヒドラジン,硫酸ヒドラジン,ジメチルアミンボラン,ジエチルアミンボラン,トリエチルアミンボラン,ホルムアルデヒド,次亜リン酸塩,グルコナート,多価アルコール,アルドン酸,アルドン酸ラクトン及び硫化物から成る群より選択される請求項18記載の方法。
- 前記金属が,0.05g/l〜5g/l,好ましくは0.3g/l〜3g/l,より好ましくは0.4g/l〜2.0g/lの濃度で存在する請求項1〜19いずれか1項記載の方法。
- 請求項1記載の金属層上に浸漬めっきにより金層をめっきする工程をさらに含む請求項1〜20いずれか1項記載の方法。
- 請求項1記載の金属が銀である請求項21記載の方法。
- 請求項21〜22いずれか1項記載の方法により被覆された被覆物。
- 前記基板がシリコン表面であり,前記金属が銀である請求項1〜22いずれか1項記載の方法。
- 前記シリコン表面と前記銀との間に中間層が存在しない請求項24記載の方法。
- (i)銀塩水溶液と,(ii)置換アルキレンオキシド化合物と,(iii)ホウ酸とを含む自己触媒無電解銀めっき浴。
- 金属が,0.5g/l〜5g/l,好ましくは0.3g/l〜3g/l,より好ましくは0.4g/l〜2g/lの濃度で存在する請求項26記載の自己触媒無電解銀めっき浴。
- 前記置換アルキレンオキシド化合物がノニルフェノールオキシレートである請求項26又は27記載の自己触媒無電解めっき浴。
- 前記置換アルキレンオキシド化合物が,0.01g/l〜10g/l,好ましくは0.1g/l〜1g/l,より好ましくは0.1g/l〜0.3g/lの濃度で存在する請求項26〜28いずれか1項記載の自己触媒無電解めっき浴。
- 分子量が100〜4000のポリエチレングリコールをさらに含み,前記ポリマーの一部が前記水溶液に対して可溶性である請求項26〜29いずれか1項記載の自己触媒無電解めっき浴。
- 前記ポリエチレングリコールが,0.2g/lまでの濃度で存在する請求項26〜30いずれか1項記載の自己触媒無電解めっき浴。
- さらに塩基を含む請求項26〜31いずれか1項記載の自己触媒無電解めっき浴。
- 前記塩基が,第I族及び第II族金属の水酸化物と,有機塩基とから成る群より選択される請求項26〜31いずれか1項記載の自己触媒無電解めっき浴。
- さらに還元剤を含む請求項26〜33いずれか1項記載の自己触媒無電解めっき浴。
- 前記還元剤が,ホウ素及びアルミニウムの水素化物及び金属水素化物塩,グルカミン,デキストロース,グリオキサール,ロッシェル塩,ロッシェル塩と結晶糖との混合物,転化糖,コバルトイオン,水素化物,金属水素化物塩,ヒドラジン,硫酸ヒドラジン,ジメチルアミンボラン,ジエチルアミンボラン,トリエチルアミンボラン,ホルムアルデヒド,次亜リン酸塩,グルコナート,多価アルコール,アルドン酸,アルドン酸ラクトン及び硫化物から成る群より選択される請求項34記載の自己触媒無電解めっき浴。
- さらに錯化剤を含む請求項26〜36いずれか1項記載の自己触媒無電解めっき浴。
- 前記錯化剤が,EDTA,ロッシェル塩,クエン酸,クエン酸ナトリウム,コハク酸,プロピオン酸,グリコール酸,酢酸ナトリウム,乳酸,ピロリン酸ナトリウム,ピリジウム−3−スルホン酸,酒石酸カリウム,クアドロール,リン酸ナトリウム,クエン酸カリウム,ホウ酸ナトリウム,シアン化ナトリウム,シアン化カリウム,トリエチレンテトラアミン及びメチルアミンから成る群より選択される請求項36記載の自己触媒無電解めっき浴。
- 介在金属層を必要とせずに銀金属をシリコン表面に直接自己触媒めっきする方法であって,
(i)前記シリコン表面をエッチングする工程と,
(ii)前記シリコン表面を請求項26記載のめっき浴に浸漬する工程と,
(iii)前記シリコン表面を銀金属で被覆する工程と,
(iiii)前記銀被覆されたシリコン表面を前記めっき浴から取り出す工程とを含む方法。
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SE0403042A SE0403042D0 (sv) | 2004-12-14 | 2004-12-14 | Improved stabilization and performance of autocatalytic electroless process |
SE0403042-5 | 2004-12-14 | ||
PCT/SE2005/001930 WO2006065221A1 (en) | 2004-12-14 | 2005-12-13 | Stabilization amd performance of autocatalytic electroless processes. |
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JP4891919B2 JP4891919B2 (ja) | 2012-03-07 |
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US (1) | US20080206474A1 (ja) |
EP (1) | EP1828435A4 (ja) |
JP (1) | JP4891919B2 (ja) |
KR (1) | KR101314035B1 (ja) |
CN (2) | CN101080512B (ja) |
AU (1) | AU2005317239B2 (ja) |
BR (1) | BRPI0519014A2 (ja) |
CA (1) | CA2591411C (ja) |
IL (1) | IL183354A0 (ja) |
MX (1) | MX2007006537A (ja) |
NO (1) | NO20072917L (ja) |
RU (1) | RU2398049C2 (ja) |
SE (1) | SE0403042D0 (ja) |
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JP2018523756A (ja) * | 2015-08-20 | 2018-08-23 | マクダーミッド アキューメン インコーポレーテッド | 無電解銀めっき浴及びその使用方法 |
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JP2016517914A (ja) * | 2013-03-27 | 2016-06-20 | アトーテヒ ドイッチュラント ゲゼルシャフト ミット ベシュレンクテル ハフツング | 無電解銅めっき溶液 |
JP2018523756A (ja) * | 2015-08-20 | 2018-08-23 | マクダーミッド アキューメン インコーポレーテッド | 無電解銀めっき浴及びその使用方法 |
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KR20070092988A (ko) | 2007-09-14 |
EP1828435A1 (en) | 2007-09-05 |
EP1828435A4 (en) | 2014-10-29 |
CN101693992B (zh) | 2012-12-26 |
WO2006065221A1 (en) | 2006-06-22 |
AU2005317239A1 (en) | 2006-06-22 |
RU2007126815A (ru) | 2009-01-27 |
UA91995C2 (ru) | 2010-09-27 |
US20080206474A1 (en) | 2008-08-28 |
CA2591411C (en) | 2014-01-28 |
CN101693992A (zh) | 2010-04-14 |
CA2591411A1 (en) | 2006-06-22 |
RU2398049C2 (ru) | 2010-08-27 |
MX2007006537A (es) | 2007-08-20 |
SE0403042D0 (sv) | 2004-12-14 |
BRPI0519014A2 (pt) | 2008-12-23 |
KR101314035B1 (ko) | 2013-10-02 |
CN101080512A (zh) | 2007-11-28 |
JP4891919B2 (ja) | 2012-03-07 |
AU2005317239B2 (en) | 2010-03-04 |
CN101080512B (zh) | 2011-08-17 |
IL183354A0 (en) | 2007-09-20 |
NO20072917L (no) | 2007-09-14 |
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