JP2015516509A - 誘電体基板と金属層との間の密着性を促進するための方法 - Google Patents
誘電体基板と金属層との間の密着性を促進するための方法 Download PDFInfo
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- JP2015516509A JP2015516509A JP2015502219A JP2015502219A JP2015516509A JP 2015516509 A JP2015516509 A JP 2015516509A JP 2015502219 A JP2015502219 A JP 2015502219A JP 2015502219 A JP2015502219 A JP 2015502219A JP 2015516509 A JP2015516509 A JP 2015516509A
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
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- C23C18/405—Formaldehyde
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Abstract
Description
本発明は、誘電体の基板表面を金属化するための新規の方法であって、シラン組成物を施与する前記方法に関する。該方法は、基板とめっきされた金属との間の高い密着性を示す金属めっきされた表面をもたらし、同時に、滑らかな基板表面は保持される。
誘電体基板表面を金属化する様々な方法が公知である。湿式化学法において、金属化されるべき表面は、適切な前処理の後、まず触媒化され、その後、無電解法において金属化され、その後、適宜、電解的に金属化されるか、または、直接的に電解的に金属化されるかのいずれかである。
a) 酸化クロム(VI)を含有するエッチング溶液で表面を前処理する段階、その直後に、
b) パラジウム化合物/スズ化合物のコロイド状酸性溶液で表面を処理する段階、その際、吸着促進溶液と先に接触することを防ぐように注意する、
c) スズ(II)化合物によって還元され得る可溶性の金属化合物、アルカリ金属またはアルカリ土類金属水酸化物、および金属用の錯体形成剤を少なくとも金属水酸化物の析出を防ぐために充分な量で含有する溶液で表面を処理する段階、
d) 電解的な金属化溶液で表面を処理する段階
を必要とする。前記の方法は、ABS基板(アクリル−ブタジエン−スチレン)およびABS/PC(ポリカーボネート)に基づくプラスチック基板のために特に適している。
従って、本発明の課題は、誘電体基板表面を金属化するための方法であって、表面を実質的に粗面化しない一方で、基板と金属層との間の高い密着性が得られる方法を提供することである。
(i) 少なくとも1つのオルガノシラン化合物を含む溶液で前記表面を処理する段階、
(ii) 過マンガン酸塩の酸性またはアルカリ性水溶液から選択される酸化剤を含む溶液で前記表面を処理する段階、および次に
(iii) 湿式化学的なめっき法を用いて、段階(ii)の後に基板を金属化する段階
を、この順で含む方法によって解決される。
本発明によれば、段階(i)において、まず、オルガノシラン化合物を含有する組成物で基板を処理する。
A(4-x)SiBx
[式中、
各々のAは独立して加水分解性基であり、
xは1〜3であり、且つ
各々のBは独立して、C1〜C20−アルキル、アリール、アミノアリール、および式
CnH2nX
[式中、
nは0〜15、好ましくは0〜10、さらにより好ましくは1〜8、最も好ましくは1、2、3、4であり、且つ、
Xは、アミノ基、アミド基、ヒドロキシ基、アルコキシ基、ハロ基、メルカプト基、カルボキシ基、カルボキシエステル基、カルボキサミド基、チオカルボキサミド基、アシル基、ビニル基、アリル基、スチリル基、エポキシ基、エポキシシクロヘキシル基、グリシドキシ基、イソシアナト基、チオシアナト基、チオイソシアナト基、ウレイド基、チオウレイド基、グアニジノ基、チオグリシドキシ基、アクリルオキシ基、メタクリルオキシ基からなる群から選択される、またはXは、カルボキシエステル残基である、またはXは、Si(OR)3 [前記RはC1〜C5−アルキル基である]である]
によって示される官能基からなる群から選択される]
によって示される群から選択される。
(i) 少なくとも1つのオルガノシラン化合物を含む溶液で前記表面を10秒から10分の時間、15〜50℃の温度で処理する段階、
(ii) 濃度20〜100g/lの過マンガン酸イオンのアルカリ性の水溶液から選択される酸化剤を含む溶液で、1〜30分の時間の間、20〜95℃の温度で前記表面を処理して、150nm未満の平均表面粗さRaを有する粗面化された表面を得る段階
を含む。
好ましくは、第一の伝導層は銅を含み、且つ、無電解めっきによって堆積される。好ましくはこの場合、銅の無電解めっきに先立って、例えば貴金属含有コロイドまたは貴金属イオン含有溶液の堆積によって基板を活性化する。最も好ましい活性化は、パラジウム・スズコロイドまたはパラジウムイオンの堆積によるものである。そのような方法は当該技術分野において確立されており、且つ当業者に公知である。
a) 基板と、コロイド状またはイオン性触媒金属、例えば貴金属、好ましくはパラジウムを含有する活性化剤溶液とを接触させて、基板表面を触媒性にする段階、
および随意に、特に活性化剤がイオン性触媒金属を含有する場合、
b) 基板と還元剤とを接触させる段階、ここで、イオン性活性化剤の金属イオンが元素状金属に還元される、
または、活性化剤がコロイド状触媒金属を含有する場合、
c) 基板と促進剤とを接触させる段階、ここで、コロイドの成分、例えば保護コロイドが触媒金属から除去される、
を含むことができる。
(i) ベアの誘電体ビルドアップ層(1)を含み、その裏面の少なくとも一部の上にコンタクト領域(2)、および、ビルドアップ層(1)の裏面に取り付けられた第二の誘電体層(3)を有する基板を提供する段階、
(ii) 基板を通ってコンタクト領域まで延びる少なくとも1つの開口部(4)を、ビルドアップ層(1)内に形成する段階、
(iii) 少なくとも1つのオルガノシラン化合物を含む溶液で前記表面を処理する段階、
(iv) 少なくとも1つの酸化剤を含む溶液で前記表面を処理する段階、
(v) 伝導性シード層(6)を誘電体ビルドアップ層(1)の上部表面(5a)および少なくとも1つの開口部(4)の誘電体側壁(5b)上に堆積させる段階、
(vi) パターニングされたレジスト層(7)の開口部中に電気めっきによって銅層(8)を選択的に堆積する段階
をこの順で含む。
プラスチックを、無電解金属化のために、貴金属を含有する活性化剤を使用して活性化し、その後、無電解金属化を行う。その後、より厚い金属層を電解的に施与することもできる。直接めっき法の場合、エッチングされた表面を通常、パラジウムコロイド溶液で処理し、その後、錯化剤と共に錯体を形成する銅イオンを含有するアルカリ性溶液で処理する。その後、該物体を直接的に、電解的に金属化することができる (EP1054081号B1)。
A) コロイドの溶液で、または化合物、特に元素周期律表VIIIBまたはIB族の金属(貴金属)の塩、特にパラジウム/スズコロイドで処理する段階、および
B) 金属化溶液を使用して電解的に金属化する段階
を必要とすることがある。
iii. 湿式化学的めっき法を適用して基板を金属めっきする段階は、
iiia. 基板を貴金属コロイドまたは貴金属イオン含有溶液と接触させること、
iiib. 基板を無電解金属めっき溶液と接触させること、および
iiic. 基板を電解的な金属めっき溶液と接触させること
を含む。
iii1. 物体または基板を予備浸漬溶液中に浸漬させる段階、
iiia1. 物体または基板を濯ぎ溶液中で濯ぐ段階、
iiia2. 物体または基板を促進溶液中または還元剤溶液中で処理する段階、
iiib1. 物体または基板を濯ぎ溶液中で濯ぐ段階、および
iiic1. 物体または基板を濯ぎ溶液中で濯ぐ段階。
iii. 湿式化学的めっき法を適用して基板を金属めっきする段階は、
iiia. 基板を貴金属コロイドと接触させること、
iiib. 基板を変換溶液と接触させて、直接的に電解金属化するために充分に導電性の層を基板表面上に形成すること、および
iiic. 基板を電解金属めっき溶液と接触させること
を含む。
(i) Cu(II)、Ag、AuまたはNi可溶性金属塩またはそれらの混合物、
(ii) 0.05〜5mol/lのIA族金属の水酸化物、および
(iii) 前記金属塩の金属イオンのための錯化剤
を含むことができる。
iiic. 基板を、水溶性ポリマーと接触させる段階、
iiid. 基板を、過マンガン酸塩溶液で処理する段階、
iiie. 基板を、少なくとも1つのチオフェン化合物と、メタンスルホン酸、エタンスルホン酸およびエタンジスルホン酸を含む群から選択される少なくとも1つのアルカンスルホン酸とを含有する酸性の水溶液または水ベースの酸性のマイクロエマルションで処理する段階、
を実施し、且つ、
iv. 湿式化学めっき法を適用して基板を金属めっきする段階は、
ivb. 基板を電解金属めっき溶液と接触させる段階
を含む。
以下の例は、本発明の利点を説明することが意図されており、本発明の範囲を限定するものではない。
流量: 1.4ml/分(6ml/分)
ノズル距離: 4cm
ノズル速度: 40mm/秒
重なり: 14.2mm
窒素フロー: 0.8〜1.0 mPa
1回の噴霧サイクル
その後、パネルを10分間保持し、その後、それらを105℃で5分間ベークした。パネルを室温に冷却し、過マンガン酸塩エッチング液へと進めた(試料P3を除く)。
Claims (15)
- 誘電体基板表面を処理して、前記表面を次の湿式化学的な金属めっきのために準備するための方法であって、
(i) 少なくとも1つのオルガノシラン化合物を含む溶液で前記表面を処理する段階、
(ii) 過マンガン酸塩の酸性またはアルカリ性水溶液から選択される酸化剤を含む溶液で前記表面を処理する段階、
をこの順で含む、前記方法。 - 過マンガン酸塩の濃度が、20〜100g/lの範囲である、請求項1に記載の方法。
- オルガノシラン化合物が、以下の式
A(4-x)SiBx
[式中、
各々のAは独立して加水分解性基であり、
xは1〜3であり、且つ
各々のBは独立してC1〜C20−アルキル、アリール、アミノアリール、および式
CnH2nX
[式中、
nは0〜15、好ましくは0〜10、さらにより好ましくは1〜8、最も好ましくは1、2、3、4であり、且つ、
Xは、アミノ基、アミド基、ヒドロキシ基、アルコキシ基、ハロ基、メルカプト基、カルボキシ基、カルボキシエステル基、カルボキサミド基、チオカルボキサミド基、アシル基、ビニル基、アリル基、スチリル基、エポキシ基、エポキシシクロヘキシル基、グリシドキシ基、イソシアナト基、チオシアナト基、チオイソシアナト基、ウレイド基、チオウレイド基、グアニジノ基、チオグリシドキシ基、アクリルオキシ基、メタクリルオキシ基からなる群から選択される、またはXは、カルボキシエステル残基である、またはXは、Si(OR)3[前記RはC1〜C5−アルキル基である]である]
によって示される官能基からなる群から選択される]
によって示される群から選択される、請求項1に記載の方法。 - 前記加水分解性基Aが、−OH、−OR1からなる群から選択され、前記R1はC1〜C5−アルキル、−(CH2)yOR2であり、前記yは1、2または3であり、且つ前記R2はHであるかまたはC1〜C5−アルキル、−OCOR3であり、且つ前記R3はHまたはC1〜C5−アルキルである、請求項3に記載の方法。
- R1、R2およびR3は独立してメチル、エチル、プロピルおよびイソプロピルから選択される、請求項4に記載の方法。
- 前記オルガノシラン化合物が、ビニルシラン、アミノアルキルシラン、ウレイドアルキルシラン、メタクリルオキシシランおよびエポキシアルキルシランからなる群から選択される、請求項1から5までのいずれか1項に記載の方法。
- 前記オルガノシランが、0.5質量%〜20質量%の範囲の濃度で施与される、請求項1から6までのいずれか1項に記載の方法。
- 前記オルガノシランが、60〜250℃の範囲の沸点を有する極性有機溶剤中で溶解される、請求項1から7までのいずれか1項に記載の方法。
- 前記オルガノシランが、ジエチレングリコール、2−イソプロポキシエタノール(IPPE)、ジ(プロピレングリコール)メチルエーテルアセテート(DPGMEA)および2−エチル−1−ヘキサノールから選択される極性有機溶剤中に溶解される、請求項1から8までのいずれか1項に記載の方法。
- 段階1 ii)による酸化剤が、過マンガン酸イオンのアルカリ性水溶液である、請求項1から9までのいずれか1項に記載の方法。
- 以下の段階:
(i) 少なくとも1つのオルガノシラン化合物を含む溶液で前記表面を10秒から10分の時間、15〜50℃の温度で処理する段階、
(ii) 濃度20〜100g/lの過マンガン酸イオンのアルカリ性の水溶液から選択される酸化剤を含む溶液で、1〜30分の時間、20〜95℃の温度で前記表面を処理して、150nm未満の平均表面粗さRaを有する粗面化された表面を得る段階
を含む、請求項1から10までのいずれか1項に記載の方法。 - さらに、
(iii) 段階(ii)の後に湿式化学めっき法を用いて基板を金属化する段階
を含む、請求項1から11までのいずれか1項に記載の方法。 - 金属化が銅金属化である、請求項12に記載の方法。
- (iii) 段階(ii)の後に、湿式化学めっき法で基板を金属化する段階が、表面を伝導性にするために以下の段階:
(iiia) 基板を、コロイド状またはイオン性触媒金属、例えば貴金属、好ましくはパラジウムを含有する活性化剤溶液と接触させて、基板表面を触媒性にする段階、
および随意に、特に活性化剤がイオン性触媒金属を含有する場合
(iiib) 基板を還元剤と接触させる段階、ここで、イオン性活性化剤の金属イオンが元素状金属に還元される、
または、活性化剤がコロイド状触媒金属を含有する場合、
(iiic) 基板を促進剤と接触させる段階、ここで、コロイドの成分、例えば保護コロイドが触媒金属から除去される、
を含む、請求項12および13に記載の方法。 - 前記誘電体基板が、ベアの誘電体ビルドアップ層(1)を含み、その裏面の少なくとも一部の上にコンタクト領域(2)およびビルドアップ層(1)の裏面に施与された第二の誘電体層(3)を有し、ビルドアップ層(1)中に、基板を通ってコンタクト領域(2)まで延びる少なくとも1つの開口部(4)を有する基板であり、
(i) 請求項1から14までのいずれか1項において定義された少なくとも1つのオルガノシラン化合物を含む溶液で前記表面を処理し、
(ii) 請求項1から14までのいずれか1項において定義された酸化剤を含む溶液で前記表面を処理し、
(iii) 伝導性シード層(6)を、誘電体ビルドアップ層(1)の上部表面(5a)および少なくとも1つの開口部(4)の誘電体側壁(5b)上に堆積し、且つ
(iv) パターニングされたレジスト層(7)の開口部中に電気めっきによって銅層(8)を選択的に堆積する、請求項1から12までのいずれか1項に記載の方法。
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JP6234429B2 (ja) | 2017-11-22 |
WO2013143961A1 (en) | 2013-10-03 |
TWI569704B (zh) | 2017-02-01 |
KR101927679B1 (ko) | 2018-12-11 |
EP2823084B1 (en) | 2015-08-19 |
TW201352102A (zh) | 2013-12-16 |
EP2644744A1 (en) | 2013-10-02 |
KR20140143764A (ko) | 2014-12-17 |
US20150050422A1 (en) | 2015-02-19 |
EP2823084A1 (en) | 2015-01-14 |
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