JP5134534B2 - 負の電流をパルスする電着を用いた合金堆積物の製造及びそのナノ構造の制御方法、並びにそのような堆積物を組み入れる物品 - Google Patents
負の電流をパルスする電着を用いた合金堆積物の製造及びそのナノ構造の制御方法、並びにそのような堆積物を組み入れる物品 Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Description
政府の権利
米国政府は、米国陸軍研究所契約/助成金#DAAD19−03−1−0235に従って本発明において特定の権利を有する。
ナノ結晶の金属は、大きさでナノメートルから1ミクロンの桁における粒度を特徴とする。そのひときわ優れた特性の組み合わせのために、これらの物質の研究に多大な尽力が注がれている。機械的設計で関心が持たれる耐力は、粒度が低下するにつれて耐力が増大するように、反比例して粒度に連鎖する。ナノ結晶の金属の研究に対する動機付けの1つは、粒度を原子長に近い大きさに低下させてこの傾向を活用することである。実際、ナノ結晶の金属はマイクロメートルの大きさより大きい結晶(マイクロ結晶)の対応物よりもはるかに高い耐力を提供し、この強度の増大と共に、ナノ結晶金属は、そのほかの利益、たとえば、耐久性の向上、並外れた腐食及び磨耗耐性、並びに望ましい磁気特性を提供することができる。
粒度制御を達成するための二極パルスの開示された方法は、制御された方式で正と負の間を反転する正及び負の電流の性能及び能力を備えた電源を付けて、既存の電着産業のいずれにおいても使用することができる。前の項で概説したように、BPPは、結晶の大きさに勾配をつける現在の方法に比べて複雑な状態なしで、勾配のついたナノ結晶の大きさを有する電着物を巧みに処理する能力を追加する。たとえば、堆積物は、基板界面では相対的に大きな(マイクロ結晶の)粒度を有すればよく、表面では粒度は単一のナノメートル規模に連続的に低下すればよく、2ナノメートル以下の極度に小さなサイズに低下さえしてもよい。この種の塗膜は、ナノ規模の結晶塗膜の優れた磨耗耐性及び腐食耐性を提供し、均一なナノ結晶の堆積物に比べて改善された耐久性及び表面下の堅牢性を持つ。
前述のことが、液体化学及びめっきパラメータを含めてNi−Wについての特定の2種系を議論したが、本発明の範囲は、この点に限定されない。複数の液体化学の変異及びめっきパラメータを、高度に制御されたナノ結晶の構造を有する電着2種合金に使用することができる。
粒度に対して利用可能な制御の程度は、系及び選択された粒度それ自体に依存する。一般に、工程の設計者及び操作者は、相対的にさらに小さな粒度に対してさらに正確な制御を有する。Ni−Wに類似し、堆積物の比率の関数としての粒度を定義する関係が図7で示されるように一般に負の傾きを有する場合、及び図8で示されるように反対に正の傾きを有し、Ag−Cu又は類似の系を説明すると考えられる場合の双方については、相対的にさらに小さな粒度を持つ本発明の最も正確な使用に対してほとんど可能性がある。
本明細書で開示され、説明される本発明は、基材上にナノ結晶合金を堆積する方法、そのような堆積された合金を組み入れる製品、並びに所望の粒度を達成するための物質選択及び電極電圧の供給のパラメータを決定する方法を包含する。
Claims (13)
- 少なくともニッケル及びタングステンを含む系の合金を堆積させる方法であって、該合金の堆積物が特定されたナノ結晶の平均粒度を有し、
a)ニッケル及びタングステンの化学種が溶解している液体を提供する工程と、
b)異なる時間帯において正の極性及び負の極性を有する非定常電位を供給するように構成された電源に連結された前記液体中に、第1の電極と第2の電極を提供する工程と、
c)第2の電極で特定されたナノ結晶の平均粒度の堆積を達成するために、異なる時間帯において正の極性及び負の極性を有する非定数の電位を供給し、その時間と極性が極性比を特徴付け、特定されたナノ結晶の平均粒度を達成するために、前記極性比が0より大きく1未満となるように電源を駆動する工程を含む堆積方法。 - さらに電源を駆動する前記工程が、電源を駆動して前記極性比を確立することを含み、前記極性比が、特定されたナノ結晶の平均粒度を相当する極性比に関連付ける補助方程式を参照して、選択されている請求項1記載の堆積方法。
- さらに電源を駆動する前記工程が、特定されたナノ結晶の平均粒度を少なくとも1つの指標粒度と比較し、少なくとも1つの指標粒度を相当する極性比に関連付け、粒度の変化を極性比の変化に関連付ける傾き情報を含む前記補助方程式を参照して、前記極性比が選択されている請求項2記載の堆積方法。
- 電源を駆動する前記工程が、正と負双方の極性を有する非定数の電位によって電源を駆動することを含み、前記極性比は、
a)前記傾き情報が指標粒度にて正の傾きを示す場合については、特定されたナノ結晶の平均粒度について、
i)指標粒度に相当する極性比より相対的に大きな極性比を用いて指標粒度よりも相対的に大きい粒度;及び
ii)指標粒度に相当する極性比より相対的に小さな極性比を用いて指標粒度よりも相対的に小さい粒度によって決定され、
b)前記傾き情報が指標粒度にて負の傾きを示す場合については、特定されたナノ結晶の平均粒度について相対的に、
i)指標粒度に相当する極性比より相対的に小さな極性比を用いて指標粒度よりも大きい粒度;及び
ii)指標粒度に相当する極性比より相対的に大きな極性比を用いて指標粒度よりも小さな粒度によって決定されている請求項3記載の堆積方法。 - 電源を駆動する前記工程が、非定数の電位によって電源を駆動することを含み、堆積中に供給される前記極性比が、
a)特定されたナノ結晶の平均粒度を有効成分の堆積物における相当する比率に関連付ける補助方程式;及び
b)有効成分の堆積物における相当する比率を堆積中に供給される極性比に関連付ける補助方程式を参照して決定されている請求項1記載の堆積方法。 - 電源を駆動する前記工程が、非定数の電位によって電源を駆動する工程を含み、堆積中に供給される前記極性比が、
a)特定されたナノ結晶の平均粒度に相当する有効成分の比率を同定すること;及び
b)特定されたナノ結晶の平均粒度に相当する同定された比率に相当する極性比を同定することによって決定されている請求項5記載の堆積方法。 - 電源を駆動する工程が、
a)補助方程式に基づいて、指標組成物のそれに相当する極性比よりも相対的に大きな極性比を用いて指標組成物における要素の比率よりも相対的に低い比率の相対的に大部分活性のある要素であるニッケル及びタングステンを有する電着組成物を達成すること;及び、
b)指標組成物のそれに相当する極性比よりも相対的に低い極性比を用いて指標組成物における要素の比率よりも相対的に大きい比率の相対的に大部分活性のある要素であるニッケル及びタングステンを有する電着組成物を達成することを含む請求項6記載の堆積方法。 - 電極にて堆積させるためのパラメータを決定する方法であって、系の合金が少なくともニッケル及びタングステンを含み、堆積物は特定されたナノ結晶の平均粒度を有し、堆積は第1の電極及び合金が堆積する第2の電極を用い、第1の電極及び第2の電極は、少なくともニッケル及びタングステンの化学種が溶解している液体中に存在し、異なる時間帯において正の極性と負の極性を有する電位を提供するように構成された電源を駆動し、
パラメータを決定する方法が、
a)少なくともニッケル及びタングステンの化学種が溶解している液体を選択する工程と;
b)供給された極性比の関数として粒度を表現する補助方程式に基づいて、特定されたナノ結晶の平均粒度に相当する、堆積中に電極に供給するための0より大きく1未満の極性比を決定する工程を含む堆積方法。 - 請求項1乃至8のいずれか1項に記載の堆積方法に従って製造されているニッケル及びタングステン合金製の製品。
- 合金の堆積物が、第1のナノ結晶の平均粒度を持つナノ結晶構造を有する第1の層領域を有し、さらに前記第1の層領域に隣接して且つそれと接触し、前記第1の粒度とは異なる第2のナノ結晶の平均粒度を持つナノ結晶構造を有する第2の層領域を有し、
電源を駆動する前記工程は、
i)第2の電極にて第1のナノ結晶の平均粒度の堆積物を達成するために、異なる時間帯において正の極性及び負の極性を有する非定数の電位を供給し、その時間と極性が第1の極性比を特徴付け、前記第1の極性比が0より大きく1未満となるように、第1の時間の間、電源を駆動する工程と、
ii)第2の電極にて第2のナノ結晶の平均粒度の堆積物を達成するために、異なる時間帯において正の極性及び負の極性を有する非定数の電位を供給し、その時間と極性が第1の極性比とは異なる第2の極性比を特徴付け、前記第2の極性比が0より大きく1未満となるように、第2の時間の間、電源を駆動する工程と、
を含んでいる請求項1記載の堆積方法。 - さらに、変動領域が第1の位置で第1のナノ結晶の平均粒度を有し、それから間隔をあけて第2の位置では、変動領域が異なった第2のナノ結晶の平均粒度を有し、第1の位置と第2の位置の間で平均粒度が異なるように、層領域の一方が平均粒度で変動を持つナノ結晶構造を有する領域を含み、
第2の時間の間、電源を駆動する前記工程がさらに、異なる時間帯において正の極性及び負の極性を有する非定数の電位によって電源を駆動することを含み、その時間と極性が異なった平均粒度の範囲に相当する非定数の極性比の範囲を特徴付け、前記範囲が0と1の間となるように電源を駆動する工程を含む請求項10記載の堆積方法。 - 少なくともニッケル及びタングステンを含む系の合金を堆積させる方法であって、
a)ニッケル及びタングステンを含む系が溶解している電気めっき液を提供する工程と、
b)液中に第1の電極及び第2の電極を提供する工程と、
c)0より大きく1以下の第1の極性比を特徴付ける非定数の電位によって第1の時間、電源を駆動する工程と、
d)第1の極性比とは異なる0より大きく1未満の第2の極性比を特徴付ける非定数の電位によって第2の時間、電源を駆動する工程を含む堆積方法。 - 合金の堆積物は平均粒度に変動を有しており、変動領域が第1の位置では第1のナノ結晶の平均粒度を有し、それから間隔をあけて第2の位置では前記変動領域は前記第1の平均粒度とは異なる第2のナノ結晶の平均粒度を有し、前記第1の位置と前記第2の位置の間では平均粒度が変動し、
電源を駆動する前記工程は、異なる時間帯において正の極性及び負の極性を有する非定数の電位によって駆動し、前記時間及び極性が、異なる平均粒度の範囲に相当する非定数の極性比の範囲を特徴付け、前記範囲が0と1の間となるように電源を駆動する工程を含む請求項1に記載の堆積方法。
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US20140242409A1 (en) | 2014-08-28 |
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