JP5767100B2 - ナノワイヤ及びナノワイヤを製造する方法 - Google Patents
ナノワイヤ及びナノワイヤを製造する方法 Download PDFInfo
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- JP5767100B2 JP5767100B2 JP2011500079A JP2011500079A JP5767100B2 JP 5767100 B2 JP5767100 B2 JP 5767100B2 JP 2011500079 A JP2011500079 A JP 2011500079A JP 2011500079 A JP2011500079 A JP 2011500079A JP 5767100 B2 JP5767100 B2 JP 5767100B2
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- nanowire
- segment
- layer
- cathode
- deposition
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Description
1.担体の腐食に起因するナノ粒子の接触の損失
2.溶解及び再度の堆積又はオストワルト熟成
3.表面エネルギーを最小化するためのナノ粒子の凝集
4.ナノ粒子の溶解及び水溶性イオンの移動
ナノワイヤ構造体の製造は、テンプレートベースの方法に基づく。該方法の部分ステップを図1において以下のように概略的に示す。
(c1)テンプレートフィルムに対するイオン照射
(b)伝導性の層の施し
(c2)イオントラックのエッチングによるナノ細孔の形成
(d1)ナノワイヤの堆積及びキャップ成長
(d2)第2の金属層の堆積
(e)テンプレートの溶解
図3は、網目状に結合したナノワイヤアレイを備えるナノワイヤ構造体の製造を概略的に示している。ここで、テンプレートフィルム12に、複数の異なる角度でイオンを照射する。それによって、潜在トラック、及び後では、交差ナノ細孔又は交差ナノワイヤが、互いに対してたとえば90度の角度で延在するようになる。当然のことながら、他の角度も可能である。
図1又は図3に基づいて説明されているようにナノワイヤ構造体1を製造することが確かに好ましいが、別個のセグメント化ナノワイヤ34を製造することも基本的に可能である。図4に製造ステップの概略図を示す。この場合、キャップ成長が始まる(d1)前に電気化学的堆積を停止させ、その後、陰極層26aを除去する。これは特に、陰極層26a、又は少なくとも第1の部分層22aがナノワイヤ34とは別の材料から成る場合に可能である。その後、ステップ(e)においてテンプレートフィルム12を溶解する。それによって、個々のナノワイヤ34が別々になる(図示せず)。
全ての上述した実施例は、本発明に従って、セグメント化ナノワイヤ34と共に製造される。
テンプレートフィルムの材料
平衡電圧に対して相対的な陰極堆積パルスの相対電圧
平衡電圧に対して相対的な陽極逆パルスの相対電圧
ナノ細孔32の直径
電解質溶液のpH値
は、ナノ細孔32内でのナノワイヤ34の堆積において、電気二重層がナノ細孔内で生成されるように、特に、ナノ細孔32内での電気二重層の大きさがナノ細孔32の直径の規模に収まるように選択される。
図5〜図7を参照すると、全ての実施例において、ナノワイヤ34の電気化学的堆積は、図5に示されている堆積装置82内で行われる。該堆積装置は、2つの電解槽86及び88を収容する金属キャリッジを押し入れることができる金属ハウジング84から成る。金属の良好な伝熱性に起因して、コントロールされる外部熱供給によって堆積装置を温度調整することが可能である。
本発明においては、様々な材料から成るナノワイヤ34の構造特性も調査した。電気化学的に堆積される材料においては、たとえば、晶子のサイズをコントロールすることが可能である。これは、機械的安定性、熱輸送特性及び電気輸送特性並びに表面積、ひいては触媒活性に対しても効果を有する。したがって、多数の特性に対して意図した通りに影響を与えることができる。
触媒のために、本発明による多数のナノワイヤ構造体1を積み重ねてまとめて扱うことが可能である。しかしながら、ナノワイヤ構造体1は寸法に起因して、1mm未満の、大抵は10マイクロメートル〜数百マイクロメートルの内部寸法を有する3次元構造体であるマイクロ構造システム内に個別に組み込むのにも適している。
本発明によれば、テンプレートフィルム12、この例ではポリマーフィルムに、対応するマスク110を通じて重イオンを照射することによって、非常に小さな寸法を有するナノワイヤ構造体又はナノワイヤアレイを生成することができる。事前に設けられているマスク、たとえばシャドーマスクが複数の開口又は孔を有し、各開口が後のマイクロ要素を規定する。マスクは、照射時にテンプレートフィルム12を覆い、それによって、覆われていない領域、すなわちマスクの開口において潜在イオントラック16が形成される。該潜在イオントラックは後にエッチングされてナノ細孔32となる。マイクロ要素の輪郭及び形状はしたがって、マスクによって与えられる。
Claims (22)
- ナノワイヤ(34)を製造する方法であって、
多数のナノ細孔(32)を有するテンプレート(12)であって、該ナノ細孔は該テンプレート(12)を、第1の面(12a)から対向する第2の面(12b)まで貫通する、テンプレート(12)と、該テンプレート(12)の前記第1の面(12a)上の陰極層(26a)とを用意するステップと、
電気化学的堆積によって前記ナノ細孔(32)内で前記ナノワイヤ(34)を成長させるステップであって、該ナノワイヤ(34)は、該ナノ細孔(32)内において前記陰極層(26a)上で成長する、成長させるステップと、
ここで、前記電気化学的堆積は、時間的に交互に連続する陰極堆積パルス(212)及び該陰極堆積パルス(212)間の陽極逆パルス(214)によってパルス化されて行われ、
前記陰極堆積パルス(212)の期間中、前記ナノワイヤ(34)はそれぞれ、それぞれの該陰極堆積パルス(212)の期間に依存する長さと、前記ナノ細孔(32)の直径によって規定される第1の直径とを有する主セグメント(34c)の分だけ、前記ナノ細孔(32)内で成長し、
前記陽極逆パルス(214)は、平衡電圧に対して正の最小電圧を有し、
前記陰極堆積パルス(212)間のそれぞれの前記陽極逆パルス(214)によって、前記ナノワイヤ(34)において第2の直径を有する結合セグメント(34d)が前記ナノ細孔(32)内で生成され、
前記第2の直径は前記第1の直径よりも小さく、それによって、厚い主セグメント(34c)と薄い結合セグメント(34d)とが前記ナノワイヤ(34)の長さに沿って交互に連続するセグメント化ナノワイヤ(34)が生成され、及び
前記テンプレート(12)を溶解すると共に除去し、前記セグメント化ナノワイヤ(34)を露出させるステップと、
を含む方法。 - 前記陽極逆パルス(214)は、平衡電圧に対して少なくとも+100mVの相対電圧を有する、請求項1に記載の方法。
- 前記陽極逆パルス(214)は、前記陰極堆積パルス(212)よりも小さい絶対電圧を有する、請求項1又は2に記載の方法。
- 前記陰極堆積パルス(212)は、少なくとも100mVの大きさの、平衡電圧に対して相対的な負の相対電圧を有する、請求項1〜3のいずれか一項に記載の方法。
- 前記陰極堆積パルス(212)は、少なくとも500mVの大きさの負の絶対電圧を有する、請求項1〜4のいずれか一項に記載の方法。
- 前記陽極逆パルス(214)は、前記陰極堆積パルス(212)間の時間的インターバルの間に印加され、前記時間的インターバルの時間は、前記陰極堆積パルス(212)の時間よりも短い、請求項1〜5のいずれか一項に記載の方法。
- 前記陰極堆積パルスの時間は60秒よりも短く、及び/又は、前記陽極逆パルス(214)は、前記陰極堆積パルス(212)間の時間的インターバルの間に印加され、かつ、前記時間的インターバルの時間は10秒よりも短い、請求項1〜6のいずれか一項に記載の方法。
- 前記陰極堆積パルス(212)と前記陽極逆パルス(214)とが時間的に連続して何回も繰り返される、請求項1〜7のいずれか一項に記載の方法。
- ナノ細孔(32)によって貫通される前記テンプレート(12)は、
(a)テンプレートフィルム(12)を用意するステップと、
(b)前記テンプレートフィルム(12)の前記第1の面(12a)上に前記陰極層(26a)を堆積するステップと、
(c1)イオンビームを前記テンプレートフィルム(12)に照射して、該テンプレートフィルム(12)を貫通する多数の潜在トラック(16)を生成するステップと、
(c2)前記潜在トラック(16)をエッチングして前記ナノ細孔(32)を形成するステップと、
によって製造される、請求項1〜8のいずれか一項に記載の方法。 - 請求項1〜9のいずれか一項に記載の方法によって製造される、セグメント化ナノワイヤ(34)。
- 電気化学的に堆積される材料から成るナノワイヤであって、
交互に連続する、第1の直径を有する多数の第1のセグメント(34c)及び第2の直径を有する多数の第2のセグメント(34d)を有し、
前記第1の直径は前記第2の直径よりも大きく、それによって、該ナノワイヤ(34)は長手方向においてセグメント化構造を有し、
前記第2のセグメント(34d)は前記第1のセグメント(34c)間の結合部分を形成し、
前記第1のセグメント(34c)及び前記第2のセグメント(34d)は、一体的に互いに結合しており、同一の電気化学的に堆積される材料から成る、
ナノワイヤ。 - 前記大きい方の直径を有する前記第1のセグメント(34c)は、前記小さい方の直径を有する前記第2のセグメント(34d)よりも長い、請求項11に記載のナノワイヤ。
- 前記大きい方の直径を有する前記第1のセグメント(34c)は、円柱形状を有する、請求項11又は12に記載のナノワイヤ。
- 前記第1のセグメント(34c)及び/又は前記第2のセグメント(34d)はそれぞれ、前記ナノワイヤの長手方向において、少なくとも部分的に一定の長さを有する、請求項11〜13のいずれか一項に記載のナノワイヤ。
- 前記第1のセグメント(34c)の直径は、前記ナノワイヤの長手方向にわたって500nmよりも小さい、請求項11〜14のいずれか一項に記載のナノワイヤ。
- 前記大きい方の直径を有する前記第1のセグメント(34c)の長さは1000nmよりも小さく、及び/又は、前記小さい方の直径を有する前記第2のセグメント(34d)の長さは50nmよりも小さい、請求項11〜15のいずれか一項に記載のナノワイヤ。
- 前記第1のセグメント(34c)及び前記第2のセグメント(34d)は、前記ナノワイヤ(34)の長手方向において規則的に交互に現れ、それによって、前記ナノワイヤ(34)の長手方向において途切れることなく、2つの第2のセグメント(34c)の間に常にちょうど1つの第1のセグメント(34d)が存在するようになる、請求項11〜16のいずれか一項に記載のナノワイヤ。
- ナノワイヤ構造体であって、
請求項11〜17のいずれか一項に記載の、多数の隣接して配置されるセグメント化ナノワイヤ(34)から成るアレイ(35)と、
該ナノワイヤのそれぞれが固く結合している少なくとも1つの陰極層(26a)と、
を備える、ナノワイヤ構造体。 - ナノワイヤ構造体であって、
請求項11〜17のいずれか一項に記載の、多数の隣接して配置されるセグメント化ナノワイヤ(34)から成るアレイ(35)と、
隔たって設けられている陰極層(26a)とカバー層(26b)とを備え、
前記セグメント化ナノワイヤ(34)は、前記陰極層(26a)と前記カバー層(26b)との間で延在し、前記セグメント化ナノワイヤ(34)は第1の端部(34a)において前記陰極層(26a)と、第2の端部(34b)において前記カバー層(26b)と固く結合しており、それによって、前記セグメント化ナノワイヤ(34)は、前記陰極層(26a)と前記カバー層(26b)とを互いに固く結合させ、前記陰極層(26a)と前記カバー層(26b)との間の空間を規定し、
前記セグメント化ナノワイヤ(34)間に相互に接続する開放空間が存在し、
それによって、両側が前記陰極層(26a)とカバー層(26b)によって境されており、かつ、多数の前記ナノワイヤ(34)によって貫通されていると共に、前記陰極層(26a)と前記カバー層(26b)とに平行な平面において2次元のオープンセル型である空隙構造(42)を有する、安定したサンドウィッチ状のナノ構造が、前記陰極層(26a)と前記カバー層(26b)との間で流体が前記2次元のオープンセル型の空隙構造(42)を通じて導かれることができるように、画定される、ナノワイヤ構造体。 - マイクロリアクタシステムであって、
流体供給部及び流体排出部を備えるマイクロ構造チャネルシステムと、
前記流体供給部と前記流体排出部間とのリアクタ要素としての、セグメント化ナノワイヤ(34)を備える、請求項18又は19に記載の少なくとも1つのナノワイヤ構造体(1)とを、
流体が、前記流体供給部から前記陰極層(26a)とカバー層(26b)との間の2次元のオープンセル型である空隙構造(42)内に導き入れられ、前記セグメント化ナノワイヤ(34)間の空間を通じて導かれ、前記流体排出部を通じて前記空隙構造(42)から排出されることができるように備え、
前記陰極層(26a)と前記カバー層(26b)との間の、前記ナノワイヤ構造体(1)の、前記空隙構造(42)は反応容積を形成し、前記ナノワイヤ(34)の円柱面は活性表面を形成し、前記流体は該活性表面と前記空隙構造(42)内で流れている間に相互作用する、マイクロリアクタシステム。 - 触媒システムであって、
流体供給部及び流体排出部を備えるマイクロ構造チャネルシステムと、
前記流体供給部と前記流体排出部間との触媒要素としての、請求項18又は19に記載の少なくとも1つのナノワイヤ構造体(1)とを、
流体が、前記流体供給部から前記陰極層(26a)とカバー層(26b)との間の2次元のオープンセル型である空隙構造(42)内に導き入れられ、前記セグメント化ナノワイヤ(34)間の空間を通じて導かれ、前記流体排出部を通じて前記空隙構造(42)から排出されることができるように備え、
前記陰極層(26a)と前記カバー層(26b)との間の、前記ナノワイヤ構造体(1)の、前記空隙構造(42)は触媒反応容積を形成し、前記ナノワイヤ(34)の円柱面は触媒活性表面を形成し、前記流体は該触媒活性表面と前記空隙構造(42)内で流れている間に相互作用する、触媒システム。 - センサ素子(150)であって、請求項18又は19に記載の第1のナノワイヤ構造体(1a)及び第2のナノワイヤ構造体(1a)を備える少なくとも1つの測定ユニットを有し、前記ナノワイヤ構造体(1a)はそれぞれ、それぞれのナノワイヤ構造体の接触のために、前記セグメント化ナノワイヤ(34)に結合している陰極層(26a)及びカバー層(26b)の少なくとも1つを備え、前記ナノワイヤ構造体間に加熱素子(152)が配置されている、センサ素子。
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