JP5690714B2 - 薄膜製作方法 - Google Patents
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Description
を含んだステップを有する薄膜材料のパルスレーザー蒸着方法を得ることである。
図4は、周囲酸素圧(1×10−2mbar)における超短レーザーを使ったPLDによって製作されたTiO2薄膜のいくつかのSEM画像と、レーザーパルスプロファイルの対応する概要を示す。図4(a)−4(c)にはっきり示されているように、レーザーバースト中のパルス数が増加するにつれてフィルム中の粒子のサイズは減少する。図4(c)と4(d)に特に描かれているように、高倍率において19パルスバーストモードPLDで蒸着されたフィルム中に粒子を見つけることは困難である。PLDプロセスの作成物ではない表面に置かれた埃粒子が、SEM画像中に視認可能な唯一の構造である。この驚くべき結果は、バーストモード動作が広い範囲に渡って、例えば、予め決められた物理的性質を有する検出可能なナノ粒子の作成から実質的に無粒子の薄膜の形成まで、形態を調整するのに使われることができることを更に示唆している。後者の場合には、本発明の様々な実施形態が、基板の現場蒸着のためのメカニズム、即ち、蒸気が文字通り「休む間もなく」行われた微粒子崩壊によって形成されるもの、を提供する。
図6(a)−6(d)は、c−カットサファイアの単一クリスタル基板上に蒸着されたLiMn2O4、LiCoO2、およびそれらの複合材料フィルム(LiMn2O4とLiCoO2の蒸着時間比は図6(b)と図6(c)でそれぞれ1:1と12:1)の選択されたX線回折(XRD)θ−2θパターンである。材料の各々についての蒸着比は各ターゲットの蒸着時間によって制御された。基板の成長温度は600℃である。レーザーパラメータ、例えばバーストパルス数、レーザーフルエンスおよびレーザー繰り返しレートは、8パルス、0.4μJ(0.64W)および200kHzである。蒸着中の処理酸素ガス圧は1×10−2mbarであった。データは、Rigaku MiniFlex X-Ray Diffractometerを使って得られた。図6(a)と(b)に示されるように、結晶質のLiMn2O4とLiCoO2フィルム(ナノ粒子)をc−カットAl2O3基板上にエピタキシャルに成長させた。図6(b)と(c)に示されるように、LiMn2O4とLiCoO2結晶相の両方が、LiMn2O4とLiCoO2薄膜の混合物中に観察された。材料は相分離された複合材料であって固溶体ではないことが示された。
パルス、最も好ましくはフェムト秒パルスのバーストを使うことは粒子サイズの制御を提供する。図7(D)−(F)は、図7(A)−(C)に描かれた例示的バーストパラメータを使って蒸着されたTiO2フィルムの追加のSEM画像である。3つの描写では、バーストモードパルス数は(A)から(C)までそれぞれ1、5、10である。バースト繰り返しレートが、レーザーショット(毎秒)の同じ総数と同じ総平均パワー(0.4W)を保つように変動されられる。パルスエネルギーは3つの場合全てにおいて0.4μJである。蒸着は、1×10−2mbarの酸素中で室温において行われた。
図9B:10パルス、0.5μJパルスエネルギー、200KHz繰り返しレート、1W平均パワー、
図9C:19パルス、0.05μJパルスエネルギー、1MHz繰り返しレート、0.95W平均パワー、
AFM結果は、特許の図4(a)−(c)に示されたSEM結果を表すものであるが、処理のために異なるサンプルが使われた。
Claims (12)
- 薄膜材料のパルスレーザー蒸着方法であって、
レーザーパルスのバーストを使うバーストモードレーザーアブレーションをターゲット材料に対して行うことであって、各バーストは、フェムト秒からピコ秒の範囲にあるパルス幅を有する一群のレーザーパルスを含み、一のバーストの少なくとも2つのパルス間の時間分離は、前記バーストの少なくとも一つのパルスと、前記バーストの少なくとも一つの先行パルスによる前記ターゲット材料のアブレーションから生じるプラズマとの相互作用をもたらすべく選択され、前記相互作用は真空チェンバー内で行われることと、
前記アブレーションがされた材料を基板上に蒸着して薄膜を形成することであって、前記基板は、前記真空チェンバー内で前記バーストによって生成されたプラズマのストリーム中に配置されることと
を含み、
前記膜の形態は、前記バーストの一以上のパラメータを調整することによって、その上又は中にナノ粒子を有する膜から粒子不存在の膜まで連続的に調整可能であり、
前記膜の上又は中にある粒子の平均粒径及び数は、数マイクロ秒までのバースト持続時間にわたり一のバースト中のパルス数を増加させることによって減少し、
各バースト中のパルス数と前記バーストの繰り返しレートは、独立して制御され、
前記パラメータ及び数マイクロ秒未満の持続時間を有する複数のバーストが、前記基板上への前記薄膜材料の前記パルスレーザー蒸着中、一秒当たりのレーザーパルス数及び平均レーザーパワーが一定のままとなるように、一のバースト繰り返しレートで生成される方法。 - 前記バーストの前記パルスは、500ps未満のパルス持続時間を有する、請求項1の方法。
- 各バーストは、2〜200個のパルスを含む、請求項1の方法。
- 個々のパルスの間の一の選択されたパルス分離は、1μs未満である、請求項1の方法。
- 前記薄膜材料は、ナノ粒子塊、ナノ粒子が埋め込まれたナノ複合材料フィルム、及び無粒子かつ無ドロップレットの平滑なフィルムを含む、請求項1の方法。
- 各バースト中のバーストパルス数及びパルス間のパルス分離、バースト繰り返しレート、並びに各パルスのパルスエネルギーを含むバーストパラメータを制御することによって、薄膜形態を選択することを含む、請求項1の方法。
- 前記薄膜材料は、金属、合金、酸化金属、窒化金属、フッ化金属、ヒ化金属、硫化金属、半導体、カーボン、ガラス、ポリマー、及び複合材料の一つ以上を含む、請求項1の方法。
- 前記薄膜材料は、アモルファス若しくは結晶相のマイクロ構造、又はアモルファス及び結晶相の両方の混合を有する、請求項1の方法。
- 前記薄膜材料は、異なるターゲット材料に対して交番に又は同時にアブレーションをすることによって形成された多材料の固溶体、ナノ複合材料又はスーパーラティス構造を含む、請求項1の方法。
- 基板上での材料合成のためのパルスレーザー蒸着システムであって、
基板マニピュレーターと、
ターゲットマニピュレーターと、
レーザーパルスのバーストを生成する手段であって、前記バーストの特性又は前記バーストのパルスの特性を制御する手段と、
前記バーストを相互作用領域に向けて指向させる光学システムと、
前記生成する手段に接続されたコントローラと
を含み、
前記システムは前記材料の物理的性質の制御可能な変更を提供し、
各バースト中のパルス数と前記バーストの繰り返しレートは、独立して制御され、
所定のパラメータ及び数マイクロ秒未満の持続時間を有する複数のバーストが、前記基板上への前記材料の前記パルスレーザー蒸着中、一秒当たりのレーザーパルス数及び平均レーザーパワーが一定のままとなるように、一のバースト繰り返しレートで生成されるシステム。 - 前記バースト中のパルスエネルギーとパルス数の一つ以上は、無粒子の薄膜を作成すべく前記合成材料上又は内の粒子数を制限するべく制御可能である、請求項10のシステム。
- 各バーストは、1kHz〜10MHzの範囲内のバースト繰り返しレートを有し、
前記バースト中のパルス繰り返しレートは1MHz〜1GHzの範囲内にあり、
隣接するバースト間の時間分離は、前記バースト内の任意の隣接するパルス間の時間間隔よりも大きい、請求項1の方法。
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US12/254,076 US20090246413A1 (en) | 2008-03-27 | 2008-10-20 | Method for fabricating thin films |
US12/254,076 | 2008-10-20 | ||
PCT/US2009/036789 WO2009148674A1 (en) | 2008-03-27 | 2009-03-11 | A method for fabricating thin films |
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US (1) | US20090246413A1 (ja) |
EP (1) | EP2274771B1 (ja) |
JP (1) | JP5690714B2 (ja) |
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