JP2012500905A - シリコン含有ダイヤモンド状炭素薄膜、その製造方法、及びその用途 - Google Patents
シリコン含有ダイヤモンド状炭素薄膜、その製造方法、及びその用途 Download PDFInfo
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
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- C—CHEMISTRY; METALLURGY
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Abstract
Description
1.Si含有DLC薄膜の製造
図1に示すRF−PACVD装置を使用して基板17の表面にSi含有DLC薄膜を形成した。以下、具体的な手順を説明する。
前記1.で得られたSi−DLC薄膜を図1に示す反応器に入れ、酸素、窒素、水素及びCF4プラズマでそれぞれ10分間表面処理した。表面処理した試片の表面エネルギーを分析するために純水との接触角を測定した結果を図2に示す。プラズマ処理時のバイアス電圧は−400V、圧力は1.33Paであった。
Si含有DLC薄膜と純粋なDLC薄膜の耐腐食特性を確認するために、生体材料として広く使用されるTi−6Al−4V基板に、Si含有DLC薄膜と純粋なDLC薄膜をそれぞれバイアス電圧−400Vでコーティングし、動電位分極試験を実施した。ここで、使用されたSi含有DLC薄膜のSi含量は2at.%であった。
図7は、Si−OとC−O結合の効果をそれぞれ調べるために、純粋な非晶質Si薄膜をコーティングして酸素プラズマ処理した試料と、純粋な非晶質炭素薄膜をコーティングして酸素プラズマ処理した試料での血小板の吸着程度を比較した結果である。各試料はSi−O結合とC−O結合のいずれか一方のみを有する。酸素プラズマ処理した炭素薄膜に比べて酸素プラズマ処理したSi薄膜において血小板の吸着が著しく減少したが、これは、薄膜表面のSi−O結合が血液適合性の向上に大きく寄与することを示す。従って、酸素プラズマで処理すると血液適合性が著しく向上するのは、表面に存在するSi−O結合のためであることが確認された。
1.DLC薄膜の製造
蒸着前に基板をアルゴンイオンビームを利用して0.49Pa、−400Vで15分間洗浄した。Si−DLC薄膜がよく吸着されるようにするために、基板に初期バッファ層として非晶質シリコン(a−Si)をDLC薄膜と基板間に蒸着した。
(1)ぬれ角測定
イオンビーム処理後、20日間各試片のぬれ角を蒸留水を利用して測定した。ぬれ角測定前に窒素ガスで表面の埃を吹き飛ばし、5μLの蒸留水(純水の水滴)を試料表面に軽く滴下して測定した。ぬれ角を正確に観察するために、ぬれ角の測定後には測定した所を表示して、試料表面の同じ部分のぬれ角を再び測定しないようにした。これは、水で汚染された表面部位において再度ぬれ角を測定すると、正確な測定が行われないためである。ぬれ角の測定にはNRL Contact Angle Goniometerを利用した。基板の基準線を合わせて、純水の水滴を軽く滴下した後、角度計で測定した角度を読み、純水の水滴のぬれ角の写真を撮った。
AFM(Atomic Force Microscope)装置としてAutoprobe CP research system(Thermo Microscope Inc, USA)を使用して、ノンコンタクトモード(Non contact mode)で2μm×2μm領域の表面粗さを測定した。表面粗さはRMS(Root Mean Square)値を採用した。
図9の(a)及び(b)に示すように、イオンビーム処理を行っていないDLC薄膜とSi−DLC薄膜(Siの含量は2.66at%)のぬれ角は全て約76゜で類似しており、この条件でぬれ角は時間の経過に関係なく一定であった。
Claims (30)
- 内部及び表面にシリコンを含有するダイヤモンド状炭素薄膜の表面に、前記薄膜の表面に存在する炭素及びシリコン原子と前記薄膜の表面に親水性を付与する原子(A)間の化学結合を有する、シリコン含有ダイヤモンド状炭素薄膜。
- シリコンの含量が0.5〜17at.%である請求項1に記載のシリコン含有ダイヤモンド状炭素薄膜。
- シリコンの含量が1.0〜2.5at.%である請求項1に記載のシリコン含有ダイヤモンド状炭素薄膜。
- 表面粗さが10〜20nmである請求項3に記載のシリコン含有ダイヤモンド状炭素薄膜。
- 薄膜の表面に親水性を付与する原子(A)は、酸素又は窒素原子である請求項1に記載のシリコン含有ダイヤモンド状炭素薄膜。
- 前記原子(A)は酸素原子であり、前記薄膜の表面のSi−O結合は30〜60%である請求項1に記載のシリコン含有ダイヤモンド状炭素薄膜。
- 表面の接触角が0゜より大きく50゜以下である請求項1に記載のシリコン含有ダイヤモンド状炭素薄膜。
- 表面の接触角が0゜より大きく20゜以下である請求項1に記載のシリコン含有ダイヤモンド状炭素薄膜。
- 請求項1に記載のシリコン含有ダイヤモンド状炭素薄膜を含む医療用材料。
- 血管ステント、心臓弁、心臓ポンプ、人工血管、血液凝固抑制用病理実験室器材、又は血液保管器である請求項9に記載の医療用材料。
- 細胞又は生体の臓器を成長させるためのものである請求項9に記載の医療用材料。
- (a)基板の表面に、内部及び表面にシリコンを含有するダイヤモンド状炭素薄膜を形成する段階と、
(b)前記薄膜の表面を活性化し、前記薄膜の表面に存在する炭素及びシリコン原子を、前記薄膜の表面に親水性を付与する原子(A)と化学的に結合させる段階と
を含む、シリコン含有ダイヤモンド状炭素薄膜の製造方法。 - 前記段階(a)では、プラズマCVD法、プラズマ合成法、スパッタリング合成法、磁気ろ過アーク合成法、及びイオンビーム合成法のいずれか1つの方法で又はこれらの方法の2つ以上の組み合わせで薄膜を形成する請求項12に記載のシリコン含有ダイヤモンド状炭素薄膜の製造方法。
- 前記段階(a)で形成されるシリコン含有ダイヤモンド状炭素薄膜のシリコンの含量が0.5〜17at.%である請求項12に記載のシリコン含有ダイヤモンド状炭素薄膜の製造方法。
- 前記段階(a)で形成されるシリコン含有ダイヤモンド状炭素薄膜のシリコンの含量が1.0〜2.5at.%である請求項12に記載のシリコン含有ダイヤモンド状炭素薄膜の製造方法。
- 前記段階(b)では、プラズマ又はイオンビーム処理して薄膜の表面を活性化する請求項12に記載のシリコン含有ダイヤモンド状炭素薄膜の製造方法。
- 前記プラズマ処理時のチャンバ内の圧力は0.1〜10Paであり、バイアス電圧は−100〜−800Vである請求項16に記載のシリコン含有ダイヤモンド状炭素薄膜の製造方法。
- 前記イオンビーム処理時の圧力は1.0×10-7〜10Paであり、電圧は100V〜50.0kVである請求項16に記載のシリコン含有ダイヤモンド状炭素薄膜の製造方法。
- 段階(b)で得られる薄膜の表面粗さが10〜20nmである請求項12に記載のシリコン含有ダイヤモンド状炭素薄膜の製造方法。
- 前記薄膜の表面に親水性を付与する原子(A)は、酸素又は窒素原子である請求項12に記載のシリコン含有ダイヤモンド状炭素薄膜の製造方法。
- 段階(b)で得られる薄膜の表面の接触角が0゜より大きく50゜以下である請求項12に記載のシリコン含有ダイヤモンド状炭素薄膜の製造方法。
- 段階(b)で得られる薄膜の表面の接触角が0゜より大きく20゜以下である請求項12に記載のシリコン含有ダイヤモンド状炭素薄膜の製造方法。
- 前記基板は、血管ステント、心臓弁、心臓ポンプ、人工血管、血液凝固抑制用病理実験室器材、又は血液保管器である請求項12に記載のシリコン含有ダイヤモンド状炭素薄膜の製造方法。
- 前記基板は、ガラス、鏡、又はシリコン基板である請求項12に記載のシリコン含有ダイヤモンド状炭素薄膜の製造方法。
- 内部及び表面にシリコンを含有するシリコン含有ダイヤモンド状炭素薄膜の表面を酸素プラズマ、窒素プラズマ、又はイオンビームで処理して、前記薄膜の表面にSi−N又はSi−O結合を生成させることを含む、シリコン含有ダイヤモンド状炭素薄膜の血液適合性の向上方法。
- 内部及び表面にシリコンを含有するシリコン含有ダイヤモンド状炭素薄膜の表面を酸素プラズマ、窒素プラズマ、又はイオンビームで処理して、前記薄膜の表面にSi−N又はSi−O結合を生成させることを含む、シリコン含有ダイヤモンド状炭素薄膜の親水性の付与方法。
- シリコン含有ダイヤモンド状炭素薄膜のシリコンの含量は0.5〜17at.%である請求項25又は26に記載の方法。
- 内部及び表面にシリコンを含有するシリコン含有ダイヤモンド状炭素薄膜の表面を酸素プラズマで処理して、前記薄膜の表面にSi−O結合を生成させることを含む、シリコン含有ダイヤモンド状炭素薄膜の親水性の半永久的維持方法。
- シリコン含有ダイヤモンド状炭素薄膜のシリコンの含量は1.0〜2.5at.%である請求項28に記載の方法。
- 鏡、ガラス、又はシリコンの表面に請求項1に記載のシリコン含有ダイヤモンド状炭素薄膜を形成して前記表面の曇りを防止する方法。
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WO2015115399A1 (ja) * | 2014-01-28 | 2015-08-06 | 太陽化学工業株式会社 | 炭素膜を備える構造体及び炭素膜を形成する方法 |
WO2016056466A1 (ja) * | 2014-10-05 | 2016-04-14 | 太陽誘電ケミカルテクノロジー株式会社 | 抗菌積層構造体及びその製造方法 |
KR102041387B1 (ko) * | 2019-04-25 | 2019-11-07 | (주)씨에스메탈 | Dlc 코팅 도마 및 그의 제조방법 |
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JP6031441B2 (ja) * | 2011-07-28 | 2016-11-24 | テルモ株式会社 | 赤血球保存容器 |
US9925295B2 (en) | 2012-05-09 | 2018-03-27 | Amedica Corporation | Ceramic and/or glass materials and related methods |
CN105821386B (zh) * | 2015-10-07 | 2018-06-08 | 重庆工业职业技术学院 | 具有抗凝血功能的人工心脏瓣膜瓣叶涂层材料的制备方法 |
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