JP2010514937A - プラズマ蒸着微孔性炭素材料 - Google Patents
プラズマ蒸着微孔性炭素材料 Download PDFInfo
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- 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
- C23C16/26—Deposition of carbon only
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- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—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 method of coating
- C23C16/52—Controlling or regulating the coating process
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- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02612—Formation types
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- H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
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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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- Y10T428/00—Stock material or miscellaneous articles
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- Y10T428/249978—Voids specified as micro
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/30—Self-sustaining carbon mass or layer with impregnant or other layer
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
- Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
- Y10T442/608—Including strand or fiber material which is of specific structural definition
- Y10T442/614—Strand or fiber material specified as having microdimensions [i.e., microfiber]
- Y10T442/624—Microfiber is carbon or carbonaceous
Abstract
Description
圧力:666.6mPa(5ミリトル)
RF電力:1000ワット
DC自己バイアス電圧:−1052ボルト
処理時間:45秒
無秩序共有結合網状組織炭化水素フィルムの蒸着:アルゴンプラズマ中における基材のプライミング後、1,3−ブタジエンガスを真空チャンバに供給することにより、炭化水素フィルムをプラズマ蒸着した。プラズマ蒸着条件は、以下のとおりである。
処理圧力:2.67Pa(20ミリトル)
RF電力:100ワット
DC自己バイアス電圧:−260〜−192ボルト
蒸着時間:16分
操作完了後、厚さ900nmのプラズマ蒸着炭化水素フィルムが、ケイ素ウエファー上に得られた。
マルチポイントBET……………………6.372E+02m2/g
t法 外部表面積………………………………1.732E+02m2/g
t法 微小孔表面積………………………………4.640E+02m2/g
NLDFT法 累積表面積…………………………6.034E+02m2/g
間隙体積データ
直径を有する孔の全間隙体積
P/P0=0.99623において5055.7Å未満……3.518E−01cc/g
t法 微小間隙体積………………………1.415E−01cc/g
SF法 累積間隙体積………………………2.557E−01cc/g
NLDFT法 累積間隙体積………………………3.056E−01cc/g
孔径データ
SF法 孔径(モード)………………………8.490E+00Å
NLDFT法 孔径(モード)………………………6.272E+00Å
実施例3(ナノ多孔性炭素フィルムの光学的特性):微孔性(すなわち、ナノ多孔性)炭素材料フィルムを可変角度分光偏光解析法(Variable Angle Spectroscopic Ellipsometery)(VASE)で特徴付け、電力を50ワットに維持し、様々な蒸着時間(試料82は32分、試料83は24分、試料84は16分)以外は実施例1に従って作製された3種の異なるフィルムの多孔率を推定した。屈折率の実数部及び虚数部をそれぞれ図6及び図7に示す。厚さ及び多孔性を以下の表にまとめる。
酸素流量:500sccm
圧力:3.33Pa(25ミリトル)
RF電力:2000ワット
処理時間:30秒
炭化水素フィルムの蒸着:アルゴンプラズマ中における基材のプライミング後、ブタンガスを真空チャンバに供給することにより、異なる厚さのプラズマ蒸着炭化水素フィルムを蒸着した。蒸着条件は、以下のとおりである。
処理圧力:13.33Pa(100ミリトル)
RF電力:2000ワット、90msで時間どおりにパルス駆動、デューティーサイクル90%
蒸着時間:2分50秒(試料66)
操作完了後、厚さ400〜500nm程度の炭化水素フィルムが得られた。これらを以下の条件で焼きなましした。
圧力:679.9Pa(5.1トル)
焼きなまし温度:520℃
焼きなまし時間:20分及び60分(「L」と付けた試料)
これら微孔性(すなわち、ナノ多孔性)炭素材料フィルムの検知反応を、トルエンについて図11に、MEKについて図12に、IPAについて図13に、85%RHのエチレンベンゼンについて図14に示す。エチルベンゼン試験については、気流85%RHに加湿し、エチルベンゼンを気流に導入する前に新たにスペクトルのベースラインを確立した。
酸素流量: 500sccm
圧力: 3.33Pa(25ミリトル)
RF電力: 3000ワット
処理時間: 30秒
プラズマ蒸着炭化水素フィルムの蒸着:酸素プラズマ中における基材のプライミング後、ブタンガスを真空チャンバに供給することにより、異なる厚さのプラズマ蒸着炭化水素フィルムを蒸着した。蒸着条件は、以下のとおりである。
処理圧力: 6.67Pa(50ミリトル)
RF電力: 3000ワット、90msで時間どおりにパルス駆動、デューティーサイクル90%
蒸着時間: 190秒
操作完了後、厚さ435nmのフィルムが得られた。この炭化水素フィルムを以下の条件で焼きなましした。
圧力: 693.2Pa(5.2トル)
焼きなまし温度: 500℃
焼きなまし時間: 20分
これらナノ多孔性炭素フィルムの検知反応を、上記実施例4に記載の方法で測定した。試料158Bは、低濃度のトルエン、メチルエチルケトン、イソプロパノール、及びアセトンに対して感受性があった(図20)。蒸気濃度が上昇すると、ピーク波長が赤方にシフトし、これは試料の光学的厚さの増加を示す。これらすべての蒸気について、波長シフトはTLV(許容限界濃度)において10nm以上である。
Claims (13)
- 0.1〜10ナノメートルの平均孔径を有し、そして1マイクロメートル超の孔を実質的に含まない多孔性炭素骨格を含んでなる、微孔性炭素材料。
- 前記多孔性炭素骨格が、1〜10ナノメートルの平均孔径を有し、そして100ナノメートル超の孔を実質的に含まない、請求項1に記載の微孔性炭素材料。
- 前記多孔性炭素骨格が、本質的に炭素からなり、10%以上の多孔率を有し、そして1未満の実効消光率を有する、請求項1に記載の微孔性炭素材料。
- 基材層と、
前記基材層上に配置された微孔性炭素骨格層とを含む物品であって、前記微孔性炭素骨格が0.1〜10ナノメートルの平均孔径を有し、そして1マイクロメートル超の孔を実質的に含まない物品。 - 前記基材層が、ガス透過性層である、請求項4に記載の物品。
- 前記微孔性炭素骨格が、1〜10ナノメートルの平均孔径を有し、そして100ナノメートル超の孔を実質的に含まない、請求項4に記載の物品。
- 前記微孔性炭素材料が、濾過層、ガス分離層、又はウイルス分離層を生成させる、請求項4に記載の物品。
- 炭化水素ガスから炭化水素プラズマを生成させる工程と、
基材上に前記炭化水素プラズマを堆積させて、炭化水素層を生成させる工程と、
前記炭化水素層を加熱し、そして前記水素の少なくとも一部を除去して、微孔性炭素材料を生成させる工程と、
を含んでなる、微孔性炭素材料の生成方法。 - 前記炭化水素プラズマを生成させる工程が、(C1〜C10)アルカン、(C1〜C10)アルケン、又は(C1〜C10)アルキン炭化水素ガスから炭化水素プラズマを生成させる工程を含む、請求項8に記載の方法。
- 前記炭化水素プラズマを生成させる工程が、ブタン又はブタジエン炭化水素ガスから炭化水素プラズマを生成させる工程を含む、請求項8に記載の方法。
- 前記加熱する工程が、前記炭化水素層を加熱し、前記水素の少なくとも一部を除去して、微孔性炭素材料を生成させる工程を含み、前記微孔性炭素材料が本質的に炭素からなる、請求項8に記載の方法。
- 前記堆積させる工程が、負のバイアス電圧又は負の自己バイアス電圧を有する基材上に前記炭化水素プラズマを堆積させて、炭化水素層を生成させる工程を含む、請求項8に記載の方法。
- 前記加熱する工程が、アンモニア雰囲気下で前記炭化水素層を加熱し、そして前記水素の少なくとも一部を除去して、1〜10ナノメートルの平均孔径を有し、そして100ナノメートル超の孔を実質的に含まない微孔性炭素材料を生成させる工程を含む、請求項8に記載の方法。
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Application Number | Priority Date | Filing Date | Title |
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US11/618,010 US7901776B2 (en) | 2006-12-29 | 2006-12-29 | Plasma deposited microporous carbon material |
PCT/US2007/087347 WO2008082897A1 (en) | 2006-12-29 | 2007-12-13 | Plasma deposited microporous carbon material |
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JP2010514937A true JP2010514937A (ja) | 2010-05-06 |
JP2010514937A5 JP2010514937A5 (ja) | 2011-01-20 |
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US (1) | US7901776B2 (ja) |
EP (1) | EP2111481A1 (ja) |
JP (1) | JP2010514937A (ja) |
KR (1) | KR20090101289A (ja) |
CN (1) | CN101573470B (ja) |
BR (1) | BRPI0720568A2 (ja) |
WO (1) | WO2008082897A1 (ja) |
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- 2007-12-13 KR KR1020097015815A patent/KR20090101289A/ko not_active Application Discontinuation
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BRPI0720568A2 (pt) | 2014-02-04 |
KR20090101289A (ko) | 2009-09-24 |
WO2008082897A1 (en) | 2008-07-10 |
CN101573470B (zh) | 2011-08-03 |
CN101573470A (zh) | 2009-11-04 |
US7901776B2 (en) | 2011-03-08 |
EP2111481A1 (en) | 2009-10-28 |
US20080160858A1 (en) | 2008-07-03 |
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