JP4708790B2 - 耐火繊維の3次元繊維構造体、これを調製する方法、および耐熱構造複合材料への適用 - Google Patents
耐火繊維の3次元繊維構造体、これを調製する方法、および耐熱構造複合材料への適用 Download PDFInfo
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- JP4708790B2 JP4708790B2 JP2004535598A JP2004535598A JP4708790B2 JP 4708790 B2 JP4708790 B2 JP 4708790B2 JP 2004535598 A JP2004535598 A JP 2004535598A JP 2004535598 A JP2004535598 A JP 2004535598A JP 4708790 B2 JP4708790 B2 JP 4708790B2
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Description
・巻型またはマンドレル上に巻き取る工程と;
・厚いフェルトを作る工程と;
・3次元的に織る、編む、または組む工程と;
・2次元(2D)織物で作られたプライで覆いまたは重ね、任意的に互いに結合させる工程とを含む。前記2D織物は、織布、一方向フィラメントのシート、異なる方向に重ね合わされた複数の一方向シートで作られた多方向シートであって、フェルトの層を、例えばニードリングまたはスティッチングによって一緒に結合させたもの、あるいはニードリングによって布またはシートに結合された自由な繊維の層で覆われた布またはシートを含む積層物であってもよい。
3D繊維構造体では、カーボンナノチューブを基体の繊維上で成長させることによって、繊維構造体の細孔内にカーボンナノチューブを分配させることができる。
・非常に強い機械的強度をもつ追加の強化用フィラメント要素を組み込む結果として、機械的性質の向上と;
・磨耗に対する抵抗性の向上と;
・熱伝導率の向上と
が得られる。
・耐火繊維の2次元プライをカーボンナノチューブの成長のための少なくとも1種の触媒を含む組成物で含浸させる工程と;
・複数の含浸された2次元プライを重ねて一緒に結合することによって3次元基体を形成する工程と;
・カーボンナノチューブを3次元基体内に成長させる工程と
を含む。
a) 耐火繊維の2次元プライをカーボンナノチューブの成長のための少なくとも1種の触媒を含む組成物で含浸させる工程と;
b) カーボンナノチューブを2次元プライ内に成長させる工程と;
c) 耐火繊維の2次元プライを重ねて一緒に結合することによって3次元繊維構造を形成する工程であって、少なくとも一部のプライが工程a)およびb)によって得られたカーボンナノチューブを含む工程と
を含む。
・耐火繊維の3次元基体をつくる工程と;
・カーボンナノチューブの成長のための少なくとも1種の触媒を含む組成物に含浸させる工程と;
・カーボンナノチューブを3次元基体内に成長させる工程と
を含む。
1200℃以下の温度で炭化処理を受けたセルロース前駆体で作られた炭素布プライを、硝酸鉄の0.2モル水溶液中に含浸させた。このように含浸した20枚のプライを互いに重ね合わせてニードリング処理を施した。文献US 4 790 052に記載されているように、ニードリングは、針が実質的に一定の深さまで貫通することを保証するために、積み重ねるパイルの数を増加させながら除々に行った。
例1と同じ種類のセルロース前駆体の炭素布プライを、硝酸鉄の0.05モル水溶液に含浸した。
布プライを硝酸ニッケルの0.2モル水溶液に含浸させ、カーボンナノチューブ成長の時間を2時間から10時間に延長したことを除き、例2と同じ手順を行った。布プライをカーボンナノチューブに富ませた後に測定された重量増加分は約175%であった。
PAN前駆体からの炭素の布プライをアセトンで処理して炭素繊維の油みを除去し、硝酸ニッケルの0.2モル水溶液に含浸させた。
例1に使用した種類のセルロース前駆体の布プライを重ね合せてニードリングによって一緒に結合させた。ニードリングは文献US 4 790 052に記載されているように、針の実質的な一定の貫通深さを維持するために、プライが積み重ねられる間に除々に行われる。
PAN前駆体糸からの炭素のシートによって構成されたプライを重ね、積み重ねを行いながらニードリングによって除々に一緒に結合させた。前記シートは、例えば文献WO 98/44183に記載されたように、非連続的な炭素繊維で作られた幾つかの一方向シートを、異なる方向に重ね合せ一緒に結合させて作った多方向シートである。ニードリングはプライを積み重ねる間に除々に行い、針が実質的に一定の貫通深さをもつことを確実にした(文献US 4 790 052に記載)。
金属触媒の良好な分布を促進するために、PAN前駆体からの高強度の炭素繊維布プライに、酸素プラズマによる表面処理を3分間にわたって施し、硝酸ニッケルの0.2モル水溶液中に含浸させた。
PAN前駆体からの高強度の炭素繊維布プライに、アルゴンプラズマによる表面処理を5分間にわたって施し、硝酸コバルトの0.1モルエタノール溶液に含浸させた。
ニードルされた3次元炭素繊維基体をリング形状に成形した。各基体は、外径150ミリメートル(mm)、内径80mm、厚さ40mm、繊維体積含量22%(すなわち、基体の22%の見かけの体積が実際に繊維によって占められている)、重量180グラム(g)である。このような基体は、特に文献US 4 790 052に記載されているように2Dプライを一緒に重ねてニードリングすることによって形成された繊維構造体を切り取ることによって得ることができる。
Claims (27)
- 炭素繊維またはセラミック繊維の間に空隙として細孔を有する、前記繊維の一体性のある多孔性基体を含む多孔性繊維構造体を作る方法であって、
前記繊維基体の細孔に位置する前記繊維上に成長するカーボンナノチューブが前記繊維基体の細孔内に分配され、当該カーボンナノチューブで前記繊維基体の細孔を細分化する、カーボンナノチューブに富んだ炭素繊維またはセラミック繊維の基体で作られる前記繊維構造体を得るように、少なくとも1種の触媒を含む組成物で前記基体を含浸させた後、前記基体の炭素繊維またはセラミック繊維上にカーボンナノチューブを成長させることによってカーボンナノチューブを繊維構造体内に組み込むことを特徴とする方法。 - ・カーボンナノチューブ成長のための少なくとも1種の触媒を含む組成物で炭素繊維またはセラミック繊維のプライを含浸させること、
・複数の含浸されたプライを一緒に重ね合せて結合させることによって基体を形成すること、
・カーボンナノチューブを多孔性基体内に成長させること
の連続工程を含むことを特徴とする請求項1に記載の方法。 - ニードリングによってプライを一緒に結合させることを特徴とする請求項2に記載の方法。
- a) カーボンナノチューブ成長のための少なくとも1種の触媒を含む組成物で炭素繊維またはセラミック繊維のプライを含浸させること、
b) カーボンナノチューブをプライ内で成長させること、
c) 炭素繊維またはセラミック繊維のプライであって、少なくとも一部のプライが工程a)およびb)によって得られたカーボンナノチューブを含んでいるプライを一緒に重ね合せて結合することによって繊維構造体を形成すること
の連続工程を含むことを特徴とする請求項1に記載の方法。 - カーボンナノチューブの含量を変化させたプライを積み重ねて繊維構造体を形成することを特徴とする請求項4に記載の方法。
- ニードリングによって前記プライを一緒に結合させることを特徴とする請求項4または5に記載の方法。
- ・炭素繊維またはセラミック繊維の基体を作ること;
・カーボンナノチューブ成長のための少なくとも1種の触媒を含む組成物で前記基体を含浸させること;
・カーボンナノチューブを前記基体内で成長させること
の連続工程を含むことを特徴とする請求項1に記載の方法。 - 基体を作る工程がプライを一緒に重ね合せて結合させる工程を含むことを特徴とする請求項7に記載の方法。
- プライをニードリングによって一緒に結合させることを特徴とする請求項8に記載の方法。
- 炭素繊維またはセラミック繊維の基体を、織り、編み、または組むことによって作ることを特徴とする請求項7に記載の方法。
- 10m2/g以上の比表面積をもつ炭素繊維またはセラミック繊維上にカーボンナノチューブを成長させるための少なくとも1種の触媒を含む組成物を使用して含浸を行うことを特徴とする請求項2ないし10のいずれか1項に記載の方法。
- 10m2/g以上の比表面積を与えるように、空気もしくは蒸気および/または二酸化炭素の酸化によって、或いは酸攻撃によって炭素繊維またはセラミック繊維上に表面処理を施すことを特徴とする請求項2ないし10のいずれか1項に記載の方法。
- カーボンナノチューブ成長のための触媒を構成する少なくとも1種の金属の塩の溶液を含む組成物で含浸を行うことを特徴とする請求項2ないし12のいずれか1項に記載の方法。
- カーボンナノチューブに富んだ繊維構造体を作った後に金属触媒の粒子を除去する工程を含むことを特徴とする請求項13に記載の方法。
- 繊維とこの繊維上に成長したカーボンナノチューブとを離し、遊離したカーボンナノチューブが前記繊維基体の細孔全体にわたり均一な態様で分布することを特徴とする請求項2ないし14のいずれか1項に記載の方法。
- 繊維構造体の少なくとも1つの表面部分の細孔に追加のカーボンナノチューブを導入することを特徴とする請求項1ないし15のいずれか1項に記載の方法。
- 液中のカーボンナノチューブの懸濁液を繊維構造体の表面にもたらすことによって追加のカーボンナノチューブを導入することを特徴とする請求項16に記載の方法。
- 繊維構造体を含む繊維プリフォームを作る工程と、前記プリフォームを耐火マトリックスで高密度化する工程とを含む耐熱構造複合材料部材を作る方法であって、前記プリフォームが請求項1ないし17のいずれか1項の方法に従って作られることを特徴とする方法。
- 炭素繊維またはセラミック繊維の間に空隙として細孔を有する多孔性基体を含む一体性のある繊維構造体であって、炭素繊維またはセラミック繊維の少なくとも一部の表面から伸びるカーボンナノチューブをさらに含み、前記細孔に位置する前記繊維から伸びる前記カーボンナノチューブを前記繊維基体の細孔内に分配し、当該カーボンナノチューブで前記繊維基体の細孔を細分化することを特徴とする構造体。
- ニードリングによって一緒に結合したプライで繊維構造体を作ることを特徴とする請求項19に記載の構造体。
- 複数の炭素繊維プライで形成される、炭素繊維の間に空隙として細孔を有する多孔性繊維基体を含み、プライがニードリングによって積層され、一緒に結合される、一体性のある炭素繊維構造体であって、前記繊維基体の炭素繊維表面から伸びるカーボンナノチューブをさらに含み、前記繊維基体の細孔に位置する炭素繊維から伸びる前記カーボンナノチューブを前記繊維基体の細孔内に分配し、当該カーボンナノチューブで前記繊維基体の細孔を細分化することを特徴とする構造体。
- 前記カーボンナノチューブは、前記基体の細孔内全体に亘って均一に分布されることを特徴とする請求項21記載の構造体。
- 前記カーボンナノチューブは、前記繊維構造体の重量の5重量%〜200重量%を構成することを特徴とする請求項19〜22のいずれか1項に記載の構造体。
- 前記カーボンナノチューブは、構造体の繊維にランダムに配置されていることを特徴とする請求項19〜23のいずれか1項に記載の構造体。
- 前記カーボンナノチューブは、繊維構造体の体積の全体に亘って実質的に均一な態様で分布することを特徴とする請求項19〜24のいずれか1項に記載の構造体。
- 前記ナノチューブの量は、繊維構造体の体積中で変化することを特徴とする請求項19〜24のいずれか1項に記載の構造体。
- 繊維構造体の形態にある繊維強化材と耐火マトリックスを含む耐熱構造複合材料部材であって、繊維構造体が請求項19ないし26のいずれか1項によるものであることを特徴とする構造体。
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FR0211302 | 2002-09-12 | ||
FR0211302A FR2844510B1 (fr) | 2002-09-12 | 2002-09-12 | Structure fibreuse tridimensionnelle en fibres refractaires, procede pour sa realisation et application aux materiaux composites thermostructuraux |
PCT/FR2003/002692 WO2004025003A2 (fr) | 2002-09-12 | 2003-09-11 | Structure fibreuse tridimensionnelle en fibres refractaires, procede pour sa realisation et application aux materiaux composites thermostructuraux. |
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JP2004535598A Expired - Lifetime JP4708790B2 (ja) | 2002-09-12 | 2003-09-11 | 耐火繊維の3次元繊維構造体、これを調製する方法、および耐熱構造複合材料への適用 |
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US (1) | US7384663B2 (ja) |
EP (1) | EP1537262B1 (ja) |
JP (1) | JP4708790B2 (ja) |
KR (1) | KR101155739B1 (ja) |
CN (1) | CN100412243C (ja) |
AU (1) | AU2003278301A1 (ja) |
BR (2) | BR0306301B1 (ja) |
CA (1) | CA2498808C (ja) |
FR (1) | FR2844510B1 (ja) |
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TW (1) | TWI287533B (ja) |
UA (1) | UA91322C2 (ja) |
WO (1) | WO2004025003A2 (ja) |
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EP1537262B1 (fr) | 2016-07-27 |
TWI287533B (en) | 2007-10-01 |
BR132013033859E2 (pt) | 2015-03-03 |
WO2004025003A2 (fr) | 2004-03-25 |
KR101155739B1 (ko) | 2012-06-12 |
BR0306301A (pt) | 2004-09-08 |
BR0306301B1 (pt) | 2014-11-25 |
CA2498808C (en) | 2011-05-03 |
RU2005106198A (ru) | 2005-11-10 |
AU2003278301A1 (en) | 2004-04-30 |
UA91322C2 (ru) | 2010-07-26 |
AU2003278301A8 (en) | 2004-04-30 |
BR132013033859E8 (pt) | 2017-03-01 |
EP1537262A2 (fr) | 2005-06-08 |
CN100412243C (zh) | 2008-08-20 |
KR20050042194A (ko) | 2005-05-04 |
FR2844510B1 (fr) | 2006-06-16 |
CA2498808A1 (en) | 2004-03-25 |
FR2844510A1 (fr) | 2004-03-19 |
WO2004025003A3 (fr) | 2004-05-06 |
RU2324597C2 (ru) | 2008-05-20 |
JP2005538026A (ja) | 2005-12-15 |
CN1694981A (zh) | 2005-11-09 |
TW200418744A (en) | 2004-10-01 |
US7384663B2 (en) | 2008-06-10 |
US20050176329A1 (en) | 2005-08-11 |
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