JP5830471B2 - 平行に配列されたカーボン・ナノチューブを含むカーボン・ナノチューブ導入繊維材料の生産方法 - Google Patents
平行に配列されたカーボン・ナノチューブを含むカーボン・ナノチューブ導入繊維材料の生産方法 Download PDFInfo
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- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- D10B2101/00—Inorganic fibres
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- D10B2101/122—Nanocarbons
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- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2913—Rod, strand, filament or fiber
- Y10T428/2933—Coated or with bond, impregnation or core
Description
本出願は、米国特許法第119条に基づき、2010年2月2日出願の米国仮特許出願第61/300,783号の優先権の利益を主張するものであり、その内容は、参照により全体を本明細書に組み込むものとする。本出願は、また、すべて2009年11月2日出願の米国特許出願第12/611,073号、第12/611,101号、及び2010年11月2日出願の第12/938,328号にも関連し、これらの内容はそれぞれ参照により全体を本明細書に組み込むものとする。
該当なし。
当該技術分野で既知の標準的なカーボン・ナノチューブ合成反応器は横断面が円形である。これには、例えば、歴史的理由(研究所では円筒状の反応器がよく用いられる)及び利便性(流体力学は円筒状の反応器にモデル化すると容易になり、また、加熱器システムは円管チューブ(石英など)に容易に対応する)、並びに製造の容易性などの多くの理由がある。本開示は、従来の円筒形状を変えて、矩形横断面を有するカーボン・ナノチューブ合成反応器を提供する。変更の理由は以下の通りである。
比較的低温のパージゾーンを提供するチャンバーは、矩形合成反応器の両端から延びる。出願人は、仮に高温ガスが外部環境(即ち、反応器の外部)と接触(mix)すると、繊維材料の劣化(degradation)が増加すると、結論を下した。低温パージゾーンは、内部システムと外部環境間の緩衝となる。当該技術分野で既知のカーボン・ナノチューブ合成反応器の構成では、通常、基材を慎重に(かつ緩やかに)冷却することが求められる。本発明の矩形カーボン・ナノチューブ成長反応器の出口における低温パージゾーンは、連続的なインライン処理に必要とされるような短時間の冷却を実現する。
ある実施形態では、金属製ホットウォール型(hot-walled)反応器(例えば、ステンレス鋼)が用いられる。金属、特にステンレス鋼が炭素の付着(即ち、煤及び副生成物の形成)を受けやすいために、この種類の反応器の使用は常識に反するようにも考えられる。従って、大部分のカーボン・ナノチューブ合成反応器は、炭素の付着が殆どないため、また、石英は洗浄し易く、また試料の観察が容易であるため、石英から作られる。しかしながら、出願人は、ステンレス鋼上における煤及び炭素付着物が増加することにより、より着実、より効率的、より高速、かつ、より安定的なカーボン・ナノチューブ成長がもたらされるということを発見した。理論に拘束されるものではないが、大気圧運転(atmospheric operation)と連動して、反応器内で起こるCVDプロセスでは拡散が制限されることが示されている。即ち、カーボン・ナノチューブ形成触媒に「過度に供給される(overfed)」、つまり、過量の炭素が、(反応器が不完全真空下で運転している場合よりも)その相対的に高い分圧により反応器システム内で得られる。結果として、開放システム(特に清浄なもの)では、過量の炭素がカーボン・ナノチューブ形成触媒の粒子に付着して、カーボン・ナノチューブの合成能力を低下させる。ある実施形態では、反応器に「汚れが付いて(dirty)」いる、即ち、金属反応器壁に煤が付着している状態の場合に、矩形反応器を意図的に運転する。炭素が反応器壁上の単分子層に付着すると、炭素は、それ自体を覆って付着し易くなる。得られる炭素の中には、この機構により「回収される(withdrawn)」ものがあるので、ラジカルの形で残っている炭素原料が、カーボン・ナノチューブ形成触媒を被毒させない速度でこの触媒と反応する。既存のシステムでは「清浄に(cleanly)」運転するが、これは連続処理のために開放状態であれば、減速した成長速度で、はるかに低い収率でしかカーボン・ナノチューブを生産できないことになる。
本明細書に開示されたカーボン・ナノチューブ合成反応器において、触媒還元及びカーボン・ナノチューブ成長のいずれもが反応器内で起こる。還元工程が個別の工程として実施されると、連続プロセスに用いるものとして十分タイムリーに行えなくなるため、このことは重要である。当該技術分野において既知の標準的なプロセスにおいて、還元工程の実施には、通常1〜12時間かかる。本開示によれば、両工程は1つの反応器内で生じるが、これは、少なくとも1つには、炭素含有原料ガスを導入するのが、円筒状反応器を用いる当該技術分野では標準的となっている反応器の端部ではなく、中心部であることに起因する。還元プロセスは、繊維が加熱ゾーンに入ったときに行われる。この時点に至るまでに、ガスには、触媒を(水素ラジカルの相互作用を介して)還元する前に反応器壁と反応して冷える時間があるということである。還元が起こるのは、この移行領域である。システム内で最も高温の等温ゾーンでカーボン・ナノチューブの成長は起こり、反応器の中心近傍におけるガス入口の近位で最速の成長速度が生じる。
Claims (11)
- 繊維材料と、該繊維材料に導入されて前記繊維材料の表面に垂直に配列されたカーボン・ナノチューブとを含むカーボン・ナノチューブ導入繊維材料を提供することと、
前記繊維材料の長手軸に平行に配列された前記繊維材料に導入されたカーボン・ナノチューブの層を形成するように、前記垂直に配列されたカーボン・ナノチューブを再配向することと、
を含み、
前記垂直に配列された前記繊維材料に導入されたカーボン・ナノチューブの少なくとも一部を、相互に、前記繊維材料に又はその両方に架橋結合することを、さらに含む方法。 - 架橋結合は、共有結合又はπ‐スタッキング相互作用を含む請求項1に記載の方法。
- 架橋ポリマーは、前記垂直に配列された前記繊維材料に導入されたカーボン・ナノチューブと前記π‐スタッキング相互作用を形成する請求項2に記載の方法。
- 前記繊維材料の長手軸に平行に配列された前記カーボン・ナノチューブが形成された前記カーボン・ナノチューブ導入繊維材料をマトリックス材料内に配置することを、さらに含む請求項3に記載の方法。
- 再配向は、機械的プロセス又は化学的プロセスを含む請求項1に記載の方法。
- 前記平行に配列された前記繊維材料に導入されたカーボン・ナノチューブの層の上に触媒ナノ粒子を付着させることと、
前記平行に配列された前記繊維材料に導入されたカーボン・ナノチューブの層の上に追加のカーボン・ナノチューブを成長させることと、
前記繊維材料の長手軸に平行に配列されるように前記追加のカーボン・ナノチューブを配向することと、
をさらに含む請求項1に記載の方法。 - 前記追加のカーボン・ナノチューブの少なくとも一部を、前記平行に配列された前記繊維材料に導入されたカーボン・ナノチューブの少なくとも一部に、相互に又はその両方に架橋結合することを、さらに含む請求項6に記載の方法。
- 連続繊維材料を提供することと、
電界又は磁界の存在下で、前記連続繊維材料上にカーボン・ナノチューブの層を成長させることと、
を含み、
前記繊維材料と該繊維材料に導入されて前記繊維材料の表面に垂直に配列されたカーボン・ナノチューブとを含むカーボン・ナノチューブ導入繊維材料を形成するように、前記カーボン・ナノチューブを前記連続繊維材料に導入し、
前記垂直に配列された前記繊維材料に導入されたカーボン・ナノチューブの少なくとも一部を、相互に、前記繊維材料に又はその両方に架橋結合させ、
前記繊維材料に導入されたカーボン・ナノチューブが前記繊維材料の長手軸に平行に配列されるように、前記電界又は前記磁界の方向を合わせる方法。 - 前記平行に配列された前記繊維材料に導入されたカーボン・ナノチューブの少なくとも一部を、相互に、前記繊維材料に又はその両方に架橋結合することを、さらに含む請求項8に記載の方法。
- 繊維材料と、該繊維材料に導入されて前記繊維材料の表面に垂直に配列されたカーボン・ナノチューブとを含むカーボン・ナノチューブ導入繊維材料を提供することと、
架橋結合して垂直に配列された前記繊維材料に導入されたカーボン・ナノチューブを形成するために、前記カーボン・ナノチューブ導入繊維材料に架橋ポリマーを添加することと、
を含み、
前記架橋ポリマーは、前記架橋結合して垂直に配列された前記繊維材料に導入されたカーボン・ナノチューブとπ‐スタッキング相互作用を形成し、さらに、
前記繊維材料の長手軸に平行に配列された架橋導入カーボン・ナノチューブ層を形成するように、前記架橋結合して垂直に配列された前記繊維材料に導入されたカーボン・ナノチューブを再配向することを含む方法。 - 連続カーボン・ナノチューブ成長プロセスであって、
連続繊維材料を提供することと、
連続カーボン・ナノチューブ成長プロセスで前記連続繊維材料上にカーボン・ナノチューブを成長させることと、
を含み、
前記カーボン・ナノチューブがカーボン・ナノチューブ導入繊維材料を形成するように、前記繊維材料に導入され、さらに、
前記繊維材料に導入されたカーボン・ナノチューブの少なくとも一部を、相互に、前記繊維材料に又はその両方に架橋結合することを含み、
架橋結合は、架橋結合した前記繊維材料に導入されたカーボン・ナノチューブを形成するように、前記繊維材料に導入されたカーボン・ナノチューブとπ‐スタッキング相互作用を形成する架橋ポリマーで前記繊維材料に導入されたカーボン・ナノチューブを処理することを含み、さらに、
前記連続繊維材料の長手軸に平行に配列された架橋導入カーボン・ナノチューブ層を形成するように、機械的プロセス又は化学的プロセスによって前記架橋導入カーボン・ナノチューブを配向することを含む連続カーボン・ナノチューブ成長プロセス。
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US30078310P | 2010-02-02 | 2010-02-02 | |
US61/300,783 | 2010-02-02 | ||
PCT/US2011/023403 WO2011146151A2 (en) | 2010-02-02 | 2011-02-01 | Fiber containing parallel-aligned carbon nanotubes |
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US9005755B2 (en) | 2007-01-03 | 2015-04-14 | Applied Nanostructured Solutions, Llc | CNS-infused carbon nanomaterials and process therefor |
JP5577356B2 (ja) * | 2009-02-17 | 2014-08-20 | アプライド ナノストラクチャード ソリューションズ リミテッド ライアビリティー カンパニー | カーボン・ナノチューブを繊維上に含んで構成された複合材料 |
US20100227134A1 (en) | 2009-03-03 | 2010-09-09 | Lockheed Martin Corporation | Method for the prevention of nanoparticle agglomeration at high temperatures |
CN101837287B (zh) * | 2009-03-21 | 2012-05-30 | 清华大学 | 碳纳米管纳米颗粒复合材料的制备方法 |
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JP2013518791A (ja) | 2013-05-23 |
CN102741465A (zh) | 2012-10-17 |
EP2531558A2 (en) | 2012-12-12 |
AU2011256789A1 (en) | 2012-07-12 |
KR20120114396A (ko) | 2012-10-16 |
EP2531558A4 (en) | 2013-07-03 |
WO2011146151A3 (en) | 2012-01-19 |
EP2531558B1 (en) | 2018-08-22 |
US20110186775A1 (en) | 2011-08-04 |
CA2785803A1 (en) | 2011-11-24 |
US8999453B2 (en) | 2015-04-07 |
KR101906262B1 (ko) | 2018-10-10 |
BR112012018244A2 (pt) | 2016-05-03 |
WO2011146151A2 (en) | 2011-11-24 |
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