JP2013511467A - カーボンナノチューブ浸出繊維材料を含有するセラミック複合材料とその製造方法 - Google Patents
カーボンナノチューブ浸出繊維材料を含有するセラミック複合材料とその製造方法 Download PDFInfo
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- JP2013511467A JP2013511467A JP2012540163A JP2012540163A JP2013511467A JP 2013511467 A JP2013511467 A JP 2013511467A JP 2012540163 A JP2012540163 A JP 2012540163A JP 2012540163 A JP2012540163 A JP 2012540163A JP 2013511467 A JP2013511467 A JP 2013511467A
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- carbon nanotube
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Abstract
【選択図】図1
Description
本願は、2009年11月23日出願の米国仮特許出願第61/263,804号、及び、2009年12月1日出願の米国仮特許出願第61/265,718号に基づき、合衆国法典第35巻(35 U.S.C.)第119条に従って優先権を主張するものであり、参照により全内容が本明細書に組み込まれる。
適用なし。
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(すなわち、反応器の外部)と接触(mix)すると、繊維材料の劣化(degradation)が増加することを究明した。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。本願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。
ある実施形態において、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。この種類の反応器の使用は、金属、特にステンレス鋼が炭素の付着(すなわち、すす及び副生成物の形成)を受けやすいために、常識に反するようにも考えられる。したがって、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、石英は洗浄しやすく試料の観察を容易にするため、石英製である。しかしながら、出願人は、ステンレス鋼上におけるすす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こと、を見つけた。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。すなわち、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(clean)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。ある実施形態において、反応器に「汚れが付いて(dirty)」いる、すなわち、金属反応器壁にすす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やすくなる。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withdrawn)」ものがあるので、ラジカルの形で残っている炭素原料が、カーボンナノチューブ形成触媒を被毒させない速度でこの触媒と反応する。既存のシステムでは「清浄に(cleanly)」運転するが、連続処理のために開放状態であれば、減速した成長速度で、はるかに低い収率でしかカーボンナノチューブを生産できない。
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。
炭化ケイ素マトリックスの複合材料は、カーボンナノチューブ浸出炭素短繊維をコロイド処理することにより作製された。炭素短繊維は、前述の連続的な浸出プロセスにより作製された平均長さ55μmのカーボンナノチューブが浸出したGrafil社(Sacramento, CA)製34−700、12kフィラメントであった。その繊維は、3mmの長さに切断された。炭化ケイ素マトリックスの複合材料は、炭化ケイ素ナノ粒子及びバインダーのコロイド混合物(SiCナノ粒子+バインダー=50重量%)をカーボンナノチューブ浸出炭素短繊維(50重量%)と混合することにより作製された。炭化ケイ素ナノ粒子、バインダー及びカーボンナノチューブ浸出炭素繊維から得られた混合物は、試験タイル(test tile)のプレス金型内置かれた。バインダーを硬化させて未焼結のセラミックタイル(ceramic tile)を形成するために、混合物を含む金型は2500psiの圧力下で30分間175℃に加熱された。未焼結のセラミックタイルが硬化した後、その未焼結タイルは、最終的に炭化ケイ素粒子を焼結させるためにオーブン(oven)内に置かれた。1950℃で2時間加熱し、これにより3インチ×3.0インチ×0.25インチの試験タイルを形成した。結果的に、図4に示される、カーボンナノチューブ浸出炭素繊維の炭化ケイ素セラミックマトリックス複合材料は、十分に焼結され、100.04S/mの電気伝導度であった。
炭化ケイ素マトリックスの複合材料は、カーボンナノチューブ浸出炭素短繊維をコロイド処理することにより作製された。炭素短繊維は、前述の連続的な浸出プロセスにより作製された平均長さ55μmのカーボンナノチューブが浸出したGrafil社(Sacramento, CA)製34−700、12kフィラメントであった。その繊維は、3mmの長さに切断された。炭化ケイ素マトリックスの複合材料は、炭化ケイ素ナノ粒子及びバインダーのコロイド混合物(SiCナノ粒子+バインダー=90重量%)をカーボンナノチューブ浸出炭素短繊維(10重量%)と混合することにより作製された。炭化ケイ素ナノ粒子、バインダー及びカーボンナノチューブ浸出炭素繊維から得られた混合物は、試験タイルのプレス金型内置かれた。バインダーを硬化させて未焼結のセラミックタイルを形成するために、混合物を含む金型は2500psiの圧力下で30分間175℃に加熱された。未焼結のセラミックタイルが硬化した後、その未焼結タイルは、最終的に炭化ケイ素粒子を焼結させるためにオーブン内に置かれた。1950℃で1時間加熱し、これにより3インチ×3.0インチ×0.25インチの試験タイルを形成した。結果的に、図5に示される、カーボンナノチューブ浸出炭素繊維の炭化ケイ素セラミックマトリックス複合材料は、部分的に焼結され、5.45S/mの電気伝導度であった。
炭化ケイ素マトリックスの複合材料は、カーボンナノチューブ浸出炭素短繊維をコロイド処理することにより作製された。炭素短繊維は、前述の連続的な浸出プロセスにより作製された平均長さ55μmのカーボンナノチューブが浸出したGrafil社(Sacramento, CA)製34−700、12kフィラメントであった。その繊維は、3mmの長さに切断された。炭化ケイ素マトリックスの複合材料は、炭化ケイ素ナノ粒子及びバインダーのコロイド混合物(SiCナノ粒子+バインダー=75重量%)をカーボンナノチューブ浸出炭素短繊維(25重量%)と混合することにより作製された。炭化ケイ素ナノ粒子、バインダー及びカーボンナノチューブ浸出炭素繊維から得られた混合物は、試験タイルのプレス金型内置かれた。バインダーを硬化させて未焼結のセラミックタイルを形成するために、混合物を含む金型は2500psiの圧力下で30分間175℃に加熱された。未焼結のセラミックタイルが硬化した後、その未焼結タイルは、最終的に炭化ケイ素粒子を焼結させるためにオーブン内に置かれた。1950℃で2時間加熱し、これにより3インチ×3.0インチ×0.25インチの試験タイルを形成した。結果的に、カーボンナノチューブ浸出炭素繊維の炭化ケイ素セラミックマトリックス複合材料は、十分に焼結され、263.97S/mの電気伝導度であった。図6は、図1〜3に表されるカーボンナノチューブ浸出炭素繊維セラミックマトリックス複合材料において、カーボンナノチューブの不足したセラミックマトリックス複合材料と比較して、電気伝導度が向上していることを明示する棒グラフを示す。
Claims (48)
- セラミックマトリックスと、
カーボンナノチューブ浸出繊維材料と、
を含んで構成される複合材料。 - 前記セラミックマトリックスは、炭化ケイ素、炭化タングステン、炭化クロム、炭化チタン、窒化チタン、ホウ化チタン、酸化アルミニウム、窒化ケイ素、ムライト、SiCN、Fe2N及びBaTiO3からなるグループより選択される少なくとも1つの化合物を含んで構成される請求項1に記載の複合材料。
- 前記セラミックマトリックスはセメントを含んで構成される請求項1に記載の複合材料。
- 前記セメントは、ポルトランドセメント、ポゾラン−石灰セメント、スラグ−石灰セメント、高硫酸塩セメント、アルミン酸カルシウムセメント、スルホアルミン酸カルシウムセメント、炭化物ベースのセメント、耐火セメント、クロム−アルミナセメント、ニッケル−酸化マグネシウムと鉄−炭化ジルコニウムのセメント、及びこれらの組み合わせからなるグループより選択される請求項3に記載の複合材料。
- 前記ポルトランドセメントは、タイプIのポルトランドセメント、タイプIIのポルトランドセメント、タイプIIIのポルトランドセメント、タイプIVのポルトランドセメント、タイプVのポルトランドセメントからなるグループより選択される種類のポルトランドセメントである請求項4に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料は、ガラス繊維、炭素繊維、金属繊維、セラミック繊維、有機繊維、炭化ケイ素繊維、炭化ホウ素繊維、窒化ケイ素繊維、酸化アルミニウム繊維及びこれらの組み合わせからなるグループより選択される少なくとも1つの繊維種を含んで構成される請求項1に記載の複合材料。
- 少なくとも前記カーボンナノチューブ浸出繊維材料をオーバーコートする保護層を更に含んで構成される請求項1に記載の複合材料。
- 前記保護層は、前記カーボンナノチューブ浸出繊維材料のカーボンナノチューブもオーバーコートする請求項7に記載の複合材料。
- 前記保護層は、ニッケル、クロム、マグネシウム、チタン、銀、スズ、又は二ホウ化チタンを含んで構成される請求項7に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料の繊維材料は、短繊維及び連続繊維からなるグループより選択される請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料のカーボンナノチューブは、前記複合材料の約0.1重量%から約10重量%で構成される請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料のカーボンナノチューブは、前記カーボンナノチューブ浸出繊維材料の約0.5重量%から約40重量%で構成される請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料のうち、繊維材料とカーボンナノチューブの少なくとも1つが、セラミック前駆体物質と少なくとも部分的に反応して、これにより前記セラミックマトリックスの少なくとも一部を形成する請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料は、前記セラミックマトリックス中に均一に分布する請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料は、前記セラミックマトリックス中に不均一に分布する請求項1に記載の複合材料。
- 前記不均一に分布することには、前記セラミックマトリックス中における勾配分布が含まれる請求項15に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料を構成するカーボンナノチューブは、前記カーボンナノチューブ浸出繊維材料の長手軸に対して略垂直である請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料を構成するカーボンナノチューブは、前記カーボンナノチューブ浸出繊維材料の長手軸に対して略平行である請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料は炭化ケイ素繊維を含んで構成され、前記セラミックマトリックスは酸化アルミニウム及び窒化ケイ素からなるグループより選択される請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料は炭素繊維及び炭化ケイ素繊維からなるグループより選択され、前記セラミックマトリックスは炭化ケイ素を含んで構成される請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料を構成するカーボンナノチューブの重量百分率は、前記カーボンナノチューブの平均長さにより決定される請求項1に記載の複合材料。
- 前記カーボンナノチューブの前記重量百分率は、前記カーボンナノチューブ浸出繊維材料の繊維材料に浸出する前記カーボンナノチューブの被覆密度により更に決定される請求項21に記載の複合材料。
- 前記被覆密度は、1平方マイクロメートル当たり最大約15,000のカーボンナノチューブ数である請求項22に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料のカーボンナノチューブの平均長さは、約1μmから約500μmの間である請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料のカーボンナノチューブの平均長さは、約1μmから約10μmの間である請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料のカーボンナノチューブの平均長さは、約10μmから約100μmの間である請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料のカーボンナノチューブの平均長さは、約100μmから約500μmの間である請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料のカーボンナノチューブの平均長さは、カーボンナノチューブが不足している複合材料と比較して、複合材料の熱膨張係数を約4分の1以下まで減少させるのに十分な長さである請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料のカーボンナノチューブの平均長さは、カーボンナノチューブが不足している複合材料と比較して、複合材料の剛性、及び複合材料の耐摩耗性を約3倍以上まで向上させるのに十分な長さである請求項1に記載の複合材料。
- 前記カーボンナノチューブ浸出繊維材料のカーボンナノチューブの平均長さは、前記複合材料における電気的伝導経路を確立するのに十分な長さである請求項1に記載の複合材料。
- セラミックマトリックスと、
前記セラミックマトリックスの第1領域おける第1部分のカーボンナノチューブ浸出繊維材料、及び、前記セラミックマトリックスの第2領域における第2部分のカーボンナノチューブ浸出繊維材料と、
を含んで構成され、
前記第1部分のカーボンナノチューブ浸出繊維材料に浸出したカーボンナノチューブの平均長さ、及び、前記第2部分のカーボンナノチューブ浸出繊維材料に浸出したカーボンナノチューブの平均長さは、前記セラミックマトリックスの前記第1領域、及び、前記セラミックマトリックスの前記第2領域が、機械的性質、電気的性質又は熱的性質を異にするよう選択される複合材料。 - 前記第1部分のカーボンナノチューブ浸出繊維材料、及び、前記第2部分のカーボンナノチューブ浸出繊維材料は、同一の繊維材料を含んで構成される請求項31に記載の複合材料。
- 前記第1部分のカーボンナノチューブ浸出繊維材料、及び、前記第2部分のカーボンナノチューブ浸出繊維材料は、異なる繊維材料を含んで構成される請求項31に記載の複合材料。
- 前記第1部分のカーボンナノチューブ浸出繊維材料と前記第2部分のカーボンナノチューブ浸出繊維材料との少なくとも1つは、少なくとも前記カーボンナノチューブ浸出繊維材料をオーバーコートする保護層を更に含んで構成される請求項31に記載の複合材料。
- カーボンナノチューブ浸出繊維材料を提供することと、
未焼結のセラミック前駆体に前記カーボンナノチューブ浸出繊維材料を分布させることと、
セラミックマトリックス及び前記カーボンナノチューブ浸出繊維材料を含んで構成される複合材料を形成するために前記未焼結のセラミック前駆体を硬化させることと、
を含んで構成される製造方法。 - 前記セラミックマトリックスは、セメント、炭化ケイ素、炭化タングステン、炭化クロム、炭化チタン、窒化チタン、ホウ化チタン、酸化アルミニウム、窒化ケイ素、ムライト、SiCN、Fe2N及びBaTiO3からなるグループより選択される少なくとも1つのセラミック化合物を含んで構成される請求項35に記載の製造方法。
- 前記カーボンナノチューブ浸出繊維材料は、ガラス繊維、炭素繊維、金属繊維、セラミック繊維、有機繊維、炭化ケイ素繊維、炭化ホウ素繊維、窒化ケイ素繊維、酸化アルミニウム繊維及びこれらの組み合わせからなるグループより選択される少なくとも1つの繊維種を含んで構成される請求項35に記載の製造方法。
- 前記カーボンナノチューブ浸出繊維材料は、前記セラミックマトリックス中に均一に分布する請求項35に記載の製造方法。
- 前記カーボンナノチューブ浸出繊維材料は、前記セラミックマトリックス中に不均一に分布する請求項35に記載の製造方法。
- 前記不均一に分布することには勾配分布が含まれる請求項39に記載の製造方法。
- 前記カーボンナノチューブ浸出繊維材料の少なくとも一部を保護層でオーバーコートすることを更に含んで構成される請求項35に記載の製造方法。
- 前記保護層は、前記カーボンナノチューブ浸出繊維材料のカーボンナノチューブもオーバーコートする請求項41に記載の製造方法。
- 前記保護層は、電気めっき及び化学蒸着からなるグループより選択される技術で付着される請求項41に記載の製造方法。
- 前記保護層は、ニッケル又は二ホウ化チタンを含んで構成される請求項41に記載の製造方法。
- 前記複合材料を高密度化することを更に含んで構成された請求項35に記載の製造方法。
- セメントを含んで構成されるセラミックマトリックスを提供することと、
カーボンナノチューブ浸出繊維材料を提供することと、
前記セメント中に前記カーボンナノチューブ浸出繊維材料を分布させることと、
前記カーボンナノチューブ浸出繊維材料を含んで構成されるコンクリートを形成するように前記セメントを硬化させることと、
を含んで構成される製造方法。 - 前記カーボンナノチューブ浸出繊維材料は短繊維を含んで構成される請求項46に記載の製造方法。
- セラミックマトリックスと、
カーボンナノチューブ浸出繊維材料と、
を含んで構成される複合材料を含む製品。
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EP (1) | EP2504164A4 (ja) |
JP (1) | JP2013511467A (ja) |
KR (1) | KR20120117978A (ja) |
CN (1) | CN102596564B (ja) |
AU (1) | AU2010321534B2 (ja) |
BR (1) | BR112012010907A2 (ja) |
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US8168291B2 (en) | 2012-05-01 |
BR112012010907A2 (pt) | 2019-09-24 |
CN102596564B (zh) | 2014-11-12 |
CA2775619A1 (en) | 2011-05-26 |
KR20120117978A (ko) | 2012-10-25 |
EP2504164A4 (en) | 2013-07-17 |
EP2504164A1 (en) | 2012-10-03 |
WO2011063422A1 (en) | 2011-05-26 |
AU2010321534A1 (en) | 2012-04-05 |
AU2010321534B2 (en) | 2015-03-26 |
US20110124483A1 (en) | 2011-05-26 |
CN102596564A (zh) | 2012-07-18 |
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