JP2010510948A - カーボンナノチューブ合成用大量エアロゾル粉末噴射装置 - Google Patents
カーボンナノチューブ合成用大量エアロゾル粉末噴射装置 Download PDFInfo
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Abstract
【解決手段】単層カーボンナノチューブ(SWNT)を連続して大規模に合成する製造装置のコンテナにおいて、このコンテナの一方の端にピストンを設置し、もう一方の端には、コンテナの反対側の壁面から吹き込まれる気体によって接線渦流を発生させる。コンテナは、微粒子の凝集を減らすまたは防ぐために加熱され、ピストンは触媒を前記渦流に向けて噴射するために用いられる。触媒の噴射速度は、輸送気体としても働く前記渦流を起こすために、ピストン速度および気体流量によって制御される。こうして、1kg/hを超えるエアロゾル化され凝集していない乾燥触媒を、一定の流量にて反応容器に輸送することができる。
【選択図】図1
Description
特に述べない限りは、明細書および請求の範囲を含む本願のなかで用いられる下記の用語を、以下に定義する。ここで、明細書および請求の範囲において用いられる用語は、文脈から複数形を含まないことが明らかな場合を除いて単数形、複数形を含むものとする。一般的な化学用語の定義は、例えば非特許文献6および非特許文献7などの参考文献が参照可能である。
本発明の、製造方法、プロセス、および装置は、触媒粉末として担持金属ナノ粒子を用いる。触媒として選ばれる金属または金属の組み合わせは、所望の粒度および粒径分布が得られるように処理することができる。この金属ナノ粒子は、カーボンナノチューブの合成時に、金属成長触媒を用いて担体に適した金属上に担持させて分離することができる。このような金属には、結晶シリコン、ポリシリコン、シリコンナイトライド、タングステン、マグネシウム、アルミニウム、およびこれら金属の酸化物、好ましくは、アルミニウム酸化物、シリコン酸化物、マグネシウム酸化物、チタン酸化物、またはこれらの酸化物の組み合わせを粉末にしたものが挙げられるが、随意他の元素を加えることもでき、担持用粉末として用いられる。この担持用粉末上に担持された金属ナノ粒子を、反応容器にエアロゾルとして噴射する。前記金属触媒は、カーボンナノチューブの成長プロセスにおいて、カーボン前駆体を分解し、カーボンがナノチューブとして配列されて堆積するのを助ける役割を果たす。
カーボンナノチューブは、炭素含有気体などのカーボン前駆体を用いて合成することができる。一般に、約1000℃まで熱分解しない炭素含有気体であればどのようなものを用いてもよい。好適な炭素含有気体の例としては、一酸化炭素、メタン、エタン、プロパン、ブタン、ペンタン、ヘキサン、エチレン、アセチレン、およびプロピレンなどの飽和および不飽和の脂肪族炭化水素、アセトンおよびメタノールなどの酸化炭化水素、ベンゼン、トルエン、およびナフタレンなどの芳香族炭化水素、さらにこれらの混合物、例えば、一酸化炭素−メタン混合物などがある。一般に、アセチレンを用いた場合は、多層カーボンナノチューブの生成が促進され、一方、単層カーボンナノチューブの生成にはCOおよびメタンが供給気体として適している。また、炭素含有気体は、水素、ヘリウム、アルゴン、ネオン、クリプトン、キセノン、またはこれらの気体の混合気体などの希釈用気体と、随意混合させてもよい。
酸化物粉末上に担持された金属ナノ粒子を、上記の噴射装置によってエアロゾル化し、反応容器に導入する。同時に、カーボン前駆体気体を反応容器に導入する。反応容器内のこれら反応原料の流れを、反応容器の壁面に付くカーボン生成物の量を少なくするように制御する。こうして、製造されたカーボンナノチューブを回収し分離することができる。
担体材料を金属塩溶液に含浸させて触媒を調製した。単一金属イオン系触媒用に、メタノールに含ませたFeAc2を、Fe:Al2O3=1:15のモル比で使用した。窒素雰囲気下、ジエチレングリコールモノ−n−ブチルエーテルに、1mM:20mMのモル比でFeAc2を加えた。マグネティックスターラーバーを用い、窒素雰囲気下、反応混合物を混合し、90分間加熱還流した。次に反応混合物を室温にまで冷却し、Al2O3(15mM)を一度に加えた。反応溶液を室温にて15分間撹拌し、3時間150℃にまで加熱した。溶媒を除くために反応混合物の上に窒素気流を流しながら、90℃にまで冷却した。反応フラスコの壁面上に形成された黒色膜を回収し、メノウ乳鉢にて粉砕して黒色の微粉末を得た。
実施例1で調製したAl2O3担持鉄触媒約10gを、コンテナに入れ、500℃まで加熱した。加熱した担持触媒を、コンテナにH2/He(1:1 v/v)を流して還元した。こうして得られた還元担持触媒乾燥粉末を、この粉末を流動層噴射装置の多孔質プレート上に運ぶコンベヤーベルトの上に滴下した。流速15Lpmでコンテナ底部およびチャンネルを通ってアルゴンガスを流すことにより、触媒粉末をエアロゾル化した。触媒粉末を乗せて運ぶこのアルゴンガスの気流は、約700℃にまで加熱され、静電気を除去されて反応容器へと輸送される。こうして、担持触媒を、約150g/m3の質量濃度でアルゴンガスに乗せ、カーボンナノチューブを製造するため反応容器に導入する前に、前加熱処理を行った。
Claims (11)
- 粉末噴射装置であって、前記粉末噴射装置は、側壁、上端部、および下端部を有するコンテナと、前記コンテナの前記下端部にあるバーと、前記バーが取り付けられているピストンと、前記コンテナの前記上端部にあるノズルと、前記ノズルと前記バーとの間の前記側壁に設けられた複数の気体導入口とから構成され、乾燥した粉末を前記バーの上方であって前記気体導入口の下方の位置に導入することを特徴とする粉末噴射装置。
- 請求項1に記載の装置であって、前記粉末は粉末化した酸化物担体上に担持された金属触媒より構成され、前記粉末化した酸化物担体は、0.5μmから5μmの粒度を有する粉末噴射装置。
- エアロゾル化した粉末を噴射装置により噴射する方法であって、前記噴射装置は側壁、上端部、および下端部から構成されるコンテナをもち、前記下端部はピストンに取り付けられたバーをもち、前記上端部はノズルをもち、前記側壁には複数の気体導入口を前記ノズルと前記バーとの間に有し、
前記方法は、前記噴射装置に乾燥した粉末を前記バーの上方であって前記気体導入口の下方の位置に導入する工程、
前記ピストンにより前記粉末を前記上端部に向けて押し上げる工程、
前記気体導入口より気体を流入させることにより前記上端部付近に渦流を発生させ、前記粉末を前記渦流に乗せて前記ノズルを通して噴射する工程を有することを特徴とするエアロゾル化した粉末の噴射方法。 - 請求項3に記載の方法であって、前記粉末は粉末状にした酸化物担体上に担持された金属触媒より構成されることを特徴とするエアロゾル化した粉末の噴射方法。
- 請求項4に記載の方法であって、前記粉末は400℃から900℃の間にある温度に加熱されることを特徴とするエアロゾル化した粉末の噴射方法。
- 請求項4に記載の方法であって、前記粉末は遷移金属酢酸塩であることを特徴とするエアロゾル化した粉末の噴射方法。
- 請求項3に記載の方法であって、前記気体はAr、Kr、Xe、N2またはこれら気体の組み合わせからなる群より選ばれることを特徴とするエアロゾル化した粉末の噴射方法。
- 請求項7に記載の方法であって、前記気体はArであることを特徴とするエアロゾル化した粉末の噴射方法。
- 請求項3に記載の方法であって、前記ピストンおよび前記気流は、前記粉末1g/hから5kg/hの割合で前記粉末を噴射するように制御されることを特徴とするエアロゾル化した粉末の噴射方法。
- 請求項9に記載の方法であって、前記ピストンおよび前記気流は、前記粉末500g/hから4.5kg/hの割合で前記粉末を噴射するように制御されることを特徴とするエアロゾル化した粉末の噴射方法。
- 請求項3に記載の方法であって、前記ピストンおよび前記気流は、前記粉末1kg/hよりも大きな割合で前記粉末を噴射するように制御されることを特徴とするエアロゾル化した粉末の噴射方法。
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US86714506P | 2006-11-24 | 2006-11-24 | |
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PCT/US2007/085533 WO2008064368A2 (en) | 2006-11-24 | 2007-11-26 | Injector for large amount of aerosol powder for synthesis of carbon nanotubes |
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JP (1) | JP5475457B2 (ja) |
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JP5475457B2 (ja) | 2014-04-16 |
US8684284B2 (en) | 2014-04-01 |
WO2008064368A2 (en) | 2008-05-29 |
WO2008064368A3 (en) | 2009-04-02 |
US20120138148A1 (en) | 2012-06-07 |
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