JP5358454B2 - カーボンナノチューブを基本構造としたエアロゲル - Google Patents
カーボンナノチューブを基本構造としたエアロゲル Download PDFInfo
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- JP5358454B2 JP5358454B2 JP2009542138A JP2009542138A JP5358454B2 JP 5358454 B2 JP5358454 B2 JP 5358454B2 JP 2009542138 A JP2009542138 A JP 2009542138A JP 2009542138 A JP2009542138 A JP 2009542138A JP 5358454 B2 JP5358454 B2 JP 5358454B2
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- carbon
- dispersion
- surfactant
- nanotubes
- foam
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Description
この生産方法によると、エアロゲルは、型として用いられる多孔性材料のポアをカーボンで充填することによって合成される。典型的には、アルミニウム、シリカ又はアルミノケイ酸塩タイプの材料が、マイクロ多孔性又はメソ多孔性材料(例えば、ゼオライト又はメソ構造のタイプMCM−41)の形態で利用される。その後、その型は、一般的には、酸の攻撃によって破壊されて、それによって、カーボンによって全体的に形成された型の痕跡が回収される。これらの技術において、テンプレート材料にカーボンを初期導入することは、カーボンの直接蒸着によって実行されよく、一般的には、気相中での化学蒸着、特には化学気相蒸着(CVD)によって実行されよく、又は代替的に、ポア内に有機溶液を含浸することによって実行されてよく、含浸後に、カーボンに変換されるためにその液は焼成される。この方法によるエアロゲルを生産する方法の例示は、L’実在の(実際の)ite chimique、no.245−246、pp.124−128(3月−4月 2006)中に、C.Vix−Guterl、J.Parmentier及びP.Delhaes著の「Nouveaux concepts d’elaboration de materiaux carbones poreux」の記事、並びに、The Journal of Physical chemistry B、103(37)、pp.7743−77468(1999)中に、R.Ryoo、S.−H.Soo及びS.Jun著の「Synthesis of highly ordered carbonmolecular sieves via template−mediated structural transformation」の記事に特に述べられている。
他のここでの実施態様によると、エアロゲル形態中のカーボンの組織化は、液体又はゲル化媒介物内で実行され、典型的には液晶の形態で実行される。この場合に、用いられる「モールド」は、本来固体ではないが、それにもかかわらず、合成されるカーボン構造に組織化した構造を提供する。
他のここでの変更例によると、エアロゲルは、前述の変形例のようなカーボンではなく、有機構成要素を直接的に構造化することによって形成され、それによって、有機エアロゲルが得られ、その後、好ましいカーボンエアロゲルを生成するために熱処理によって、カーボン化される。この記載内で、D.Wu、R.Fu、M.S.Dresselhaus及びG.Dresselhaus著による、carbon、44、pp.675−680(2005)中の「Fabrication of nano−structure contol of carbon arerogels via microemulsion templatted sol−gel polymerisation method」記事、又はS.A.Al−Muthtsabeb及びJ.A.Ritter著による、Adv.Mater.、15(2)、pp.101−104(2003)中の「Preparation and propertied of resorcinol formaldehyde organic and carbon gels」記事に述べられている方法を特に利用することは可能である。
(A)分散用界面活性剤(一般的には、イオン性、好ましくはアニオン性)を用いることによってカーボンナノチューブの水分散液を作る工程、
(B)発泡剤の存在下、ガスの作用でその分散液を膨張させることによって、工程(A)で得られたナノチューブのその水分散液から泡を作り出す工程、並びに
(C)工程(B)で得られた泡を凍結し、その後、昇華、一般的には、低温フリーズドライによってその水を取り除く工程を、
含む。
泡立ちをもたらすガスの作用で泡が出来上がるので、形成する泡は、重力によって水を失う傾向があり、その水は下向きに流れる傾向がある。この現象は、多角形形状で比較的不安定な非球状の空洞である比較的「乾燥した」泡を形成する傾向がある。球状の空洞を更に得て、安定性を改良する目的で、泡中の水分度を増加してよく、特に、泡の上部に、水を有する成長中の泡を供給することによって重力による水のロスを補うことによって増加する。このため、泡の組成が同時に変わらないように、工程(B)の成長中の泡の上部は、膨張することによって泡立ちする分散液と同一の組成を有する分散液でまき散らされてよく、散布は一定の流量で実行されることが好ましい。そのことによって、任意の合一現象を追加的に回避しながら、均一な組成の泡が得られる。
この大きさは、用いられるガスの流量は勿論こと、膨張を実行するために最初に導入されるガスの泡の大きさに作用することによって(特には、用いられる多孔性膜のポアの大きさに作用することによって)制御され得る。一定のガス流量である場合、注入されるガスの泡が大きければ大きいほど、結果物の泡の空洞の大きさは、一般的には、大きくなる。例えば、0.1〜1ml/sのオーダーの一定の流量と10〜250μmのオーダーのポアの多孔性膜を用いて、結果として得られた泡の気泡の平均サイズは、典型的には、50〜600μmまで変わる。
この特定の実施例の範囲内において、多壁のカーボンナノチューブが用いられる(市販のPyrographIII、PR−24−PSタイプ)。
1gのTergitol NP9(1質量%濃度 のTergitol溶液に対応する)が、前工程で調製された分散液(d)に加えられた。
そのビーカーは、−80℃条件下に素早く置かれて5時間その温度で放置された。
前工程で得られたエアロゲルが、次の条件下で熱処理された。
2時間かけて、室温(25℃)から400℃まで昇温し、
1時間、400℃で安定に保ち、
2時間かけて、400℃から室温(25℃)まで降温する。
見掛け密度:0.2、
実際の密度(濃度):2.1、
特有のBET表面域:36m2/g、
寸法上約50μmのポアを有する多孔性マクロ構造であって、そのマクロ構造の内壁に2〜50nmのポアを有した多孔質。
Claims (29)
- カーボンエアロゲルを生産する方法であって、
(A)分散用界面活性剤を用いることによって、カーボンナノチューブの水分散液を作る工程、
(B)発泡剤の存在下、ガスの作用で該分散液を膨張させることによって、該工程(A)で得られたナノチューブの該水分散液から泡を作り出す工程、及び、
(C)該工程(B)で得られた該泡を凍結し、その後、昇華によって該水を取り除く工程を、
含む、方法。 - 前記工程(A)から前記工程(C)まで終了した後に、更に工程(D)を含み、該工程(D)において、前記工程(C)の終了後に得られた材料が400℃超の温度で熱処理を受ける、請求項1に記載の方法。
- 前記工程(D)が、有機化合物の存在下で、かつ、800℃超の温度で実行される、請求項2に記載の方法。
- 前記工程(D)が、1200℃以上の温度で実行される、請求項3に記載の方法。
- 前記工程(A)で用いられる前記ナノチューブが、10から100nmの平均径と1から20μmの平均長とを有する、請求項1から請求項4のいずれか1項に記載の方法。
- 前記工程(A)で用いられる前記界面活性剤がイオン性界面活性剤である、請求項1から請求項5のいずれか1項に記載の方法。
- 前記イオン性界面活性剤が、硫酸塩、スルホン酸塩又はカルボン酸塩タイプのアニオン性界面活性剤である、請求項6に記載の方法。
- 前記工程(A)の前記界面活性剤がカルボキシメチルセルロース塩である、請求項6に記載の方法。
- 前記カルボキシメチルセルロース塩がカルボキシメチルセルロースナトリウム塩である、請求項8に記載の方法。
- 前記工程(A)で調製された分散液が、1リットル当たり1から15gのナノチューブを含む、請求項1から請求項9のいずれか1項に記載の方法。
- 前記工程(B)において、発泡剤が、前記工程(A)の終了後に得られる前記分散液に添加される、請求項1から請求項10のいずれか1項に記載の方法。
- 前記添加される発泡剤が非イオン性エトキシ化界面活性剤である、請求項11に記載の方法。
- 前記非イオン性エトキシ化界面活性剤が式:C 15 H 24 O(C 2 H 4 O) 9 によって表される化合物である、請求項12に記載の方法。
- 前記添加される発泡剤がスターチ又は糖類である、請求項11に記載の方法。
- 前記添加される発泡剤がポリサッカリドである、請求項11に記載の方法。
- ドデシル硫酸ナトリウムSDSが、前記工程(A)の分散用界面活性剤と前記工程(B)の発泡剤との両方の試薬として用いられる、請求項1から請求項6のいずれか1項に記載の方法又は請求項10に記載の方法。
- 前記工程(B)の泡の形成が、前記工程(A)の終了後に得られた分散液中にガスの気泡を注入することによって実行され、必要に応じて該ガスに前記発泡剤が添加され、該ガスの気泡の該注入が、分散液の下部に配置された焼結ガラスのような多孔性膜の中を通って実行される、請求項1から請求項16のいずれか1項に記載の方法。
- 前記工程(B)において、成長中の泡の上部が、膨張によって泡立ちする分散液と同一の組成を有する分散液でまき散らされる、請求項1から請求項17のいずれか1項に記載の方法。
- 前記工程(B)で作り出された前記泡中の液体/ガスの体積比が0.1未満である、請求項1から請求項18のいずれか1項に記載の方法。
- 請求項1から請求項19のいずれか1項に記載の方法によって得られることが可能であって、気泡構造形態でカーボンナノチューブを凝固することによって生成するカーボンエアロゲル。
- 実質的に開口した多孔質を備えた構造を有するカーボンエアロゲルであって、
40μm超の平均サイズを有する気泡(又は「マクロポア」)で構成された「マクロ多孔質」及び、
該マクロ多孔質の気泡の壁内に実質的に配置された「スーパーメソ多孔質」であって、このナノ多孔質が60nm未満の平均サイズを有するポアを含む、「スーパーメソ多孔質」の両方を含む、請求項20に記載のカーボンエアロゲル。 - 0.25g/cm3以下の見掛け密度を有する、請求項20又は請求項21に記載のカーボンエアロゲル。
- 前記ポアによって占められる容積が前記材料の全容積の少なくとも80%に相当する、請求項20から請求項22のいずれか1項に記載のカーボンエアロゲル。
- 25から300m2/gの特有表面域を有する、請求項20から請求項23のいずれか1項に記載のカーボンエアロゲル。
- 分離材としての請求項20から請求項24のいずれか1項に記載のカーボンエアロゲルの使用。
- 固体/液体タイプの分離を実行するための分離材としての請求項20から請求項24のいずれか1項に記載のカーボンエアロゲルの使用。
- バイオマテリアルとしての請求項20から請求項24のいずれか1項に記載のカーボンエアロゲルの使用。
- 細胞成長の支持体としての請求項20から請求項24のいずれか1項に記載のカーボンエアロゲルの使用。
- 触媒種、非湿潤液の保存、若しくは燃料電池膜中の高エネルギー液の保存のための支持体、リチウム電池の負極、又は遮音材若しくは防振材としての請求項20から請求項24のいずれか1項に記載のカーボンエアロゲルの使用。
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CN114436241B (zh) * | 2022-01-28 | 2023-06-27 | 西安理工大学 | 模具辅助阶梯式成型的碳管增韧密度渐变碳气凝胶及方法 |
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US20100092371A1 (en) | 2010-04-15 |
FR2910458A1 (fr) | 2008-06-27 |
EP2111292A1 (fr) | 2009-10-28 |
JP2010513202A (ja) | 2010-04-30 |
FR2910458B1 (fr) | 2009-04-03 |
DE602007009875D1 (de) | 2010-11-25 |
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