JP5785079B2 - 規則性メソポーラス炭素−ケイ素ナノ複合材料の合成 - Google Patents
規則性メソポーラス炭素−ケイ素ナノ複合材料の合成 Download PDFInfo
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Description
・本発明の方法は、無機テンプレートの使用を排除し、これによって調製工程の数、およびこれらの材料の生産に関する費用を低減することが可能である。無機テンプレートの必要性を回避することによって、本方法は、強塩基および/またはHFエッチングに依存せずに済む。・900℃〜1600℃の温度範囲での炭素熱還元は、一定のメゾスコピックd−スペーシングおよび不変質量を示す(表面積および細孔体積に正規化した)。これは、得られたOMSiCが元のメソポーラスC/SiO2構造を複製するという結果を支持している。このような複製は、優れたプロセス柔軟性および構造進化の制御を備えた、幅広いOMSiC構造を可能にする。
材料
OMSiCナノ複合材料では、幾つかの異なる出発配合物を使用して、六角形に規則化した細孔構造を形成することができ、ここで、炭素/ケイ素含量はフェノール樹脂/オルトケイ酸テトラエチル(TEOS)の質量比を調整することによって変化する。
1つの実施の形態に従ったケイ素・炭素・ナノ複合材料は、以下の方法を用いて製造することができる。最初に3.7gのF127を無水エタノール(〜9ml)に加え、界面活性剤が少なくともある程度溶解するまで、加熱と同時に攪拌することによって配合210を調製した。次に、3mlのフェノール樹脂をゆっくりと加えた後、強攪拌した。その後、1.5mlのブタノールを混合物に加え、攪拌を続けた。
上記のように調製した配合物を、900℃または1600℃で最初に熱処理し、炭素およびシリカ含量について分析した。表1は、「プルロニック」F127、フェノール樹脂、前加水分解したTEOS、およびブタノールに基づいた初期の組成を示している。熱処理後、元素分析データからC/SiO2のモル比を計算した。表1に記載されるC/SiO2の値から、炭素のシリカに対する比が>3、すなわち約6〜20であることが分かる。
SiO2(s)+ 3c(s) → SiC(s)+2 CO(g)
によれば、炭素含量は、これらの組成についてのシリカの炭素熱還元にとって十分である。
図1は、(a)900℃または(b)1600℃で3時間加熱したOMSiC配合物209〜211の広角XRD反射を示している。900℃の処理温度(図1(a))の後、明らかなSiC回折ピークは観察されなかったが、非晶質炭素の存在の明らかな兆候が存在した。対照的に、結晶質のSiCは、材料が1600℃に加熱された場合に検出された(図1(b))。β−SiCの(111)、(200)および(220)面の指標となりうる、2θ値35.6°、41.4°および59.9°における3つの回折ピークがはっきりと観察できる。1600℃で処理した後、これらの3つの配合物について、残留非晶質炭素相もまた検出される。
N2 流下、(i)600、(ii)900および(iii)1600℃で加熱処理したサンプルの29Si MAS NMRスペクトルを、図4(a)にプロットした。600℃のサンプルの拡大スペクトルを、破線で示したガウスフィットと共に、図4(b)に示す。この低い処理温度では、検出されたケイ素種のみが、中心が−105ppm近くにある共鳴を生じさせる(図4aの(i)および(ii)参照)。このピークの要因は、シリカ環境にある。図4(a)の600℃サンプルは、図4(b)のように拡大した場合に、3つのガウス共鳴の合計に適合しうる、追加の微細構造を示している。−111、−102および−94ppmの化学シフトにおけるこれらの3つのピークは、それぞれ、0、1つおよび2つのシラノールを有するシリカに相当する。
900℃および1600℃に加熱した3つの配合物(配合物209、210および211)について、窒素およびアルゴン(N2およびAr)の物理吸着の測定を表2に示す。これらのサンプルの異なるOMC/SiO2比を表1に示す。物理吸着データによれば、これらの材料は、OMSiC−900では400〜500m2/g、OMSiC−1600については600〜900m2/gの高い比表面積を有する。
走査電子顕微鏡法を用いて、サンプル209、210および211を評価した。209および211は両方とも粉末であったが、210は圧粉の劈開表面であった。900℃(図5(a))および1600℃(図5(b))で処理した2種類の配合物のSEM顕微鏡写真(210:左側の画像、および211:右側の画像)およびその対応するフーリエ変換を図5(a)および(b)に示す。
Claims (3)
- 規則性メソ多孔質炭化ケイ素ナノ複合材料を形成する方法であって、
炭素前駆体、シリカ前駆体、界面活性剤、および油を含む前駆体混合物を形成し、
前記前駆体混合物を乾燥し、前記炭素前駆体およびシリカ前駆体を架橋して、界面活性剤系の自己組織化テンプレートと、前記テンプレートによって規則化された、炭素前駆体およびシリカ前駆体系のメソ構造相とを形成し、
前記前駆体を熱処理して、規則性メソ多孔質炭化ケイ素ナノ複合材料を形成する、
各工程を有してなる方法。 - 前記炭素前駆体がフェノール樹脂を含み、前記シリカ前駆体が予め加水分解したオルトケイ酸テトラエチルを含み、前記界面活性剤が3ブロック共重合体を含むことを特徴とする請求項1記載の方法。
- 炭素のシリカに対するモル比が3より大きいことを特徴とする請求項1記載の方法。
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US12/190,867 | 2008-08-13 | ||
US12/190,867 US7910082B2 (en) | 2008-08-13 | 2008-08-13 | Synthesis of ordered mesoporous carbon-silicon nanocomposites |
PCT/US2009/004610 WO2010019229A1 (en) | 2008-08-13 | 2009-08-12 | Synthesis of ordered mesoporous carbon-silicon nanocomposites |
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US7910082B2 (en) * | 2008-08-13 | 2011-03-22 | Corning Incorporated | Synthesis of ordered mesoporous carbon-silicon nanocomposites |
US20100040861A1 (en) * | 2008-08-13 | 2010-02-18 | William Peter Addiego | Ordered Mesoporous Free-Standing Carbon Films And Form Factors |
JP2010235387A (ja) * | 2009-03-31 | 2010-10-21 | Ngk Insulators Ltd | 炭化珪素質体及びその製造方法 |
CN102049273B (zh) * | 2009-10-27 | 2013-05-01 | 中国科学院大连化学物理研究所 | 一种介孔炭担载的碳化钨催化剂及其制备和应用 |
KR100995154B1 (ko) * | 2010-02-11 | 2010-11-18 | 전남대학교산학협력단 | 다공성탄소나노섬유 제조방법, 상기 방법으로 제조된 다공성탄소나노섬유, 및 이를 포함하는 탄소나노섬유응용제품 |
KR101190202B1 (ko) * | 2010-05-04 | 2012-10-12 | 한국과학기술연구원 | 에멀젼 전기 방사법을 이용한 탄화규소 나노섬유의 제조방법 및 이에 따라 제조된 탄화규소 나노섬유 |
KR101354712B1 (ko) * | 2011-10-12 | 2014-01-24 | 광주과학기술원 | 입상화 탄소 메조 기공 구조체의 제조 방법 |
WO2013084560A1 (ja) | 2011-12-07 | 2013-06-13 | インターナショナル・ビジネス・マシーンズ・コーポレーション | 電子文書の表示を行う方法、並びにその装置及びコンピュータ・プログラム |
WO2013180764A1 (en) | 2012-01-20 | 2013-12-05 | Free Form Fibers Llc | High strength ceramic fibers and methods of fabrication |
CN102674354B (zh) * | 2012-05-11 | 2014-04-09 | 南京工业大学 | 一种介孔碳化硅材料的制备方法 |
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