通过对聚甲基(苯基)硅树脂(SR249)在1250～1350℃、真空气氛下裂解以及氢氟酸酸洗处理制备得到具有高比表面积的纳米多孔炭材料.采用X-ray衍射光谱、拉曼光谱、元素分析、透射电镜及氮气吸附法对不同温度所制样品进行元素组成及结构研究.裂解产物中的SiO2相作为一种天然模板经腐蚀处理除去.裂解温度和酸洗处理对多孔炭材料的成分和结构变化影响较大.HF酸处理前,裂解产物的比表面积小于55 m2/g;而酸洗后产物比表面积和总孔容量显著增加,而最高值是裂解温度为1300℃时获得,分别为1148 m2/g、0.608cm3/g.经酸洗处理得到的多孔炭,孔径分布均相对较窄,在1～4nm.透射电镜结果显示炭材料中的自由碳相和少量的SiC纳米晶及SiOC陶瓷彼此相互包裹.
参考文献
| [1] | Dan Liu;Jia-Heng Lei;Li-Ping Guo .Simple hydrothermal synthesis of ordered mesoporous carbons from resorcinol and hexamine[J].Carbon: An International Journal Sponsored by the American Carbon Society,2011(6):2113-2119. |
| [2] | Miguel Teixeira;Marta C. Campo;David A. Pacheco Tanaka .Composite phenolic resin-based carbon molecular sieve membranes for gas separation[J].Carbon: An International Journal Sponsored by the American Carbon Society,2011(13):4348-4358. |
| [3] | Xiaoping Dong;Jie Fu;Xingxing Xiong;Chen Chen .Preparation of hydrophilic mesoporous carbon and its application in dye adsorption[J].Materials Letters,2011(15/16):2486-2488. |
| [4] | Wei Xie;Haifeng Cheng;Zengyong Chu .Effect of carbonization temperature on the structure and microwave absorbing properties of hollow carbon fibres[J].CERAMICS INTERNATIONAL,2011(6):1947-1951. |
| [5] | Chang CF.;Tsai WT.;Chang CY. .Effects of burn-off and activation temperature on preparation of activated carbon from corn cob agrowaste by CO2 and steam[J].Journal of Colloid and Interface Science,2000(1):45-49. |
| [6] | Huang, D.C.;Liu, Q.L.;Zhang, W.;Ding, J.;Gu, J.J.;Zhu, S.M.;Guo, Q.X.;Zhang, D. .Preparation of high-surface-area activated carbon from Zizania latifolia leaves by one-step activation with K_2CO_3/rarefied air[J].Journal of Materials Science,2011(15):5064-5070. |
| [7] | Zengyong Chu;Rongan He;Xiaobin Zhang .Fabrication of porous SiC_y (core)/C (shell) fibres using a hybrid precursor of polycarbosilane and pitch[J].Carbon: An International Journal Sponsored by the American Carbon Society,2010(7):2115-2118. |
| [8] | Peng-Xiang Hou;Toshiaki Yamazaki;Hironori Orikasa .An easy method for the synthesis of ordered microporous carbons by the template technique[J].Carbon: An International Journal Sponsored by the American Carbon Society,2005(12):2624-2627. |
| [9] | Hao Wang;Xiaodong Li;Lan-Young Hong;Dong-Pyo Kim .Preparation of phenolic resin derived 3-D ordered macroporous carbon[J].Journal of porous materials,2006(2):115-121. |
| [10] | Adsorption and structural properties of soft-templated mesoporous carbons obtained by carbonization at different temperatures and KOH activation[J].Applied Surface Science: A Journal Devoted to the Properties of Interfaces in Relation to the Synthesis and Behaviour of Materials,2010(17):5187. |
| [11] | Wen-Hua Zhang;Changhai Liang;Huijiao Sun;Zhiqi Shen;Yejun Guan;Pinliang Ying;Can Li .Synthesis of Ordered Mesoporous Carbons Composed of Nanotubes via Catalytic Chemical Vapor Deposition[J].Advanced Materials,2002(23):1776-1778. |
| [12] | An-Hui Lu;Wen-Cui Li;Wolfgang Schmidt;Ferdi Schuth .Template synthesis of large pore ordered mesoporous carbon[J].Microporous and Mesoporous Materials,2005(1/3):117-128. |
| [13] | Volker Presser;Min Heon;and Yury Gogotsi .Carbide-Derived Carbons - From Porous Networks to Nanotubes and Graphene[J].Advanced functional materials,2011(5):810-833. |
| [14] | Cekdar Vakifahmetoglu;Volker Presser;Sun-Hwa Yeon .Enhanced hydrogen and methane gas storage of silicon oxycarbide derived carbon[J].Microporous and mesoporous materials: The offical journal of the International Zeolite Association,2011(1/3):105-112. |
| [15] | Ryoo R;Joo S H;Jun S .Synthesis of highly ordered carbon molecular sieves via template-mediated structural transformation[J].Journal of Physical Chemistry B,1999,103:7743-7746. |
| [16] | Maria Jorda-Beneyto;Dolores Lozano-Castello;Fabian Suarez-Garcia .Advanced activated carbon monoliths and activated carbons for hydrogen storage[J].Microporous and mesoporous materials: The offical journal of the International Zeolite Association,2008(1/3):235-242. |
| [17] | Y. D. Blum;D. B. MacQueen;H.-J. Kleebe .Synthesis and characterization of carbon-enriched silicon oxycarbides[J].Journal of the European Ceramic Society,2005(2/3):143-149. |
| [18] | Sandra Martmez-Crespiera;Emanuel Ionescu;Hans-Joachim Kleebe .Pressureless synthesis of fully dense and crack-free SiOC bulk ceramics via photo-crosslinking and pyrolysis of a polysiloxane[J].Journal of the European Ceramic Society,2011(5):913-919. |
| [19] | Tian Liang;Ya-Li Li;Dong Su;He-Bao Du .Silicon oxycarbide ceramics with reduced carbon by pyrolysis of polysiloxanes in water vapor[J].Journal of the European Ceramic Society,2010(12):2677-2682. |
| [20] | Saha A;Raj R;Williamson DL .A model for the nanodomains in polymer-derived SiCO[J].Journal of the American Ceramic Society,2006(7):2188-2195. |
| [21] | Varga, T;Navrotsky, A;Moats, JL;Morcos, RM;Poli, F;Muller, K;Sahay, A;Raj, R .Thermodynamically stable SixOyCz polymer-like amorphous ceramics[J].Journal of the American Ceramic Society,2007(10):3213-3219. |
| [22] | Scarmi A;Soraru GD;Raj R .The role of carbon in unexpected visco(an)elastic behavior of amorphous silicon oxycarbide above 1273 K[J].Journal of Non-Crystalline Solids: A Journal Devoted to Oxide, Halide, Chalcogenide and Metallic Glasses, Amorphous Semiconductors, Non-Crystalline Films, Glass-Ceramics and Glassy Composites,2005(27/29):2238-2243. |
| [23] | Kroll P .Modeling the 'free carbon' phase in amorphous silicon oxycarbide[J].Journal of Non-Crystalline Solids: A Journal Devoted to Oxide, Halide, Chalcogenide and Metallic Glasses, Amorphous Semiconductors, Non-Crystalline Films, Glass-Ceramics and Glassy Composites,2005(12/13):1121-1126. |
| [24] | Pena-Alonso R;Soraru GD;Raj R .Preparation of ultrathin-walled carbon-based nanoporous structures by etching pseudo-amorphous silicon oxycarbide ceramics[J].Journal of the American Ceramic Society,2006(8):2473-2480. |
| [25] | Hans-Joachim Kleebe;Yigal D. Blum .SiOC ceramic with high excess free carbon[J].Journal of the European Ceramic Society,2008(5):1037-1042. |
| [26] | Belot V;Corriu R J P;Leclercq D et al.Silicon oxycarbide glasses with low O/Si ratio from organosilicon precursors[J].Journal of Non-Crystalline Solids,1994,176:33-44. |
| [27] | Yang ZX;Zhou WM;Zhu F;Zhang YF .SiC/SiO2 core-shell nanocables formed on the carbon fiber felt[J].Materials Chemistry and Physics,2006(2/3):439-441. |
| [28] | Schiavon M A;Radovanovic E;Yoshida I V P .Microstructural characterization of monolithic ceramic matrix composites from polysiloxane and SiC powder[J].Powder Technology,2002,123:232-241. |
| [29] | Ferrari A C;Robertson J .Interpretation of Raman spectra of disordered and amorphous carbon[J].Physical Review B,2000,61:14095-14107. |
| [30] | Cambaz Z G;Yushin G N;Gogotsi Y et al.Formation of carbide-derived carbon on b-silicon carbide whiskers[J].Journal of the American Ceramic Society,2006,89:509-514. |
| [31] | Ferrari A C .Robertson.Raman spectroscopy of amorphous,nanostructured,diamond-like caroon and nanodiamond[J].Philosophical Transactions of the Royal Society of London Series A Mathematical and Physical Sciences,2004,362:2477-2512. |
| [32] | Tuinstra F;Koenig J L .Raman spectrum of graphite[J].Journal of Chemical Physics,1970,53:1126-1130. |
| [33] | Sing K S W;Everett D H;Haul R A W.Reporting physisorption data for gas/solid systems[A].,2008:1217-1230. |
| [34] | Liqun Duan;Qingsong Ma .Effect of pyrolysis temperature on the pore structure evolution of polysiloxane-derived ceramics[J].CERAMICS INTERNATIONAL,2012(4):2667-2671. |
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