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以多孔块状硅体为模板,通过一步浸渍、炭化、酸处理工艺,制备出结构可控、孔隙联通且具有多重孔隙的铸型炭体.分别采用氮吸附技术、高分辨透射电镜和扫描电镜对模板硅、硅碳复合物及相应炭体进行了结构表征.从微米尺度分析,该炭体是由高度联接的枝状结构单元为骨架构筑而成.与模板硅相比较,此炭体是硅体的正复本.从纳米尺度分析,这种炭体枝状骨架是由分布均匀且相互连接的中孔构成,此中孔及其孔壁对应于模板硅的孔壁及中孔,是多孔硅的负复本.此外构成中孔的炭骨架本体又含有大量炭化过程产生的微孔.因此该法合成的铸型炭具有孔隙高度发达和结构层层嵌套的特点.

Carbon monoliths with a multi-modal hierarchical porosity have been prepared by a nanocasting method with silica monoliths as the scaffold, in which volume and surface templating has been successfully combined in a one-step impregnation approach, and the smaller pores in the silica template are impregnated in a straightforward way. The monoliths obtained at different stages of the process were characterized by N2-adsorption, scanning electron microscopy and transmission electron microscopy. It is shown that the carbon monoliths represent a positive replica of the starting silica monoliths on the micrometer scale. The surface templated mesopores can be regarded as a positive replica, while the volume templated mesopores are a negative replica of the silica scaffold.

参考文献

[1] Akira Taguchi;Jan-Henrik Smatt;Mika Linden .Carbon Monoliths Possessing a Hierarchical, Fully Interconnected Porosity[J].Advanced Materials,2003(14):1209-1211.
[2] Smatt JH.;Schunk S.;Linden M. .Versatile double-templating synthesis route to silica monoliths exhibiting a multimodal hierarchical porosity[J].Chemistry of Materials,2003(12):2354-2361.
[3] Takashi Kyotani;Takayuki Nagai;Sanjuro Inoue .Formation of new type of porous carbon by carbonization in zeolite nanochannels[J].Chemistry of Materials,1997(2):609-615.
[4] An-Hui Lu;Wolfgang Schmidt;Bernd Spliethoff;Ferdi Schuth .Synthesis of Ordered Mesoporous Carbon with Bimodal Pore System and High Pore Volume[J].Advanced Materials,2003(19):1602-1606.
[5] Ryoo R;Joo S H;Kun S .Synthesis of highly ordered carbon molecular sieves via template-mediated structural transformation[J].Journal of Physical Chemistry B,1999,103:7743-7746.
[6] An-Hui Lu;Wolfgang Schmidt;Akira Taguchi;Bernd Spliethoff;Bernd Tesche;Ferdo Schuth .Taking Nanocasting One Step Further: Replicating CMK-3 as a Silica Material[J].Angewandte Chemie International Edition,2002(18):3489-3492.
[7] Min Kang;Seung Hwan Yi;Hyung Ik Lee;Jae Eui Yie;Ji Man Kim .Reversible replication between ordered mesoporous silica and mesoporous carbon[J].Chemical communications,2002(17):1944-1945.
[8] 陆安慧,Wolfgang Schmidt,Ferdi Schüth.结构有序、双重孔隙中孔炭材料的合成与表征[J].新型炭材料,2003(03):181-185.
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