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Characterization of Pore Framework Structure in Monolithic Mesoporous Silica

Published online by Cambridge University Press:  31 January 2011

Ching-Mao Wu ,
Szu-Yin Lin ,
Chin-Cheng Weng  and
Kuo-Tung Huang
Ching-Mao Wu
Affiliation:
ChingMaoWu@itri.org.tw, Industrial Technology Research Institute, Chutung, Hsinchu, Taiwan, Province of China
Szu-Yin Lin
Affiliation:
szuyinlin@itri.org.tw, Industrial Technology Research Institute, Chutung, Hsinchu, Taiwan, Province of China
Chin-Cheng Weng
Affiliation:
ccweng@itri.org.twccweng1999@gmail.com, Industrial Technology Research Institute, Chutung, Hsinchu, Taiwan, Province of China
Kuo-Tung Huang
Affiliation:
GordonHuang@itri.org.tw, Industrial Technology Research Institute, Chutung, Hsinchu, Taiwan, Province of China
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Abstract

Mesoporous silica materials have received much interest due to commercial applications in chemical separations and heterogeneous catalysis. Recent studies have reported via a sol-gel nanocasting technique, monolithic mesoporous silica with wormlike pore framework could be prepared by utilizing room-temperature ionic liquids (RTILs) as templates and solvents. Although previous reports have indicated that the wormlike pores would be formed in the silica, the detailed pore network structure still remained the crucial issues to be resolved. In the present study, we investigated the pore structure in the monolithic mesoporous silica, which was templated by RTIL (1-butyl-3-methyl-imidazolium-tetrafluoroborate). We revealed an open fractal pore network with a branched and self-similar appearance was formed by the aggregation of the individual spherical pores. Transmission electron microscopy micrographs displayed that the disordered wormlike pore framework was formed in the silica. Furthermore, the small angle X-ray scattering profile measured herein further exhibited three distinct regions of power-law scattering on the respective length scales. In the high-q region, the profile followed Power behavior and a power-law of -4 was observed for the surface fractal dimension of 2, manifesting the primary pore with a smooth surface and a spherical appearance. In the intermediate-q region, a power-law of -2.5 (mass fractal dimension of 2.5), indicating an open mass fractal network was formed by the aggregation of the individual primary pores. Moreover in the low-q region, the power-law of -4 was observed for mass-fractal agglomerates of aggregates. With the proceeding analysis of unified equation in terms of two structural levels, the radiuses of gyration of primary pore (Rg1)and its aggregates (Rg2) were fitted as ca. 0.9 nm and 5.5 nm, respectively. For a spherical-model pore, the radius of pore (R) was ca. 1.16 nm; thus, the averaged pore diameter (D) was 2.32 nm. The number of primary pores in a fractal aggregate (degree of aggregation, z) was calculated as ca. 67.

Keywords

nanostructureself-assemblysol-gel
Type
Research Article
Information
MRS Online Proceedings Library (OPL) , Volume 1217: Symposium Y – Catalytic Materials for Energy, Green Processes and Nanotechnology , 2009 , 1217-Y03-56
Copyright
Copyright © Materials Research Society 2010

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