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Direct Observation of Plugs and Intrawall Pores in SBA-15 Using Low Voltage High Resolution Scanning Electron Microscopy and the Influence of Solvent Properties on Plug-Formation

Kjellman, Tomas; Asahina, Shunsuke; Schmitt, Julien; Impéror-Clerc, Marianne; Terasaki, Osamu; Alfredsson, Viveka

By 12 March 2019No Comments

Chemistry of Materials, 2013, vol 25, 20, pp. 4105-4112

DOI:10.1021/cm402635m

Abstract

Through the use of low voltage high resolution scanning electron microscopy (LV-HRSEM) we have studied the fine details of the intricate pore structure of SBA-15. Intrawall pores and deviations from the ideal and uniform cylindrical pores are clearly observed, and we report for the first time the direct observation of ?plugs? in the pores. N2-sorption measurements confirm their existence. LV-HRSEM provides an opportunity to quantify the frequency of occurrence of plugs within the pore structure. The rate of mesophase formation, followed with in situ small angle X-ray scattering (SAXS) under different solvent conditions, is shown to have a significant influence on the development of plugs and how frequently they occur. We suggest a mechanism explaining the existence of the plugs, providing means for a better understanding and control over material properties.

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