In situ observation of phase separation processes in gelling alkoxy-derived silica system by light scattering method |
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Authors: | Hironori Kaji Kazuki Nakanishi Naohiro Soga Tadashi Inoue Norio Nemoto |
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Institution: | (1) Department of Industrial Chemistry, Faculty of Engineering, Kyoto University, 606-01 Kyoto, Japan;(2) Division of Material Chemistry, Faculty of Engineering, Kyoto University, 606-01 Kyoto, Japan;(3) Institute for Chemical Research, Kyoto University, Uji, 611 Kyoto, Japan |
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Abstract: | The investigation of phase separation processes induced by polymerization reactions of tetramethoxysilane (TMOS) was attempted by a time-resolved light scattering method for TMOS-formamide-water system under the acid-catalyzed condition. Since the early stage of the phase separation exhibits very fast kinetics and weak scattering intensity, the experimental set-up was designed so as to reduce the experimental error and to obtain higher time resolution by using a laser beam expander. For the gels whose morphologies are interconnected structure and aggregates of particles, it was experimentally found that the wavelength of the concentration fluctuation in the early stage of phase separation was time-independent and its amplitude grew exponentially with time. This suggests that these samples phase-separate by spinodal decomposition mechanism. In the later stages of phase separation, the coarsening process and the following structure-freezing process by gel-network formation were observed. |
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Keywords: | porous silica gel light scattering phase separation spinodal decomposition Cahn's theory |
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