Heat-Treatment Effects on Polyorganosiloxane Spherical Particles Prepared in W/O Emulsion

Taichi MATSUMOTO; Yasushi TAKAYAMA; Noriyuki WADA; Hiroaki ONODA; Kazuo KOJIMA; Hideo YAMADA; Hajimu WAKABAYASHI

doi:10.14852/jcersjsuppl.112.0.S239.0

Journal of the Ceramic Society of Japan, Supplement 112-1, PacRim5 Special Issue

Session ID : 3

DOI https://doi.org/10.14852/jcersjsuppl.112.0.S239.0

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Host: The Ceramic Society of Japan

Co-host: Iketani Science and Technology Foundation, International Ceramic Federation, Commemorative Organization for the Japan World Exposition '70, The American Ceramic Society, The Australasian Ceramic Society, The Chinese Ceramic Society, The Korean Ceramic Society, Joint Research Consortium of Synergy Ceramics/Fine Ceramics Research Association, Nanotechnology Researchers Network Center of Japan, The Special Coordination Funds for Promoting Science and Technology, Japan National Tourist Organization, Aichi Prefectural Government, CASIO SCIENCE PROMOTION FOUNDATION, DAIKO FOUNDATION, Nagoya Convention and Visitors Bureau, The Asahi Glass Foundation, The Kao Foundation For Arts And Sciences, The Murata Science Foundation, The Ogasawara Foundation for the Promotion of Science & Engineering, ASAHI GLASS CO., LTD. Research Center, CENTRAL GLASS CO., LTD., ELECTRIC GLASS INDUSTRY ASSOCIATION OF JAPAN (EGAJ), Hattori Company, Ltd., Hitachi Research Laboratory, Hitachi, Ltd., HOYA CORPORATION, INAX Corporation, ITOCHU CERATECH CORP., Japan Cement Association, KYOCERA Corporation, KYUSHU REFRACTORIES CO., LTD., MINO CERAMIC CO., LTD., Murata Manufacturing Co., Ltd., NGK INSULATORS LTD., NGK SPARK PLUG CO., LTD., NICHIAS Corporation, NIKKO COMPANY, Nippon Electric Glass Co., Ltd., Nippon Sheet Glass Co., Ltd., NORITAKE CO., LIMITED, Tokuyama Corporation, TOTO LTD.

Papers

Heat-Treatment Effects on Polyorganosiloxane Spherical Particles Prepared in W/O Emulsion

Taichi MATSUMOTO, Yasushi TAKAYAMA, Noriyuki WADA, Hiroaki ONODA, Kazuo KOJIMA, Hideo YAMADA, Hajimu WAKABAYASHI

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Keywords: Sol-gel process, Heat-treatment, Polyorganosiloxane, W/O emulsion, Spherical particle, ²⁹Si MAS NMR, Polymerization, Shrinkage

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Abstract

Monodispersed micro polyorganosiloxane spherical particles synthesized from methyltrimethoxysilane in W/O emulsion consisting of sorbitantrioleate (SPAN85), n-octane, and H₂O were heat treated from 100 to 600°C in the air, and examined from SEM, NMR, FT-IR, and specific surface area measurements. The heating process is characterized as follows. Before the formation of the Si-O-Si linkage by oxidation of CH₃ in Si-CH₃ near 410°C, silica network in the particles consists of only T² and T³ units and the transformation of T² into T³ and the shrinkage of the particles were observed up to 400°C, specific surface area showing the maximum value (18 m² g^-1) for the particles heat treated at 300°C. We concluded that the origin of the change in thespecific surface area was related to the changes in both the degree of polymerization and the shrinkage. On the other hand, after the formation of the new Si-O-Si linkage by the oxidation, silica network consists of only Q units and the particles were thermally stable with almost constant diameter and specific surface area.

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