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Oligomeric Alkoxysilanes with Cagelike Hybrids as Cores: Designed Precursors of Nanohybrid Materials
Authors:Hideki Kuge  Yoshiaki Hagiwara  Atsushi Shimojima  Dr.  Kazuyuki Kuroda  Prof.
Affiliation:1. Department of Applied Chemistry, Waseda University, Ohkubo‐3, Shinjuku‐ku, Tokyo, 169‐8555, Japan, Fax: (+81)?3‐5286‐3199;2. Core Research for Evolutional Science and Technology (CREST), Japan Science and Technology Agency (JST), Honcho 4‐1‐8, Kawaguchi‐shi, Saitama, 332‐0012, Japan;3. Department of Chemical System Engineering, The University of Tokyo, Hongo‐7, Bunkyo‐ku, Tokyo 113‐8656, Japan;4. Kagami Memorial Laboratory for Materials Science and Technology, Waseda University, Nishiwaseda‐2, Shinjuku‐ku, Tokyo, 169‐0051, Japan
Abstract:Well‐defined alkoxysilane oligomers containing a cagelike carbosiloxane core were synthesized and used as novel building blocks for the formation of siloxane‐based hybrid networks. These oligomers were synthesized from the cagelike trimer derived from bis(triethoxysilyl)methane by silylation with mono‐, di‐, and triethoxychlorosilanes ((EtO)nMe3?nSiCl, n=1, 2, and 3). Hybrid xerogels were prepared by hydrolysis and polycondensation of these oligomers under acidic conditions. The structures of the products varied depending on the number of alkoxy groups (n). When n=2 and 3, microporous xerogels (BET surface areas of 820 and 510 m2 g?1, respectively) were obtained, whereas a nonporous xerogel was obtained when n=1. 29Si NMR spectroscopic analysis suggested that partial rearrangement of the siloxane networks, which accompanied the cleavage of the Si–O–Si linkages, occurred during the polycondensation processes. By using an amphiphilic triblock copolymer surfactant as a structure‐directing agent, hybrid thin films with a 2D hexagonal mesostructure were obtained when n=2 and 3. These results provide important insight into the rational synthesis of molecularly designed hybrid materials by sol–gel chemistry.
Keywords:mesoporous materials  organic–  inorganic hybrid composites  self‐assembly  siloxanes  sol–  gel processes
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