ポリシロキサザンの調製とその窒化酸化ケイ素への変換過程(<ゲストエディターによる特集>有機-無機変換プロセス)

概要

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Cyclic and bicyclic oligosiloxazanes were synthesized by the reaction of 1,3-diamino-1,3-di-t-butoxy-1,3-dimethyldisiloxane with 1,1,3,3-tetraisocyanato-1,3-dimethyl-1,3-disiloxane (M-TIDS) in 1:1 and 1:2 molar ratios, respectively. Based on these results, polysiloxazane M-PSZ was prepared by the ammonolysis of M-TIDS in tetrahydrofuran (THF) at 213K. The structure and stability against the gelation of M-PSZ were found to be dependent on the temperature and polarity of the solvents. The molecular weight of M-PSZ was increased by aging a THF solution of M-PSZ at room temperature. A maximum weight average molecular weight of 70000 was observed for M-PSZ, for which a dilute solution was stable over 6 months. Silicon oxynitride was prepared by the pyrolysis of M-PSZ under an ammonia atmosphere. The ceramization process was monitored by infrared and nuclear magnetic resonance spectra, which showed the replacement of a methyl group with an amino group following a condensation reaction to provide silicon oxynitride at 1173K.
社団法人日本セラミックス協会の論文
2006-06-01