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硼氢化反应合成聚硼硅氮烷和热压成型-热解制备SiBCN陶瓷

SYNTHESIS OF POLYBOROSILAZANE VIA HYDROBORATION AND WARM PRESSING-PYROLYSIS TO SiBCN CERAMICS

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【作者】 孟凡星唐宁苏冬李亚利

【Author】 MENG Fanxing,TANG Ning,SU Dong,LI Yali (Key Laboratory of Advanced Ceramics and Machining Technology,Ministry of Education,Tianjin University; School of Materials Science and Engineering,Tianjin University,Tianjin 300072,China)

【机构】 天津大学先进陶瓷与加工技术教育部重点实验室天津大学材料科学与工程学院

【摘要】 对甲基乙烯基二氯硅烷(MeViSiCl2)进行氨解形成聚甲基乙烯基硅氮烷(PMVS),进而用二甲基硫醚硼烷(BH3-SMe2)和PMVS进行硼氢化反应,合成出SiBCN陶瓷的前驱体聚硼硅氮烷(polyborosilazane,PBSZ)。Fourier红外光谱分析表明:合成的PBSZ中有C-B-C和Si-N特征吸收峰,分别对应HC-B(CH)-CH和≡Si-NH-基团;11B和29Si的核磁共振分析产物中有BC3,SiN2C2,SiN3C和SiC3N等结构单元,这些光谱结果表明合成的产物为PBSZ。对PBSZ热压成型,在1000℃氩气中热解制备出SiBCN陶瓷体。PBSZ的热重分析表明:氩气中1300℃热解的陶瓷产率为52.6%。陶瓷局部致密,表明用前驱体热解法有望获得致密的SiBCN陶瓷体。

【Abstract】 Methylvinyldichlorosilane (MeViSiCl2) was ammonolyzed to form polymethylvinylsilazane (PMVS),and then polyboro-silazane (PBSZ) precursor of SiBCN ceramic was synthesized by the reacting between PMVS and borane dimethylsulfide (BH3-SMe2). Fourier transform infrared spectral analysis of PBSZ shows characteristic absorption bands for C—B—C and Si-N bonds corresponding to HC—B(CH)—CH and ≡Si—NH—functional groups,respectively. Solid-state nuclear magnetic resonance (NMR) (11B-NMR,29Si-NMR) analyses show that the PBSZ has the chemical shifts for BC3,SiN2C2,SiN3C and SiC3N units,and it indicates that the synthesized product is PBSZ. The bulk SiBCN ceramics were prepared via pyrolyzing the PBSZ precursor hot-pressing at 1 000 ℃ in Argon. Thermogravimetric analysis of PBSZ shows that the yield of SiBCN ceramic prepared by pyrolyzing the PBSZ precursor at 1 300 ℃ in argon is 52.6%. The ceramic is locally dense,indicating that it is possible to form compact bulk ceramic by the warm-pressing and pyrolysis process.

【基金】 国家重大基础研究项目(2010CB934700);国家杰出青年科学基金(50625207)资助项目
  • 【文献出处】 硅酸盐学报 ,Journal of the Chinese Ceramic Society , 编辑部邮箱 ,2010年08期
  • 【分类号】TQ174.6
  • 【被引频次】11
  • 【下载频次】598
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