高等学校化学学报 ›› 2013, Vol. 34 ›› Issue (10): 2415.doi: 10.7503/cjcu20130520

• 高分子化学 • 上一篇    下一篇

高硼含量的SiC陶瓷先驱体的合成和表征

朱旖华, 王浩, 邵长伟   

  1. 国防科学技术大学新型陶瓷纤维及其复合材料重点实验室, 长沙 410073
  • 收稿日期:2013-05-31 出版日期:2013-10-10 发布日期:2013-10-10
  • 作者简介:王浩,男,博士,研究员,主要从事陶瓷先驱体及陶瓷纤维研究.E-mail:whlucky2002@hotmail.com
  • 基金资助:

    国家自然科学基金(批准号:51172280, 51203184)、国家“八六三”计划(批准号:2012AA03A210)、湖南省杰出青年基金项目(批准号:12JJ1008)、湖南省高校科技创新团队支持计划和国防科技大学创新群体资助.

Synthesis and Characterization of SiC Ceramic Precursor with High Boron Content

ZHU Yi-Hua, WANG Hao, SHAO Chang-Wei   

  1. National University of Defense Technology, Science and Technology on Advanced Ceramic Fibers and Composites Laboratory, Changsha 410073, China
  • Received:2013-05-31 Online:2013-10-10 Published:2013-10-10

摘要:

采用经典硼氢化反应, 通过硼烷二级硫醚(BH3·SMe2)与二甲基二乙烯基硅烷(DVS)反应, 合成了聚硼碳硅烷(PBCS)陶瓷先驱体, PBCS在氮气中经高温裂解得到了高硼含量的SiC陶瓷.利用红外光谱、核磁共振波谱和热重分析对聚合物的结构和性能进行了表征; 利用元素分析、X射线衍射和扫描电子显微镜对聚合物的裂解产物进行了分析.结果表明, 聚合物的结构中含有B—C, Si—C和C—H键, 在1000℃氮气气氛中, 其陶瓷产率在50%以上.陶瓷产物在1100℃以无定形态存在, 硼含量高达6.46%, 在1300℃时出现明显结晶, 形成B2O3, C和β-SiC三相组成的多元复相陶瓷, 在1500℃以下陶瓷产物表面光滑, 结构致密.

关键词: 硼氢化反应, 聚硼碳硅烷, 裂解, 先驱体转化陶瓷

Abstract:

Polyboroncarbosilane(PBCS) was synthesized via hydroboration BH3·SMe2 and dimethyldivinylsilane(DVS) as starting materials. SiC ceramics with high boron content were obtained by pyrolysis of PBCS in N2. The structures and properties of the polymers were investigated via FTIR, NMR, TGA; and their pyrolytic products were investigated via elemental analysis, X-ray diffraction and SEM. The results indicate that B—C, Si—C, C—H bonds exist in the structure of PBCS; and ceramic yields for the precursor in N2 are up to 50%. The ceramics exist in amorphous state with the B content of 6.46% after pyrolyzed at 1100℃, and crystallize distinctly to form a multiple phases of B2O3, C and β-SiC at 1300℃. The results show a glazed surface and a dense structure when treated below 1500℃.

Key words: Hydroboration, Polyboroncarbosilane, Pyrolysis, Polymer derived ceramics

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