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化学学报
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化学学报 ›› 2011, Vol. 69 ›› Issue (16): 1936-1940. 上一篇    下一篇

研究论文

新型氮化硼陶瓷纤维先驱体——含硅聚硼氮烷的合成与表征

李文华*，王军，谢征芳，王浩，唐云   

  1. (国防科技大学新型陶瓷纤维及其复合材料国防科技重点实验室 长沙 410073)
  • 投稿日期:2011-01-22 修回日期:2011-05-17 发布日期:2011-06-07
  • 通讯作者: 李文华 E-mail:wenhua_cn_kd@yahoo.com.cn

Synthesis and Characterization of Silicon-containing Polyborazine to Boron Nitride Ceramic Fiber

LI Wen-Hua, WANG Jun, XIE Zheng-Fang, WANG Hao, TANG Yun   

  1. (State Key Laboratory of Advanced Ceramic Fibers & Composites, National University of Defense Technology, Changsha 410073)
  • Received:2011-01-22 Revised:2011-05-17 Published:2011-06-07
  • Contact: Wen-Hua LI E-mail:wenhua_cn_kd@yahoo.com.cn

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1282

被引次数

16

以三氯化硼、六甲基二硅氮烷为起始原料, 采用一步法合成了一种新型含硅氮化硼陶瓷纤维先驱体——含硅聚硼氮烷. 该法合成工艺简单, 且合成收率约为87%(质量分数). 采用元素分析、傅立叶红外光谱、核磁共振波谱、热机械分析、动态流变分析等对含硅聚硼氮烷的组成、结构和性能进行了表征. 结果表明, N—B为含硅聚硼氮烷先驱体的骨架结构, 其中, B, N主要以硼氮六环形式存在, 而Si则以Si—CH3, Si—N形式存在. 该先驱体软化点为110 ℃, 具有优良的成型性, 在190 ℃的N2气氛中可纺丝得到20～25 μm的有机纤维.

关键词: 含硅聚硼氮烷, 先驱体转化法, 陶瓷先驱体, 合成

Silicon-containing polyborazine, a novel precursor to boron nitride ceramic fibers, was synthesized via “one-pot” approach with a yield of about 87% (w%) using boron trichloride (BCl3) and hexamethydisilazane (HMDZ) as the starting materials. The chemical composition, structure and properties of the obtained precursor were investigated using EA, FT-IR, NMR, TMA and dynamic rheological measurement. The results indicate that the backbone of the polymer is N—B linkage in the form of borazine and Si is in the form of Si—CH3 and Si—N in the pendant or end group. The softening point of the precursor is 110 ℃. The precursor shows good processability and the precursor fibers with diameters of 20～25 μm can be obtained by melt spinning at 190 ℃ in N2 atmosphere.

Key words: silicon-containing polyborazine, polymer derived ceramic, preceramic polymer, synthesis