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化学学报
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化学学报 ›› 2009, Vol. 67 ›› Issue (11): 1182-1188. 上一篇    下一篇

研究论文

乙烯基硅氮烷-巯基共聚物热裂解研究

陈立新* 王亚洲 宋家乐 张教强

  

  1. 西北工业大学理学院应用化学系 西安 710072

  • 投稿日期:2008-07-14 修回日期:2009-01-16 发布日期:2009-06-14
  • 通讯作者: 陈立新

Pyrolysis of Polysilazane Containing Vinyl-thiol Copolymer

Chen, Lixin* Wang, Yazhou Song, Jiale Zhang, Jiaoqiang   

  1. Department of Applied Chemistry, School of Science, Northwestern Polytechnical University, Xi’an 710072
  • Received:2008-07-14 Revised:2009-01-16 Published:2009-06-14
  • Contact: Chen, Lixin

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采用红外(FTIR)、热失重, 热分析以及质谱联用(TGA-DTA-MS)、X射线衍射仪(XDR)、能谱仪对紫外光固化乙烯基硅氮烷-巯基共聚体系的热裂解行为进行了分析和表征. 结果表明: 300～500 ℃为聚合物裂解反应的主要温度范围. 裂解过程会逸出多种小分子气体, 其中体系中的S元素可能主要是以H2S和SO2和噻吩类的形式逸出; 最终质量保持率为55.3 wt%; 热裂解转化物表观密度出现先下降后上升的趋势, 最终达到2.09 g•cm－3; 在保温2 h的条件下, 热裂解转化物在1400 ℃下生成少量Si3N4晶体, 在1600 ℃下, 热裂解转化物晶体质量组成为m(SiO2)∶m(Si3N4)∶m(SiC)＝3∶26∶71, 结晶度达到91.3%.

关键词: 乙烯基硅氮烷-巯基, 共聚体系, 紫外光固化, 热裂解

The pyrolysis of UV curable polysilazane containing vinyl-thiol copolymer has been analyzed and characterized by FTIR, TGA-DTA-MS, XRD and energy spectrometry. Thermal decomposition of the UV curable copolymer occurred from 300 to 500 ℃. Many different kinds of gas molecules evolved during the pyrolysis, in which S element escaped from the copolymer as H2S, SO2 and thiofuran, with the total weight loss being 44.7 wt%. The density of pyrolysate dropped down at the beginning of pyrolysis, then successively increased, and finally reached 2.09 g•cm－3. Si3N4 crystal could be formed in the pyrolytic process at 1400 ℃ after 2 h and the crystalline degree could reach 91.3% at 1600 ℃ meanwhile. The quality ratio of the final product was m(SiO2)∶m(Si3N4)∶m(SiC)＝3∶26∶71.

Key words: polysilazane containing vinyl-thiol, copolymer, UV-curing, pyrolysis