文献类型：期刊文献

中文题名：高耐热氧化稳定性硅炔聚合物的制备与表征

英文题名：Preparation and characterization of high heat resistant oxidation stability of silicon and acetylene polymer

作者：胡浩[1];周权[1];刘帅帅[1];倪礼忠[1]

机构：[1]华东理工大学材料科学与工程学院特种功能高分子材料及相关技术教育部重点实验室,上海200237

年份：2017

卷号：40

期号：1

起止页码：90

中文期刊名：固体火箭技术

外文期刊名：Journal of Solid Rocket Technology

收录：CSTPCD;;Scopus;北大核心:【北大核心2014】；CSCD:【CSCD2017_2018】；

基金：国家自然科学基金(51573044);上海市自然科学基金(15zr1409800)

语种：中文

中文关键词：硅炔聚合物;耐热氧化;陶瓷化

外文关键词：silicon and acetylene polymer; heat resistant oxidation; ceramization

摘要：以二甲基二氯硅烷(Me_2SiCl_2)、三氯乙烯(HClC=CCl_2)和正丁基锂(n-BuLi)为原料,通过偶联反应及LiAlH_4还原制备主链含有Si—C≡C的硅炔聚合物(PSA)。采用FT-IR和NMR对其结构进行表征,利用DSC与TGA分别探讨其固化行为及耐热性能;TGA测试表明,PSA树脂具有良好的耐热及热稳定性能,在氮气和空气气氛下T_(d5)(质量损失5%的温度)分别达到617℃和599℃,1 000℃时的质量保留率分别为86.6%和75.6%。通过XRD与Raman研究PSA的陶瓷化性能,陶瓷化性能结果表明,PSA结构中含有C≡C键,在固化过程中交联形成致密的三维网状结构,赋予PSA优异的耐热性能,且在1 600℃氩气气氛下得到高度结晶的SiC陶瓷。
Precursor polycarbosilane containing acetylenic and Si—CH_3group（PSA） was prepared successfully by the coupling reaction,using dimethyldichlorosilane,trichlorethylene and n-butyl lithium as starting material.The structure of PSA was characterized by FT-IR; the curing behavior of PSA was analyzed by DSC and its thermal stability was studied by TGA; TGA test indicated that PSA resin had excellent thermal stability.Under nitrogen atmosphere,the temperature of 5% mass loss（Td5） was 617 ℃and the residual of mass at 1 000 ℃ was 86.6%.Under air,the Td5 was 599 ℃ and the highest mass residual ratio was 75.6%based on the initial mass at 1 000 ℃.Its ceramization performance was investigated by XRD with Raman.The results show that PSA can form dense three-dimensional network structure by cross-linking in curing process and possess excellent heat resistance owing to the alkynyl in the molecular structure,and high crystallinity of Si C ceramics at 1 600 ℃ under argon atmosphere.