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作 者:程祥珍[1] 宋永才[1] 谢征芳[1] 肖加余[1] 王应德[1]
机构地区:[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
出 处:《硅酸盐学报》2004年第11期1352-1355,1360,共5页Journal of The Chinese Ceramic Society
基 金:国防预研和国家自然科学基金(50082007)资助项目。
摘 要:以聚二甲基硅烷(PDMS)为原料,在高压釜内高温高压反应合成了聚碳硅烷(PCS)先驱体,经多孔熔融纺丝制备了PCS纤维。研究了不熔化温度、时间对PCS纤维质量、Si—H键反应程度、凝胶含量及氧含量的影响。研究表明:在不熔化过程中,PCS结构中的Si—H键与氧反应,在PCS分子间形成Si—O—Si交联结构;随着不熔化温度的提高,时间的延长,PCS纤维的质量、Si—H键反应程度、凝胶含量、氧含量均逐渐增加,并逐渐趋于稳定。高压合成的PCS不溶化反应活性较高,引入少量的氧(4%~7%)即可实现不熔化。The polycarbosilane (PCS), as precursor of SiC fiber, was synthesized in an autoclave by thermal decomposition of polydimethylsilane (PDMS) and PCS green fiber was prepared by melt-spinning. The influences of curing time and temperature on the mass, Si-H bond reaction degree, gel content and oxygen content of PCS fiber were investigated. The results show that Si-H bond in the molecular structure of PCS reacts with oxygen during the curing process and Si-O-Si cross linked structures are therefore formed among PCS molecules. With the increase of curing temperature and extension of curing time, the mass, Si-H bond reaction degree, gel content, and oxygen content of PCS fiber increase gradually until come to stable. The curing reactivity of the PCS synthesized at high pressure is higher than that synthesized under normal pressure. Therefore less oxygen, 4%-7% (in mass fraction), can realize the curing of the green fiber.
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