低氧含量液态超支化聚碳硅烷的合成与陶瓷化研究  

Synthesis and pyrolytic conversion of a hyperbranched liquid polycarbosilane with low oxygen content

作　　者：李然[1,2] 詹俊英[2] 周聪[2] 余兆菊[2] 丁马太[2,3] 夏海平[1,2] 

机构地区：[1]厦门大学化学化工学院,福建厦门361005 [2]厦门大学材料学院高性能陶瓷纤维教育部重点实验室,福建厦门361005 [3]龙岩学院化学与材料工程学院,福建龙岩364000

出　　处：《功能材料》2010年第12期2166-2168,2173,共4页Journal of Functional Materials

基　　金：国家自然科学基金资助项目(50802079);航空科学基金资助项目(2008ZH68005)

摘　　要：以甲醇对氯甲基三氯硅烷(Cl3SiCH2Cl)进行烷氧化反应,然后经过格氏偶联反应和还原反应,制备了低氧含量液态超支化聚碳硅烷(HBPCS)。通过凝胶渗透色谱法(GPC)、核磁共振(NMR)以及元素分析对由此制备的HBPCS进行表征。结果表明,提高烷氧化比例,可以有效抑制溶剂四氢呋喃开环的副反应,降低先驱体氧含量。通过热失重分析(TGA)和X射线衍射(XRD)分别对HBPCS的热性能及相应陶瓷在高温下的结晶行为进行研究。A hyperbranched liquid polycarbosilane（HBPCS）with a low oxygen content was prepared by Grignard coupling of partially methoxylated chloromethyltrichlorosilane,followed by reduction with lithium aluminum hydride.The as-synthesized HBPCS was characterized by gel permeation chromatography（GPC）,nuclear magnetic resonance（NMR）spectroscopy and elemental analysis.It is suggested that side reactions of THF and chlorosilanes can be avoided with the increase of methoxylation ratio.Less oxygen is expected in the precursors.Pyrolysis behavior of the HBPCS and crystallization behavior of the resultant ceramic were studied by means of thermal gravimetric analysis（TGA）and X-ray diffraction（XRD）,respectively.

关 键 词：烷氧化 聚碳硅烷 先驱体法 碳化硅 超支化 

分 类 号：TQ163[化学工程—高温制品工业] TL344[核科学技术—核技术及应用]