| 引用本文: | 袁钦,宋永才.Si(Al)C纤维先驱体聚铝碳硅烷的合成.[J].国防科技大学学报,2017,39(1):182-188.[点击复制] |
| YUAN Qin,SONG Yongcai.Synthesis of precursor polyaluminocarbosilane for Si(Al)C fibers[J].Journal of National University of Defense Technology,2017,39(1):182-188[点击复制] |
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| Si(Al)C纤维先驱体聚铝碳硅烷的合成 |
| 袁钦, 宋永才 |
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(国防科技大学 新型陶瓷纤维及其复合材料重点实验室， 湖南 长沙 410073)
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| 摘要: |
| 采用低分子量固态聚碳硅烷和乙酰丙酮铝为原料，利用Si-H与乙酰丙酮铝之间的交联反应合成适于熔融纺丝的聚铝碳硅烷。研究了反应条件对产物数均分子量、软化点和组成结构的影响及交联反应程度与可纺性之间的关系。实验结果表明：随着反应温度的升高和反应时间的延长，反应程度提高，残余乙酰丙酮基减少，Si-O-Al交联支化结构增多，分子量和软化点增大，可纺性随之下降。当乙酰丙酮铝投料比为8 %时，在370 ℃下反应4~6 h，可得到软化点为206~221 ℃，Al wt%=0.68%，具有良好可纺性的聚铝碳硅烷。 |
| 关键词: 聚铝碳硅烷 SiC纤维 交联反应 可纺性 |
| DOI：10.11887/j.cn.201701028 |
| 投稿日期：2015-08-27 |
| 基金项目:湖南省高校科技创新团队支持计划和国防科技大学创新群体资助项目（CJ 12-01-01） |
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| Synthesis of precursor polyaluminocarbosilane for Si(Al)C fibers |
| YUAN Qin, SONG Yongcai |
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(National Key Laboratory of New Ceramic Fibers and Composites, National University of Defense Technology, Changsha 410073, China)
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| Abstract: |
| A melt-spinnable polyaluminocarbosilane was synthesized via the crosslink reaction between Si-H and acetylacetone aluminum(Ⅲ) by using low-molecular-weight solid polycarbosilane and acetylacetone aluminum(Ⅲ) as starting materials. The effects of reaction conditions on the number average molecular weight, softening point and structure of polyaluminocarbosilane were investigated, and the relationship between the extent of crosslink reaction to the spinnability of polyaluminocarbosilane was also discussed. It was found that elevating the reaction temperature or prolonging reaction time would lead to an enhanced extent of reaction, a gradually decreased acetylacetonate and an increased crosslinked structure of Si-O-Al, resulting in poorer spinnabilty. Polyaluminocarbosilane with softening point of 206~221 ℃, Al wt%=068% and good spinnability was successful synthesized at the optimized reaction conditions of the temperature at 370 ℃, the reaction time at 4~6 h and the mass ratio of acetylacetone aluminum(Ⅲ) at 8 wt%. |
| Keywords: polyaluminocarbosilane SiC fibers crosslink reaction spinnability |
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