高等学校化学学报

高等学校化学学报 ›› 2009, Vol. 30 ›› Issue (12): 2525.

• 研究论文 • 上一篇    下一篇

基于液态聚碳硅烷的聚铝碳硅烷的合成与表征

杨景明, 杨露姣, 余煜玺, 程璇, 张颖   

  1. 厦门大学材料学院材料科学与工程系, 特种先进材料福建省重点实验室, 厦门 361005
  • 收稿日期:2009-02-23 出版日期:2009-12-10 发布日期:2009-12-10
  • 通讯作者: 张颖, 男, 博士, 教授, 博士生导师, 主要从事材料微结构与性能研究, E-mail: yzh@xmu.edu.cn
  • 基金资助:

    特种先进材料福建省重点实验室(批准号: 2006L2003)和国家自然科学基金重点项目(批准号: 50532010)资助.

Synthesis and Characterization of Liquid Polycarbosilane-derived Polyaluminocarbosilane

YANG Jing-Ming, YANG Lu-Jiao, YU Yu-Xi, CHENG Xuan, ZHANG Ying*   

  1. Fujian Key Laboratory of Advanced Materials, Department of Materials Science and Engineering, College of Materials, Xiamen University, Xiamen 361005, China
  • Received:2009-02-23 Online:2009-12-10 Published:2009-12-10
  • Contact: ZHANG Ying, E-mail: yzh@xmu.edu.cn
  • Supported by:

    特种先进材料福建省重点实验室(批准号: 2006L2003)和国家自然科学基金重点项目(批准号: 50532010)资助.

PDF (PC)

被引次数

8

摘要：

采用液态聚碳硅烷与乙酰丙酮铝在常压下反应合成了具有不同铝含量的聚铝碳硅烷(PACS), 由于不需要循环回流过程, 因此该方法简单方便, 安全性高. 在与合成聚铝碳硅烷相同的条件下, 对单纯的液态聚碳硅烷原料进行保温处理, 所得产物的分析表征结果显示, 该原料在反应条件下基本保持稳定, 不会自聚或者裂解. 不同铝含量的聚铝碳硅烷的元素分析结果表明, 随着乙酰丙酮铝加入量的增加, 聚铝碳硅烷中的铝含量增加, 同时氧含量增加, 氢含量减少, 且乙酰丙酮铝中的铝元素几乎全部引入到液态聚碳硅烷中. GPC分析结果显示, 随着铝含量的增大, PACS的数均分子量增大, 分子量分布变宽. 红外光谱和核磁共振波谱分析结果表明, 液态聚碳硅烷与乙酰丙酮铝的反应主要以消耗Si—H键的方式进行, 铝元素以AlO4, AlO5和AlO6 3种配位形式存在, 同时形成Si—O—Al交联键, 使得聚铝碳硅烷的分子量增大, 分子量分布变宽.

关键词: 液态聚碳硅烷; 聚铝碳硅烷; 乙酰丙酮铝; 元素分析; 结构表征

Abstract:

Polyaluminocarbosilanes(PACS) with different Al contents were synthesized by reacting liquid polycarbosilane(LPCS) with aluminum acetylacetonate[Al(AcAc)3]. Compared with those reported in literatures, this route is considered to be more convenient and safer since no circulating reflux is needed. It was shown that the composition and structure of LPCS heated and kept at the synthesis temperature of PACS remained fairly stable. The chemical elemental analysis results of PACS indicated that through this route the Al contents were almost fully introduced into PACS from Al(AcAc)3, and with the increasing of Al contents, the O contents also increased. Furthermore, the formation of AlO4, AlO5 and AlO6 was confirmed by 27Al MAS NMR results. On the base of the structure analysis it was suggested that LPCS reacted with Al(AcAc)3 by consuming Si—H bonds. Then Si—O—Al crosslinking bonds were formed, leading to the increases of the number average molecular weight and the polydispersion index in molecular weight with the increase of Al contents in PACS.

Key words: Liquid polycarbosilane; Polyaluminocarbosilane; Aluminum acetylacetonate; Elemental analysis; Structure characterization

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