无机材料学报

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混杂聚硼硅氮烷的陶瓷化过程研究

李斌, 张长瑞, 曹峰, 王思青, 姜勇刚   

  1. 国防科学技术大学航天与材料工程学院CFC重点实验室, 长沙 410073
  • 收稿日期:2007-03-18 修回日期:2007-04-24 出版日期:2008-03-20 网络出版日期:2008-03-20

Ceramization of Hybrid Polyborosilazanes

LI Bin, ZHANG Chang-Rui, CAO Feng, WANG Si-Qing, JIANG Yong-Gang   

  1. State Key Laboratory of Advanced Ceramic Fibers & Composites,
    College of Aerospace & Materials Engineering, National University of Defense Technology, Changsha 410073, China
  • Received:2007-03-18 Revised:2007-04-24 Published:2008-03-20 Online:2008-03-20

摘要: 合成了新型的陶瓷先驱 体混杂聚硼硅氮烷(H-PBSZ), 分析了其结构, 并采用TG-DTA、FT-IR、XRD以及SEM等分析手段对其裂解过程进行了研究. 结果表明, H-PBSZ结构中含有B-N、Si-N、B-H、N-H、Si-H等化学键, 随着裂解温度的升高, 含氢键逐渐减少直至消失, 最终得到BN和Si3N4的混合物. 在裂解过程中, 失重主要发生在100~400℃之间, 陶瓷产率约为83wt%. 裂解产物的结晶程度随着温度的升高逐渐增强, 800℃的产物基本上为无定形态, 微观形貌主要以球形颗粒为主; 1600℃的产物则已经晶化, 可以观察到层片状结构的h-BN及少量的α-Si3N4晶粒.

关键词: 聚硼硅氮烷, 裂解, 陶瓷化, 氮化硼

Abstract: New preceramic polymers-hybrid polyborosilazanes (H-PBSZ) were synthesized and characterized. The ceramization process of H-PBSZ was investigated by TGA, FT-IR, XRD and SEM. The results show that there exist bonds of B-N, Si-N, B-H, N-H, Si-H in the structures of H-PBSZ. With the increase of pyrolysis temperature, the bonds contained H atoms decrease till they disappear. The ultimate product is a mixture comprised of BN and Si3N4 . The loss of weight in the process of pyrolysis mainly occurs between 100℃ and 400℃, and the ceramic yield is about 83wt%. The pyrolytic product is crystallized as the temperature increases. The products pyrolyzed at 800℃ are almost amorphous with mainly spherical particles, while those pyrolyzed at 1600℃ are well crystallized, and h-BN crystal flakes and α-Si3N4 grains can be observed by SEM.

Key words: polyborosilazane, pyrolysis, ceramization, boron nitride

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