| 引用本文: | 齐共金,张长瑞,胡海峰,等.全氢聚硅氮烷的合成与表征.[J].国防科技大学学报,2005,27(6):14-17.[点击复制] |
| QI Gongjin,ZHANG Changrui,HU Haifeng,et al.Synthesis and Characterization of Perhydropolysilazane[J].Journal of National University of Defense Technology,2005,27(6):14-17[点击复制] |
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| 全氢聚硅氮烷的合成与表征 |
| 齐共金, 张长瑞, 胡海峰, 曹峰, 王思青, 姜勇刚 |
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(国防科技大学 航天与材料工程学院，湖南 长沙 410073)
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| 摘要: |
| 采用二氢二氯硅烷氨解法合成了氮化硅陶瓷先驱体全氢聚硅氮烷，并用红外光谱、凝胶渗透色谱、热重、X射线衍射和元素分析等进行了表征。所合成的先驱体低聚物的分子骨架为［SiH2NH］n，数均分子量为106，重均分子量为178。固化后的先驱体在氮气下1000℃裂解转变为棕色粉末，陶瓷产率78wt%。将陶瓷产物在氮气下1400℃处理后，其主要成分为α-Si3N4，并含有少量富余硅，化学经验式为SiN1.036O0.060C0.028。陶瓷产物在氮气下1600℃处理后的X射线衍射谱图表明，游离硅已基本消失，α-Si3N4衍射峰加强，但是没有观察到从α-Si3N4到β-Si3N4的相转变。 |
| 关键词: 全氢聚硅氮烷 陶瓷先驱体聚合物 合成 表征 裂解 氮化硅 |
| DOI： |
| 投稿日期：2005-07-16 |
| 基金项目:国防预研基金资助项目 |
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| Synthesis and Characterization of Perhydropolysilazane |
| QI Gongjin, ZHANG Changrui, HU Haifeng, CAO Feng, WANG Siqing, JIANG Yonggang |
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(College of Aerospace and Materials Engineering, National Univ. of Defense Technology，Changsha 410073，China)
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| Abstract: |
| Perhydropolysilazane, a preceramic polymer for silicon nitride ceramics, was synthesized by the ammonolysis of dichlorosilane and characterized by FT-IR, GPC, TG, XRD and elemental analysis. The main backbone of the as-synthesized precursor oligomer was［SiH2NH］n, with a number average molecular weight of 106 and a weight average molecular weight of 178. The cured precursor polymer was converted into brown ceramic powder after pyrolysis at 1000℃ in nitrogen atmosphere, and the ceramic yield was 78wt%. X-ray patterns showed that the main phases of the polymer-derived ceramic product at 1400℃ in nitrogen atmosphere were α-Si3N4 and some free silicon, and the empirical chemical formula for the product was SiN1.036O0.060C0.028 by elemental analysis. After further treatment at 1600℃ in nitrogen atmosphere, extremely weak diffraction peaks for free silicon and intense peaks for α-Si3N4 were observed by XRD patterns, however, there was no phase transition from α-Si3N4to β-Si3N4all along. |
| Keywords: perhydropolysilazane preceramic polymer synthesis characterization pyrolysis silicon nitride |
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