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采用沉淀共聚合方法制备了聚乙烯基硅氮烷腈(PVSZ)微球。其中乙烯基环硅氮烷与二乙烯基苯为共单体,偶氮二异丁腈(AIBN)为引发剂,乙腈为溶剂。聚合反应12h制备的微球表面光滑,粒径为700 nm~780 nm,分散性良好。能量色谱(EDS)证明微球包含Si、C、N元素;红外光谱(FT-IR)表明微球化学结构是PVSZ;微球1000℃热解,陶瓷产率为35%。热解温度低于1300℃时,PVSZ微球的热解产物能完整地保持球形结构、表面光滑;X射线衍射(XRD)表明产物呈非晶态;热解温度1500℃时,球形结构破坏,产物结晶,生成了Si3N4晶粒。

The polyvinylsilazane (PVSZ) microspheres were prepared by co-precipitation polymerization: vinylsilazane and divinylbenzene as co-monomer, azodiisobutyronitrile (AIBN) as initiator, and acetonitrile as solvent. After reaction 12h, the microspheres with a smooth surface have completely formed, which have an average diameter size between 700 nm and 780 nm. The energy dispersive spectrometer (EDS) spectrum reveals that the microspheres consist of silicon, carbon, and nitrogen element. The PVSZ microspheres were pyrolyzed at 1000 ℃, and the ceramic yield was 35%. When pyrolysis temperature 〈 1300 0(2, the pyrolyzed PVSZ microspheres holds integrally spherical architecture, which was amorphous phase structure. At 1500℃, the pyrolysis products were composed of grains with different sizes, and the amorphous phase partially crystallizes to produce Si3N4 phase.

参考文献

[1] Kroke E.;Konetschny C.;Lecomte E.;Fasel C.;Riedel R.;Li YL. .Silazane derived ceramics and related materials [Review][J].Materials Science & Engineering, R. Reports: A Review Journal,2000(4/6):97-199.
[2] Choi J.;Kwak SY.;Kang S.;Lee SS.;Park M.;Lim S.;Kim J.;Choe CR. Hong SI. .Synthesis of highly crosslinked monodisperse polymer particles: Effect of reaction parameters on the size and size distribution[J].Journal of Polymer Science, Part A. Polymer Chemistry,2002(23):4368-4377.
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