以炔基聚硅烷(PEPSI)为硅源和聚锆氧烷(PNZ)为锆源,制备了SiC-ZrC复相陶瓷先驱体。SiC-ZrC先驱体通过炔基的聚合、硅氢加成和锆氧烷与硅氢键的缩合,在260~340℃热固化。SiC-ZrC先驱体中加入乙酰丙酮镍(NIAA),会降低先驱体的固化温度、提高陶瓷产率和促进陶瓷结晶,表明乙酰丙酮镍(NIAA)对SiC-ZrC先驱体具有催化固化和促进结晶的作用。N2气氛下,先驱体PEPSI-0.8PNZ-NIAA(PEPSI∶PNZ∶NIAA质量比为1.00∶0.80∶0.01)经1 600℃裂解的陶瓷产率为43%。XRD和SEM-EDS结果表明,SiC-ZrC先驱体在1 600℃下发生碳热还原反应,得到了纯度较高的SiC-ZrC复相陶瓷,Si、Zr和C元素在陶瓷材料中均匀分布。SiC-ZrC先驱体有望作为理想的高温陶瓷基体树脂。
A novel kind of SiC-ZrC multi-phase ceramic precursor was prepared by reactive blending of Ethynylpolysilane ( PEPSI, as silicon source) and Polyzirconoxanesal( PNZ, as zirconium source). The thermal cure of SiC-ZrC precursor was realized by polymerization of ethynyl groups, hydrosilylation and condensation of zirconate with Si-H at 260- 340 ℃. NIAA can reduce the curing temperature of the precursors, accelerate the pyrolysis and crystallization, and improve the ceramic yields, which shows that NIAA has an obvious catalytical effect on thermal cure and pyrolysis. For the optimized formula (PEPSI-0.8PNZ-NIAA), the mono- lithic ceramic was formed upon pyrolysis at 1 600 % in a yield of 43% under N2 atmosphere. XRD and SEM-EDS results show that: SiC-ZrC precursor is converted into almost pure SiC-ZrC multi-phase ceramic upon heat treatment at 1 600 ~C. Porous ceramic tex- ture can occur due to the carbon thermal reduction, which generate carbon oxides. The Si, Zr and C elements are distributed uni- formly in the obtained SiC-ZrC ceramic. The SiC-ZrC precursor is a promising candidate for the production of ultra-high temperature