新型含锆硅炔陶瓷材料的制备与性能

Preparation and Properties of New Zirconium-Containing Silylacetylene Precursor for Ceramic Material

以甲基氢二氯硅烷(MeHSiCl2)、正丁基锂(n-BuLi)、三氯乙烯(HClC CCl2)与四氢铝锂(LiAlH4)为原料制备主链含H—Si—C≡C的硅炔聚合物(HS),将硅源与锆源(HG)进行共混,制备了一种新型复合陶瓷前驱体(GP)。采用傅里叶变换红外光谱(FT-IR)和核磁共振(NMR)对HS结构进行表征;利用FT-IR、差示扫描量热分析(DSC)与热失重分析(TGA)分别探讨GP固化行为及其耐热性能;通过X射线衍射(XRD)与激光显微拉曼光谱(Raman)等研究GP的陶瓷化性能。结果表明,GP具有优良的热稳定性能与陶瓷化性能,在1 600℃氩气气氛下保温3h可得到ZrC-ZrO2-SiC复相陶瓷,质量保留率达到75.64%。

A novel complex phase ceramic precursor(GP)was prepared by adding zirconium based powder of polymer(HG)into the silicon source(HS),a silylacetylene precursor with H—Si—C≡C backbone which was prepared from the reaction of n-BuLi,trichloroethylene,methyl hydrogen dichlorosilane and lithium aluminum hydride.The structure of HS was characterized by FT-IR and NMR.The curing behavior and thermal oxidation performance of GP were fully investigated by FT-IR,DSC and TGA,while the ceramic performance was investigated by XRD and Raman.The results showed that GP exhibited excellent thermal stability and ceramic performance,and it could turn into complex phase ceramics composed of ZrC-ZrO2-SiC with a yield of 75.64% after being sintered at 1 600 ℃in Ar for 3h.