非水解凝胶化工艺对低温合成硅酸锆的影响.pdf

· 383 · 硅 酸 盐 学 报 2011 年 第39 卷第3 期 硅 酸 盐 学 报 Vol. 39 ，No. 3 2 0 1 1 年 3 月 JOURNAL OF THE CHINESE CERAMIC SOCIETY March ，2011 非水解凝胶化工艺对低温合成硅酸锆的影响 江伟辉，张 缇，朱庆霞，刘健敏 (景德镇陶瓷学院材料科学与工程学院；江西省先进陶瓷材料重点实验室，江西 景德镇 333001) 摘 要：以工业纯无水ZrCl 、正硅酸乙酯(Si(OC H ) )为前驱体，LiF 为矿化剂，通过非水解溶胶–凝胶法低温合成出硅酸锆粉体。应用热重–差热分 4 2 5 4 析、X 射线衍射和透射电子显微镜等研究了不同非水解凝胶化工艺对低温合成硅酸锆的影响。结果表明：通过容弹工艺无法低温合成硅酸锆；采用回 流工艺虽然能低温合成出硅酸锆粉体，但所制得的硅酸锆晶体轮廓不清、发育较差。只有将回流和容弹工艺相结合才能在700 ℃合成出充分发育的四 方柱状硅酸锆晶体。 关键词：硅酸锆；非水解溶胶–凝胶法；凝胶化工艺；低温合成 中图分类号：O782 文献标志码：A 文章编号：0454–5648(2011)03–0383–04 Effect of Non-Hydrolytic Gelation Process on Synthesis of Zircon at Low Temperature JIANG Weihui ，ZHANG Ti ，ZHU Qingxia ，LIU Jianmin (School of Material Science and Engineering, Jingdezhen Ceramic Institute; Jiangxi Key Laboratory of Advanced Ceramic Materials, Jingdezhen 333001, Jiangxi, China) Abstract: Zircon powder was synthesized at a low temperature via a non-hydrolytic sol–gel route, using zirconium tetrachloride and tetraethoxysilane as precursors, lithium fluoride as a mineralizer. The effect of the nonhydrolytic gelation process on the zircon syn- thesis at a low temperature was investigated by thermogravimetry–differential thermal analysis, X-ray diffraction and transmission electron microscope. The results indicate that the zircon can not be synthesized by a direct solvothermal treatment at a low tempera- ture, and the direct reflux process can result in the formation of the zircon with fuzzy crystal configuration due to the incomplete crystal growth. The zircon particles with the tetragonal columnar shape can be synthesized by the combined processes of direct sol- vo