以工业纯无水ZrCl4、正硅酸乙酯(Si(OC2H5)4)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。
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-vothermal treatment and direct reflux process at 700 ℃.