硅酸盐学报

非水解溶胶-凝胶法制备硅酸锆晶须

单位：1. 景德镇陶瓷学院材料科学与工程学院江西景德镇 333000 2. 江西省先进陶瓷材料重点实验室江西景德镇 333001

关键词：硅酸锆晶须非水解溶胶-凝胶法氟化锆

分类号：TQ 174

出版年,卷(期):页码：2015,43(3):322-326

DOI：DOI：10.14062/j.issn.0454-5648.2015.03.12

摘要：

以无水四氯化锆为锆源、正硅酸乙酯为硅源、氟化锂为矿化剂、乙醇为溶剂、氟化锆为生长助剂，采用非水解溶胶-凝胶法制备硅酸锆晶须。借助综合热分析、X射线衍射分析、扫描电子显微镜和透射电子显微镜等研究了硅酸锆干凝胶在氮气气氛中热处理的物相变化以及成型压力、氟化锆用量对形成硅酸锆晶须的影响，探讨了硅酸锆晶须的形成机理。结果表明：氮气气氛下热处理并不影响硅酸锆的低温合成，成型压力过大或过小、氟化锆用量过多或过少均不利于硅酸锆晶体的一维择优生长，成型压力为2 MPa、氟化锆用量为10%(质量分数)时，硅酸锆晶须直径为0.2～0.4 μm、长径比达到15～30。

Zircon whiskers were prepared via a non-hydrolytic sol-gel method with anhydrous zirconium tetrachloride as zirconium source, tetraethylorthosilicate as silicon source, lithium fluoride as a mineralizer, ethanol as a solvent and anhydrous zirconium fluoride as a whisker growth promoter. The zircon dry gel annealed in nitrogen atmosphere was characterized by thermogravimetric-differential thermal analysis, X-ray diffraction, scanning electron microscopy and transmission electron microscopy, respectively. The influences of molding pressure and amount of ZrF4 on the formation of zircon whiskers were investigated. In addition, the formation mechanism of zircon whisker was also discussed. The results show that heat treatment in nitrogen atmosphere does not hinder the synthesis of zircon at a low temperature. It is ineffective to grow zircon whisker in one-dimension either at rather high/low molding pressure or in the presence of more/less ZrF4. The well-developed zircon whiskers with the diameter of 0.2–0.4 μm and the aspect ratio of 15–30 can be obtained at the molding pressure of 2 MPa and the amount of ZrF4 of 10%.

基金项目：

国家自然科学基金(51162013, 51362014)；江西省主要学科学术和技术带头人培养计划(20113BCB22009)；江西省博士后研究人员择优项目(2013KY34)资助。

作者简介：

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