非水解溶胶-凝胶法制备硅酸锆晶须初探

Preliminary Study on Zirconium Silicate Whiskers Prepared by NHSG Method

以无水四氯化锆为锆源，正硅酸乙酯（TEOS）为硅源，氟化锂为矿化剂，乙醇为溶剂，炭黑为还原剂，采用非水解溶胶-凝胶法制备硅酸锆晶须，研究了炭黑种类与坩埚密封程度对硅酸锆晶须生长的影响。结果表明：相对于比表面积过小的炭黑8001或比表面积过大的超级活性炭，竹炭更利于硅酸锆晶须的生长；采用敞开坩埚方式热处理时能获得直径为30～90nm，长径比为6～15，沿[001]方向择优生长的硅酸锆晶须，半敞开或密封的反应体系均不能形成硅酸锆晶须。

Zirconium silicate whiskers were synthesized by nonhydrolytic sol-gel process （NHSG） method, using anhydrous zirconium tetraehloride as zirconium source, TEOS as silicon source, lithium fluoride as mineralizer, ethanol as solvent and carbon black as reducing agent. The influences of carbon black kind and sealing degree on the growth of zircon whiskers were investigated. The results show that bamboo charcoal is more conductive to the growth of zircon whiskers compared with the carbon black 8001 with a smaller surface area or super activated carbon with a larger surface area; using open mode for reaction system, optimized zircon whiskers can be prepared with the growth direction of [ 001 ], whose diameter and aspect ratio are in the range of 30-90 nm and 6-15, respectively. Both semi open and closed mode for action system will reduce the growth quality of zircon whiskers.