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,氟化锆为生长助剂,采用非水解溶胶-凝胶法于800℃制备出硅酸锆晶须,借助XRD、SEM和TEM等测试手段研究了热处理气氛、氟化锂用量、氟化锆的引入方式等工艺因素对硅酸锆晶须形成的影响。结果表明:与空气气氛相比,氮气气氛更加有利于硅酸锆晶体的一维择优生长;矿化剂用量过多或过少均不利于晶须的形成;氟化锆以外置的方式引入能获得直径为0.2~0.4μm,长径比达15~30,沿c轴方向择优生长的硅酸锆晶须。
Zirconium silicate whiskers were synthesized at 800 ℃ by non-hydrolytic sol-gel method using anhydrous zirconium tetrachloride( Zr Cl4) as zirconium source,tetraethylorthosilicate( TEOS) as silicon source,lithium fluoride( Li F) as mineralizer,ethanol as solvent and anhydrous zirconium fluoride( Zr F4)as growth promoter. The influences of heat treatment atmosphere,the amount of Li F and introducing manner of Zr F4 on the formation of zircon whiskers were studied by X-ray diffraction analysis( XRD),scanning electron microscope( SEM) and transmission electron microscopy( TEM). The results show that compared with air atmosphere,nitrogen atmosphere is more favorable to the one-dimension preferential growth of zirconium silicate. Too much or too little mineralizer is not benefit to the formation of zircon whiskers. When Zr F4 is introduced by the outside addition,zircon whiskers elongated along the c-axis,with diameter and aspect ratio in the range of 0. 2-0. 4 μm and 15-30,respectively,can be achieved.