以无水三氯化铝为铝源、正硅酸乙酯为硅源、无水乙醚为氧供体、选用K2SO4-KCl作为熔盐,采用非水解溶胶-凝胶工艺结合熔盐法制备莫来石晶须,借助XRD、SEM和TEM等测试手段研究了在熔盐环境下莫来石干凝胶的物相转变以及熔盐的引入、热处理温度及保温时间对莫来石晶须形貌的影响。结果表明:引入熔盐后,非水解溶胶-凝胶法在850℃即可合成莫来石晶相,且熔盐K2SO4-KCl对莫来石晶体的一维生长有显著促进作用;热处理温度过低或过高、保温时间过短或过长均不利于莫来石晶须的制备,900℃保温3 h能制备出产率高、直径在100~150 nm,长径比为20~35、沿[001]方向择优生长的莫来石晶须。
Mullite whiskers were synthesized by a non-hydrolytic sol-gel process combined with molten salt method using anhydrous aluminum chloride as aluminum source, tetraethylorthosilicate (TEOS) as silicon source, ethyl ether as oxygen donor, K2SO4-KCl as a molten salt.The phase transition of muUite dry gel in the presence of the molten salt as well as the influences of adding molten salt, heat treatment temperature and holding time on the microstructure of mullite whisker were investigated by means of XRD, SEM and TEM. The results showed that mullite crystal phase could be formed via non-hydrolytic sol-gel process combined with the molten salt method at 850℃. The presence of K2SQ-KC1 can promote the one-dimensional growth of mullite. Both heat treatment temperature at too high or low level and holding time at too long or short level were unbeneficial to the growth of whisker. The mullite whiskers along the growth direction of [001], the diameter of 100 - 200 nm and the aspect ratio of 20 - 30 can be synthesized at 900℃ for 3 h.