回流老化由ZrOCl2水解得到的ZrO(OH)2水凝胶,然后经焙烧制备了高比表面积的ZrO2. 采用氮吸附、X射线衍射和FT-Raman光谱等技术,研究了老化温度、老化时间、碱液的碱度和搅拌速度以及焙烧气氛对ZrO2比表面积、晶相组成和晶粒大小的影响. 结果表明,回流老化可明显提高ZrO2的比表面积和耐热性. 用比色法分析了样品中Si4+杂质的含量,结果表明,回流老化引起二氧化锆比表面积和热稳定性增大的主要原因是热碱溶液使玻璃容器中的Si4+溶解并掺杂至ZrO2. 样品中Si4+杂质含量愈大,ZrO2的比表面积和热稳定性愈高,ZrO2的晶粒愈小. 将ZrO(OH)2水凝胶在pH=11.5的NH4OH溶液中于96 ℃回流老化24 h,再经600 ℃焙烧可获得比表面积高达305 m2/g的无定形ZrO2; 经800 ℃焙烧可制得晶粒为5.2 nm, 比表面积为174 m2/g的四方晶相ZrO2.
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