Abstract: Three-dimensionally ordered macroporous (3DOM) SiO2 materials were synthesized by using colloid crystal template which was assembled by centrifugation of polystyrene spheres with 480nm diameter．The sol from tetraetoxysilane was filled in the voids between spheres，and transformed into gel in-situ．The template was removed by calcination．The sample had a hexagonally well-ordered array as shown by SEM observation．The diameter of macroporores was 360 nm corresponding to a shrinkage of 25%．The macropores kept three-dimensionally interconnected macroporous networks through small windows．The walls of pores contained the mesoporous structure with a narrow pore size distribution　in 3~4nm according to the result of N2 adsorption-desorption．The XRD spectrum showed that the sample consisted of amorphous SiO2．

摘要： 将粒径为480 nm的聚苯乙烯微球离心组装为胶体晶体模板，以正硅酸乙酯为硅源配制SiO₂溶胶并填充到模板间隙，原位形成凝胶，最后通过焙烧去除模板，得到三维有序大孔（3DOM）SiO₂。通过SEM检测，大孔以六方有序的方式排列，其孔径及孔径收缩率分别为360 nm和25％。大孔之间由小窗口连通，构成内部三维交联的大孔网络。低温N₂吸附测试表明，大孔孔壁上存在中孔孔隙，其中在3～4 nm有一集中的孔分布。XRD显示，制备的3DOM材料由无定形SiO₂组成。