The sub-micron polystyrene microspheres were successfully synthesized by emulsion polymerization with a small amount of emulsifier. Using polystyrene colloidal crystals as porous template, alumina hydrosols as precursor for filling the template, alumina materials were prepared via calcination. Nanoparticle Size Analyzer, SEM, XRD and N2 adsorption-desorption techniques were used to characterize the polystyrene colloidal crystals and the alumina materials. The results show that the polystyrene microspheres have characteristics of smaller average diameter (100~350 nm), better monodispersion(<0.005)and higher yield(about 80%); the polystyrene colloidal crystals from directed self-assembly of polystyrene spheres have ordered arrangement, and the surface of the spheres is smooth and clean. The alumina materials prepared with the polystyrene colloidal crystals as the template, have ordered macroporous structures and adjustable apertures.%采用少皂乳液聚合法成功制备了单分散的聚苯乙烯微球，以微球自组装后的聚苯乙烯胶体晶体为大孔模板，铝溶胶为前驱体填充模板，干燥焙烧除去模板后制备了氧化铝载体。用激光粒度仪、扫描电镜、X射线衍射和氮气吸脱附对聚苯乙烯胶体晶体和氧化铝载体进行了表征。结果表明：少皂乳液聚合法制备的聚苯乙烯微球具有粒径较小（100~350 nm）、单分散性好（<0.005）、收率高(约80%)等优点；自组装的胶体晶体呈规则有序排列，微球表面光滑洁净，并以此为模板成功制备了具有三维有序结构的、大孔孔径可调的氧化铝材料。
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