The mesoporous silica/alumina membrane was prepared by the template-tailored sol-gel method, using the surfactant of cetyltrimethyl ammonium bromide (CTAB) as the template. Further a novel procedure was explored to synthesize free-standing mesoporous silica oriented by the self-assembles of surfactants. Characterization of SEM and BET indicated that this free-standing silica films had good development of mesoporosity and a special asymmetric structure, which make it not only an attractive materials for preparing new types of catalysts, medical carriers and chemical sensors, etc. but also has promising applications in manufacturing asymmetric mesoporous membranes. (C) 2003 Elsevier B.V. All rights reserved.