This paper reports on a new method for the preparation of mesoporous silica membranes on alumina hollow fibers. A surfactant-silica sol is filled in the lumen of an alpha-alumina hollow fiber. The filtration technique combined with an evaporation-induced self-assembly (EISA) process results in the formation of a continuous ordered mesoporous silica layer on the outer side of a-alumina hollow fibers. X-ray diffraction (XRD), transmission electron microscopy (TEM), and nitrogen isothermal adsorption measurements reveal that these membranes possess hexagonal (P6mm) mesostructures with pore diameters of 4.48 nm and BET surfaces of 492.3 m(2) g(-1). Scanning electron microscopy (SEM) studies show that the layers are defect free and energy-dispersive spectroscopy (EDS) mapping images further confirm the formation of continuous mesoporous silica layer on the outer side of a-alumina hollow fibers. Nitrogen and hydrogen permeance tests show that the membranes are defect free. (c) 2008 Elsevier Inc. All rights reserved.