Two kinds of novel phenyl-functionalized mesoporous silica materials have fabricated for the first time by an instant-direct-templating method using poly(ethylene glycol)-block-poly(propylene glycol)block-poly(ethylene glycol) and tetraethyl orthosilicate as surfactant template and precursor, respectively. Samples were characterized by Fourier transform infrared spectroscopy, small-angle Xray diffraction, thermogravimetric analysis, N-2 adsorption-desorption, scanning electron micrography and transmission electron micrography. The results show that phenyl groups are attached covalently to the pore wall of mesoporous materials after modi. cation. The functionalized materials still preserve a desirable ordered hexagonal P6mm and cubic Ia3d mesophase structure, respectively, have high specific surface area, large pore volume and narrow pore size distribution. (C) 2009 Elsevier B. V. All rights reserved.