Spherical-particle MCM-41 was synthesized at room temperature, and, then, impregnated with aqueous solutions of NH4VO3 to produce variously loaded VOx/MCM-41 composite materials. Bulk and surface properties of the materials thus produced were characterized by means of X-ray powder diffractometry (XRD), infrared spectroscopy (FTIR), N-2 sorptiometry and X-ray photoelectron spectroscopy (XPS). Results obtained indicated that subsequent calcination at 550 degrees C (for 2 h) of the blank and impregnated MCM-41 particles, results in materials assuming the same bulk structure of MCM-41, and exposing uniformly mesporous, high area surfaces (P-w = 2.0-2.3 nm; 974-829m(2)/g), except for the material obtained at 20 wt%-V2O5 that was shown to suffer a considerable loss on surface area (down to 503m(2)/g). XPS results implied that the immobilization of the VOx species occurs via interaction with surface OH/H2O groups of MCM-41, leading to the formation of vanadate (VO3) surface species, as well as minor V-O-Si and V2O5-like species. However, in all cases, the vanadium sites remained pentavalent and exposed on the surface. (C) 2010 Elsevier B. V. All rights reserved.