V2O5/TiO2 aerogels were made by a two-step sol-gel process characterized by surface area measurements, X-ray diffraction, Raman and infrared spectroscopies and high resolution electron microscopy. Catalytic performance in the selective reduction of NO by propane was found to be significantly better than those of their homologues prepared by a conventional method. (C) 1998 Elsevier Science B.V. All rights reserved.