A method with modifying tetraethyl orthosilicate (TEOS) with nickel species has been developed for the synthesis of mesoporous silica with high nickel content (11.8 wt.% of Ni or even higher). With the method, MCM-41-type materials were obtained with high BET surface area reaching 868 m(2)/g and pore volume up to 0.73 cm(3)/g. The materials were characterized by means of X-ray powder diffraction, transmission electron microscopy, energy dispersive X-ray spectroscopy, N-2 adsorption, Fourier transform infrared and X-ray photoelectron spectroscopy. Nickel species were incorporated into the silica frameworks. The mesostructures still remain after activation using H-2 at 773 K. (C) 2005 Elsevier Ltd. All rights reserved.