Nickel and copper incorporated MCM-41-like mesoporous nanocomposite materials prepared by the direct hydrothermal synthesis and the impregnation procedures showed highly attractive pore structure and surface area results for catalytic applications. The XRD patterns showed that characteristic MCM-41 structure was preserved for the materials synthesized following an impregnation procedure before the calcination step. The surface area of the Cu impregnated material with a quite high Cu/Si atomic ratio (0.19) was 631 m(2)/g. Very narrow pore size distributions with an average pore diameter of about 2.7 nm were obtained as a result of plugging of some of the smaller pores by Cu nanoballs. For lower metal to Si ratios (for instance for Ni/Si = 0.06) much higher surface area values (1130 m(2)/g) were obtained. In the case of nanocomposite materials synthesized by the direct hydrothermal route, MCM-41 structure was not destroyed for samples containing metal to Si atomic ratios as high as 0.12. In the case of materials containing Cu/Si and Ni/Si ratios over 0.2 wider pore size distributions and some decrease of surface area were observed.