Nanostructural characteristics of vanadium/cerium mixed-oxide film, prepared by sol-gel process at 55 atom% of V and intercalated by lithium ions, were studied by grazing incidence small-angle X-ray scattering (GISAXS). Particle size distributions were estimated probing different film regions, from its surface to the substrate. The intercalation of lithium affects the particle size distribution in film: the average particle size is reduced, while the size distribution width is increased. The surface is smoothed after intercalation, and its contribution to the scattering becomes dominating. The average particle size is the greatest at the surface, decreasing with the depth, and this is not essentially influenced by intercalation. (c) 2006 Elsevier B.V. All rights reserved.