Effect on hydrothermal treatment of lamellar vanadium oxides was investigated and the formation of hexagonal and cubic mesophase was found. This lamellar materials were prepared by mixing of cetyltrimethylammonium-bromide and pH-controlled sodium metavanadate solution. Thermal method and UV/O₃treatment were applied to extract organic template. The structure of resulting product was studied by powder X-ray diffraction and transmission electron microscopy (TEM).