Vanadium- and molybdenum-containing compositions prepared by mechanochemical and following thermal treatments of V2O5/(NH4)2Mo2O7 (V/Mo = 0.7/0.3)

X-ray powder diffraction, DTA, FT-IR spectroscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), nitrogen adsorption, and mercury porometry were used to characterize samples prepared as a result of mechanochemical treatment (MCT) of a V₂O₅/(NH₄)₂Mo₂O₇ (V/Mo = 0.7/0.3) composition in water, ethanol, and air, as well as after calcining them at temperatures from the range 300–700°C. The MCT of nonporous powders in water yields porous materials with definite meso- and macropore sizes. Heat treatment in air at 300–450°C enhances the formation of a molybdenum substitutional solid solution in V₂O₅ and conserves rather high values of specific surface areas and pore volumes. An increase in heat treatment temperature is accompanied by the degradation of the solid solution and the formation of a V₂MoO₈ phase.