Modified compositions in the system V2O5/(NH4)2Mo2O7 have been prepared by means of mechanochemical, hydrothermal, microwave and ultrasonic treatments in aqueous medium. Chemical and phase transformations occurring on the stages of modification and following calcinations have been studied with the help of XRD, DTA-TG, FTIR and UV-Vis spectroscopy, nitrogen adsorption, and SEM. It has been established that precursors of catalytically active phases possessing meso-macroporous structure have been formed during modification. The comparison of the properties of compositions prepared via different methods has been carried out. Particularly, precursors modified via various procedures possess different morphology.