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Mechanochemical treatment (MChT) in various media (water, air, ethanol) of the V2O5/ammonium dimolybdate composition at the ratio V:Mo = 0.7:0.3 has been carried out. Physicochemical transformations in this system have been studied by means of X-ray powder diffraction (XRD) and thermal analysis as well as FTIR spectroscopy. Ammonium dimolybdate undergoes hydration with formation of 4-aqueous ammonium paramolybdate during the MChT in water. Changes of phase and chemical composition at activation are determined first of all by nature of medium in which milling was carried out. Maximal interaction of components occurs during modification of the studied system in water.

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