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Thermal transformations of mechanochemically activated (MCA) termites Al/ V2O5 were analyzed by the method of X-ray diffraction, calorimetry and EPR spectroscopy. The influence of the treatment time of MCA on stages of thermal transformations during oxidation of aluminum in the reaction 10Al + 3V2O5 → 5Al2O3 + 6V was revealed and the optimal conditions of MCA were established. Importance of such composites is caused by their activity as perspective termites with high energy production up to explosion. The EPR study of such systems provides valuable invornation about their structure and features