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Titanium dioxide, TiO2, invariably draws researchers’ attention due to its unique physical and chemical properties and one of the most promising application areas of TiO2 is photocatalysis. It was shown before that the combination of redox-active oxides (such as MoO3 or V2O5) weakly active during illumination with a high-photoactive semiconductors (TiO2) makes it possible to create a photocatalytic systems with a function of accumulation of the photoexcited charge carriers. The use of nanocrystalline titanium dioxide as the photogeneration component of the photo-accumulating systems allows the production of photocatalysts, which ensures the generation, separation, and accumulation of photoexcited charge carriers. The aim of this work is study of interaction of photoexcited charge carriers with defects (the most part of that is paramagnetic) in TiO2/MoO3 nanoheterostructures.