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The current research deals with the urgent task of creating highly efficient photocatalysts for wastewater treatment from various organic pollutants. For these purposes, we carried out a mechanochemical synthesis, heat treatment, and study of a non-toxic, thermally and chemically stable catalysts with a heterostructure based on Fe 2 TiO 5 pseudobrookite. The morphology and the properties of the as-prepared composites were characterized through different techniques. The chemical reactions occurring during the step-by-step heat treatment of the samples were proposed using info from XRD analysis, IR spectroscopy, thermal analysis, and mass spectra. The influence of the gaseous medium on the phase composition and the degree of crystallinity of materials has been established. The analysis of the elemental composition and morphology of powder particles was carried out at an annealing temperature in the range from 100 to 1000 °C in air. The photocatalytic activity of pseudobrookite was studied during the decomposition of the organic dye Rhodamine B, and the mechanism of photocatalysis associated with the absorption of photons and the formation of an electron-hole pair was considered. It was found that samples thermally treated in nitrogen were demonstrated greater catalytic activity than those treated in air. • Precursor of Fe 2 TiO 5 pseudobrookite was obtained by solid-phase synthesis. • Heating the obtaining powder resulted to the formation of the Fe 2 TiO 5 crystalline phase. • Powders exhibited photocatalytic activity upon discoloration of the Rhodamine B solution. • For the powder calcined in nitrogen, the photocatalytic activity was higher than that for air. [ABSTRACT FROM AUTHOR]