Abstract <p>This paper presents the results of studying the effect of mechanochemical treatment on the TiFe_0.85Mn_0.05 alloy, which has the potential to be used as a hydrogen storage material on an industrial scale. The morphology and structure of the reference and treated powders were studied using a scanning electron microscope, and the phase composition was determined using X-ray diffraction. A part of the alloy with dimensions from 40 to 100 µm was used as a reference powder. The selected fraction was ground in argon medium at a frequency of 350 and 450 rpm with a duration of 30 and 60 min. In all selected modes, the powder size decreases and the number of defects increases, which is confirmed by both the results of X-ray diffraction and images of the scanning electron microscope. Such defects are additional diffusion paths for hydrogen atoms. This fact is also confirmed by a decrease in the time of the first hydrogen absorption. In this regard, the mechanochemical method makes it possible to solve one of the main problems of industrial application of titanium-iron alloy, namely, the difficulty of alloy activation. The results obtained are promising for the development of hydrogen storage materials, which will further open up the prospect of using them on an industrial scale.</p>