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A high-energy ball-milling method was applied for different milling times (1 h, 3 h, and 10 h) to synthetize nanocrystalline MgH₂ powder samples catalyzed by Fe₂Ti. Morphology and microstructure of the powders were characterized by scanning electron microscopy and X-ray diffraction. The recorded diffraction profiles were evaluated by the convolutional multiple whole profile fitting algorithm, in order to determine microstructural parameters of the composites, such as average crystallite size and average dislocation density. Differential scanning calorimetry was performed to investigate the dehydrogenation characteristics of the alloys. It was obtained that there exists an optimal milling time (3 h) when desorption occurs at the lowest temperature. X-ray diffraction of partially dehydrided states confirmed a two-step H-release, including the subsequent desorption of γ-MgH₂ and α-MgH₂. The effect of milling time on the H-sorption performance was investigated in a Sievert-type apparatus. The best overall hydrogenation performance was obtained for the composite milled for 3 h.