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In this study, hematite (Fe₂O₃) and aluminum (Al) powder mixtures were mechanically alloyed in a high-energy shaker ball mill to synthesize the iron-alumina (Fe-Al₂O₃) nanocomposite powder. The structural changes and phase developments occurring during mechanochemical process were studied by X-ray diffractometery (XRD) and scanning electron microscopy (SEM). The results showed that mechanochemical reaction of Fe₂O₃ and Al completed after 3 hours of milling time in a nanocrystalline Fe and Al₂O₃ embedded form and further milling produced a Fe-Al₂O₃ nanocomposite powder. Kinetics consideration according to the calculated adiabatic temperature demonstrated the sudden displacement reaction during mechanical alloying that accord well with XRD results. Also, particle size decrease as well as crystallite size with increasing the milling time.