The mechanochemical effects on the reactivity and properties of a titanium/hematite powder mixture with molar ratio of 1/2 are investigated. Crystalline-phase structure, composition, hyperfine and magnetic behaviors were analyzed as a function of activation time by means of X-ray diffraction, scanning electron microscopy, Mossbauer spectroscopy and vibrating sample magnetometry. The results showed that at relatively short activation times metallic Ti reduces part of the ferric ions, yielding a complex product formed mainly by a mix of two solid solutions Fe3-xTi3O4 (titanomagnetites), both with very different x values (0 < x < 1). Also metallic iron and superparamagnetic hematite particles were detected by Mossbauer spectroscopy. As the mechanical treatment extends the composition of the reactive mixture changes, prevailing in the end the solid solution with higher x value. In contrast, when these activated samples are thermally treated the fraction of the solid solution which is richer in Ti diminishes. This fact produces a significant variation of the saturation magnetization of the obtained material. (C) 2010 Elsevier Ltd. All rights reserved.