In this work, a mechanochemical procedure is proposed as a simple and fast method to synthesize the pure BiFeO 3 perovskite phase as a nanostructured material without the need for purification treatments, while the mechanochemical reaction mechanism has been investigated and correlated with that of the conventional solid-state reaction. Thus, different milling conditions have been used as a tool for tailoring the crystallite size of the resulting BiFeO 3 nanoparticles. The materials prepared by the mechanochemical reaction could be annealed or sintered without the formation of undesirable phases.Both the ferroelectric and ferromagnetic transitions were observed by DSC. Finally, the dielectric constants of the prepared material at different frequencies as a function of the temperature have been measured, showing that the material is clearly an isolator below 200 C, characteristic of a high quality BiFeO 3 material.