LiFePO4 powder was synthesized by means of a new route, using a two step process. In the first step, an intermediate compound was synthesized by the sol-gel method. This precursor compound to LiFePO4 was characterized by thermal analysis (TG/DTG and DSC), Mossbauer spectroscopy, Transmission Electronic Microscopy (TEM) and Small Angle Scattering (SAXS). In the second step, the precursor was sintered and analyzed by X-ray diffraction (XRD), showing the formation of the proposed single phase material. (c) 2005 Elsevier B.V. All rights reserved.