The potential of LiFePO4 as cathode material has not been fully exploited due to its intrinsic poor electronic and ionic conductivities. Attempts have been made to improve these properties of which coating of the active carbon on the particle surface is the most viable method so far. Phase-pure LiFePO4 and two LiFePO4/C composites were synthesized by mechanical activation process employing two different methods: (i) direct addition of acetylene black carbon and (ii) addition of sucrose as carbon precursor. The samples were well characterized by various techniques like elemental analysis, Brunauer-Emmett-Teller (BET) method, scanning electron microscopy (SEM), X-ray powder diffraction (XRD), and Raman spectroscopy to establish their composition, morphology, particle size and surface area. The structure of these samples is investigated as olivine structure space group Prima by X-ray powder diffraction. Transmission electron microscopy (TEM) confirms that the carbon nanocoating on the LiFePO4 particles has no visible dislocations and fractures. The electrochemical performance of LiFePO4/C is significantly affected by the nature of the carbon nanocoating, which in turn is affected by the choice of synthesis method. (C) 2013 Elsevier B.V. All rights reserved.