As a new approach, LiFePO4 nanoparticles were directly synthesized from precursors iron(III) nitrate and lithium dihydrogen phosphate by a polyol process without post heat treatment in one step. The obtained powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and combined thermogravimetry and differential scanning calorimetry and mass spectroscopy TG/DSC/MS. The X-ray diffraction showed the orthorhombic crystal structure of LiFePO4 without any impurity phases. The synthesized LiFePO4 has rhombohedral morphology with high aspect ratio with a thickness of less than 100 nm. TG/DSC/MS revealed a weight loss of only 10.9 wt.% when heating up to 1000 degrees C. Electrodes prepared from the LiFePO4 particles were electrochemically characterized by cycling at 0.1C current rate and temperatures in half cell measurements against lithium foil between 2 and 4.2 V in an EC/DMC electrolyte with 1 M LiPF6 as conductive salt. A reversible specific capacity of 146 mAh/g was achieved by applying carbon coating on the rhombohedral particles. (C) 2011 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.