The Olivine-type LiFePO4, which is one of the most attractive cathode materials for lithium ion batteries, was synthesized via calcining amorphous LiFePO4 obtained by chemical reduction and lithiation of FePO4 using Vitamin C as reducer and lithium acetate as lithium source in alcohol solution. The prepared LiFePO4 was characterized by XRD and SEM. The results showed that the LiFePO4 powder has good crystallinity and spherical morphology with an average diameter of about 150 nm. Electrochemical measurement results indicated that the material exhibited high-rate characteristic and delivered a stable discharge capacity of 159 mAh g(-1) at 0.1 C rate. (C) 2007 Published by Elsevier B.V.