Three different synthetic routes, including solid-state reaction, sol-gel and hydrothermal methods are successfully used for preparation of Li3V2(PO4)(3)/C. Ascorbic acid is used as a reducing agent and/or as a chelating agent. The Li3V2(PO4)(3)/C synthesized by hydrothermal method with fine particles exhibits lower impedance and smaller potential difference values between oxidation and reduction peaks than those by solid-state reaction and sol-gel methods. Thus as cathode material for Li-ion batteries, the Li3V2(PO4)(3)/C synthesized by hydrothermal method shows higher discharge capacity, better rate capability and cyclic performance. Even at a high charge-discharge rate of 10C, it still can deliver a discharge capacity of 101.4 mAhg(-1) and 106.6 mAh g(-1) in the potential range of 3.0-4.3V and 3.0-4.8V, respectively. The hydrothermal synthesis has been considered to be a competitive process to prepare Li3V2(PO4)(3)/C cathode materials with excellent electrochemical performances. (C) 2011 Elsevier Ltd. All rights reserved.