Li3V2(PO4)3/C (LVP/C) cathode materials for lithium ion batteries have been successfully synthesized via carbon thermal reduction method using pitch as both a new carbon source and a reduction agent. The influences of different carbon sources (pitch, Super P, KS15 and Vulcan-XC72) and heat treatments between 650 and 950°C on the LVP/C materials have also been investigated. The structural and electrochemical properties of the samples are characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscope (TEM) and high resolution transmission electron microscopy (HRTEM) as well as charge-discharge experiments. The LVP/C synthesized with pitch have smooth surface with uniform residue carbon distribution and presents the best electrochemical performance. In addition, the oxidation of carbon has been discussed. The results indicate that carbons obtained from four carbon sources are tended to be oxidized to CO2 than CO. Electrochemical tests show the LVP/C-750°C exhibits the highest discharge capacity and the most excellent capacity retention. Spherical LVP/C particles are obtained using the spray drying method. The spray drying-LVP/C composite deliver higher discharge capacity than those of LVP/C composites obtained by carbon thermal reduction method or by drying with oven.