Spherical Li3V2(PO4)3 (LVP) and carbon-coated LVP with a monoclinic phase for the cathode materials are synthesized by a hydrothermal method using N2H4 as the reducing agent and saccharose as the carbon source. The results show that single phase monoclinic LVP without impurity phases such as LiV(P2O7), Li(VO)(PO4) and Li3(PO4) can be obtained after calcination at 800 oC for 4 h. SEM and TEM images show that the particle sizes are 0.5~2 μm and the thickness of the amorphous carbon layer is approximately 3~4 nm. CV curves for the test cell are recorded in the potential ranges of 3.0~4.3 V and 3.0~4.8 V at a scan rate of 0.01 mV s–1 and at room temperature. At potentials between 3.0 and 4.8 V, the third Li+ ions from the carbon-coated LVP can be completely extracted, at voltages close to 4.51 V. The carbon-coated LVP exhibits an initial specific discharge capacity of 118 mAh g–1 in the voltage region of 3.0 to 4.3 V at a current rate of 0.2 C. The results indicate that the reducing agent and carbon source can affect the crystal structure and electrochemical properties of the cathode materials.