In this study, Li3V2(PO4)3 (LVP) powders are prepared by a solution synthesis method. The effects of two reducing agents on crystal structure and morphology and electrochemical properties are investigated. Preliminary studies on reducing agents such as oxalic acid and citric acid, are used to reduce the vanadium (V) precursor. The oxalic acid-assisted synthesis induces smaller particles (30 nm) compared with the citric acid-assisted synthesis (70 nm). The LVP powders obtained by the oxalic acid exhibit a higher specific capacity (124 mAh g-1 at 1C) and better cycling performance (122 mAh g-1 following 50 cycles at 1C rate) than those for the citric acid. This is due to their higher electronic conductivity caused by carbon coating and downsizing the particles. The charge-discharge plateaus obtained from cyclic voltammetry are in good agreement with galvanostatic cycling profiles.