In this work, we have synthesized LiFePO4 particles with the size around 200 nm by solvothermal method. The crystalline LiFePO4 was synthesized from LiOH.H2O, FeSO4.7H2O and H3PO4 precursors, using ethylene glycol and water as solvents. Ascorbic acid was added to the solution to prevent oxidation of Fe2+ to Fe3+. The structure was characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). Carbon black is determined to reduce the phase structure of Fe3+ remaining in the LiFePO4 composition into Fe2+ after the annealing step. The LiFePO4 particles were also mixed with EC 600JD carbon black and followed by the annealing at 550 oC for composite formation. Their electrochemical properties were determined by cyclic voltammetry (CV) and galvanostatic cycling with potential limit (GCPL).