A glycol based solvothermal process combined with carbon coating is attempted to prepare nano particle LiFePO4 cathode materials for Li-ion batteries. Different concentration of starting materials, process time, pH values and process temperature are tried. Samples are characterized by XRD and SEM analysis. A carbon coating process with sucrose is used to make LiFePO4/C composites. The optimized sample delivers capacity retention of 100% after 100 cycles at 100% depth of discharge with initial columbic efficiency of 98.9%, cycling capacity of about 163 mAh g−1 at 0.1 C-rate, 159 mAh g−1 at 0.5 C-rate, 157.8 mAh g−1 at 1 C-rate, and 145.9 mAh g−1 at 5 C-rate, under the electrode formula of 80% LiFePO4/C composites, 10% carbon black and 10% binder. This study shows that proposed process can be a potential promising way to prepare high performance LiFePO4 cathode materials for lithium ion batteries.