Li0.5Ni0.25TiOPO4/C composite was synthesized by the co-precipitation method using polyethylene glycol as carbon source. X-ray diffraction study showed that the as-prepared material crystallizes in the monoclinic system (S.G. P21/c). This 3D structure exhibits an open framework favourable to intercalation reactions. The morphology and the microstructure characterisation was performed by scanning electron microscopy (SEM). Small particles (∼1μm) coated by carbon were observed. Raman study confirms the presence of carbon graphite in the Li0.5Ni0.25TiOPO4/C composite. Cyclic voltammetry (CV) and charge–discharge galvanostatic cycling were used to characterize its electrochemical properties. The Li0.5Ni0.25TiOPO4/C composite exhibits excellent electrochemical performances with good capacity retention for 50 cycles. Approximately 200mAh/g could be reached at C, C/2, C/5 and C/20 rates in the 0.5–3V potential range. These results clearly evidenced the positive effect of the carbon coating on the electrochemical properties of the studied phosphate.