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In order to control the size and distribution of the high conductive Fe2P in LiFePO4/Fe2P composite, two different cooling rates (Fast: 15 ℃·min-1, Slow: 2 ℃·min-1) were employed after mechanical alloying.The discharge capacity of the fast cooled was 83 mAh·g-1 and the slow cooled 121 mAh·g-1.The particle size of the synthesized powder was examined by transmission electron microscopy and distribution of Fe2P was characterized using scanning electron microscopy (SEM).In addition, two-step heat treatment was carried out for better distribution of Fe2P.X-ray diffraction (XRD) and Rietveld refinement reveal that LiFePO4/Fe2P composite consists of 95.77% LiFePO4 and 4.33% of Fe2P.