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[en] Olivine lithium iron phosphate (LiFePO4) is a promising cathode material for Li-ion battery. A temperature around 700 − 800 ◦C is generally required to prepare LiFePO4 powder with good crystallinity. The LiFePO4 materials are synthesized via a solid-state method by using a highenergy nano mill (HENM). The conventional ball-milling process is also conducted for the same material for a comparative study. The effect of the precursor’s mixing processes on the synthesis temperature of LiFePO4 is investigated in this study. The required reaction temperature of LiFePO4 is 432 ◦C for the HENM process and 480 ◦C for the ball-mill process as found from the differential scanning calorimetry (DSC) results. The HENM process improves the reaction activity and the homogeneity of the materials used throughout process and lowers the reaction temperature as compared with the conventional ball-mill process. The milled powders are characterized by using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The sample synthesized by using the HENM process exhibits a discharge capacity of 136 mAhg−1 at 0.1 C rate. The results in this study indicate that the HENM process is a substantial and promising process for LiFePO4 cathode preparation owing to its short fabrication time and ability to improve the reaction condition. A HENM can be used to promote formation of LiFePO4 at lower temperatures.