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The formation kinetics of LiFePO 4 Olivine synthesized through sol-gel route has been studied by non-isothermal approach. LiFePO 4 precursors were prepared by mixing lithium dihydrogen phosphate (LiH 2 PO 4) and iron (III) citrate (C 6 H 5 FeO 7) and subsequently calcined in an Argon atmosphere at temperatures ranged from of 300–900 °C to form LiFePO 4 products. Thermal behaviors of calcination process were analyzed by thermogravimetry (TGA) and differential scanning calorimetry (DSC) simultaneously, while the mineralogical properties of LiFePO 4 were characterized using X-ray diffractometer (XRD). The kinetic parameters were determined by Ozawa–Flynn–Wall (OFW), Kissinger, and Kissinger-Akahira-Sunose (KAS) methods, and the reaction mechanism model was evaluated by Coats–Redfern approach. The results indicated that the reaction model of LiFePO 4 formation agreed with the three-dimensional diffusion mechanism. The temperature had an essential role in the synthesis of LiFePO 4. The optimum calcination temperature was 700 °C where this condition produced LiFePO 4 Olivine with high degree of crystallinity, better lattice parameters and phase purity. [ABSTRACT FROM AUTHOR]