| Summary: | This work focuses on the synthesis of LiFePO<sub>4</sub>–PANI hybrid materials and studies their electrochemical properties (capacity, cyclability and rate capability) for use in lithium ion batteries. PANI synthesis and optimization was carried out by chemical oxidation (self-assembly process), using ammonium persulfate (APS) and H<sub>3</sub>PO<sub>4</sub>, obtaining a material with a high degree of crystallinity. For the synthesis of the LiFePO<sub>4</sub>–PANI hybrid, a thermal treatment of LiFePO<sub>4</sub> particles was carried out in a furnace with polyaniline (PANI) and lithium acetate (AcOLi)-coated particles, using Ar/H<sub>2</sub> atmosphere. The pristine and synthetized powders were characterized by XRD, SEM, IR and TGA. The electrochemical characterizations were carried out by using CV, EIS and galvanostatic methods, obtaining a capacity of 95 mAhg<sup>−1</sup> for PANI, 120 mAhg<sup>−1</sup> for LiFePO<sub>4</sub> and 145 mAhg<sup>−1</sup> for LiFePO<sub>4</sub>–PANI, at a charge/discharge rate of 0.1 C. At a charge/discharge rate of 2 C, the capacities were 70 mAhg<sup>−1</sup> for LiFePO<sub>4</sub> and 100 mAhg<sup>−1</sup> for LiFePO<sub>4</sub>–PANI, showing that the PANI also had a favorable effect on the rate capability.
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