This work focuses on the synthesis of LiFePO4-PANI hybrid materials and studies their electrochem. properties (capacity, cyclability and rate capability) for use in lithium ion batteries. PANI synthesis and optimization was carried out by chem. oxidation (self-assembly process), using ammonium persulfate (APS) and H3PO4, obtaining a material with a high degree of crystallinity. For the synthesis of the LiFePO4-PANI hybrid, a thermal treatment of LiFePO4 particles was carried out in a furnace with polyaniline (PANI) and lithium acetate (AcOLi)-coated particles, using Ar/H2 atm. The pristine and synthesized powders were characterized by XRD, SEM, IR and TGA. The electrochem. characterizations were carried out by using CV, EIS and galvanostatic methods, obtaining a capacity of 95 mAhg-1 for PANI, 120 mAhg-1 for LiFePO4 and 145 mAhg-1 for LiFePO4-PANI, at a charge/discharge rate of 0.1 C. At a charge/discharge rate of 2 C, the capacities were 70 mAhg-1 for LiFePO4 and 100 mAhg-1 for LiFePO4-PANI, showing that the PANI also had a favorable effect on the rate capability.