olivine lifepo4/c cathode materials for lithium ion batteries were synthesized using monodisperse polystyrene (ps) nano-spheres and other carbon sources. the structure, morphology, and electrochemical performance of lifepo4/c were investigated by x-ray diffraction (xrd), scanning electron microscopy (sem), galvanostatic charge-discharge tests, electrochemical impedance spectroscopy (eis) measurements, and raman spectroscopy measurements. the results demonstrated that lifepo4/c materials have an ordered olivine-type structure with small particle sizes. electrochemical analyses showed that the lifepo4/c cathode material synthesized from 7 wt.% ps nano-spheres delivers an initial discharge capacity of 167 mah g(-1) (very close to the theoretical capacity of 170 mah g(-1)) at 0.1 c rate cycled between 2.5 and 4.1 v with excellent capacity retention after 50 cycles. according to raman spectroscopy and eis analysis, this composite had a lower i (d)/i (g), sp (3)/sp (2) peak ratio, charge transfer resistance, and a higher exchange current density, indicating an improved electrochemical performance, due to the increased proportion of graphite-like carbon formed during pyrolysis of ps nano-spheres, containing functionalized aromatic groups.