In an attempt to enhance the energy storage capacity and discharge voltage, a new cathode material based on ferrocene and LiF for lithium-ion batteries has been explored [Fe/LiF/C] nanocomposite (1) has been synthesized by pyrolysis of a ferrocene/LiF mixture at 700°C using a rotating quartz tube setup in a furnace. The structure and morphology of the composite were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), Brunauer–Emmer–Teller (BET) analysis, Raman, and Mössbauer spectroscopy. The nanocomposite is composed of well-defined nanotubes which are interlinked by graphitic shell-type structures containing uniformly distribution of Fe, Fe–C, and LiF nanoparticles. The binder-free nanocomposite cathode showed enhanced electrochemical performance with the reversible specific capacity of 230mAhg−1 (1.3–4.3V) at 20.8mAg−1 at room temperature. It exhibited a remarkable cyclic stability and good rate capability performances. The morphology of 1 was changed by ball milling, and the resulting nanocomposite 2 did not show any cyclic stability as a cathode. Thus, the cyclic stability and rate capability performances of 1 were attributed to its structure and morphology.