The compounds, FeCo 2 O 4 and MgCo 2 O 4 are synthesized by the urea combustion and oxalate decomposition method, respectively. Powder X-ray diffraction (XRD), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED) and X-ray photoelectron spectroscopy (XPS) have been used to characterize the phases. Scanning electron microscopy (SEM) showed the distinct features in the morphology, submicron-size of FeCo 2 O 4 and needle-shaped particles of MgCo 2 O 4 . Galvanostatic cycling was carried out in the voltage range 0.005–3.0 V vs. Li at a current of 60 mA g −1 (~0.08 C) up to 50 cycles. The observed first-cycle charge capacities are, FeCo 2 O 4 : 827 mA h g −1 (corresponding to theoretical 7.3 mol of Li per mole of FeCo 2 O 4 ) and MgCo 2 O 4 : 736 mA h g −1 (5.7 Li). At the end of 50 cycles, FeCo 2 O 4 retained ~90% of the first-charge capacity, and a coulombic efficiency of ~99% is noted between 20 and 50 cycles. MgCo 2 O 4 showed extensive capacity-fading and retained only 0.9 mol of cyclable Li in the range 28–50 cycles. These results show that Fe is a better counter ion than Mg. The average charge and discharge voltages are ~2.0 V and ~1.2 V, respectively, for both the compounds. Cyclic voltammograms, up to 12 cycles on FeCo 2 O 4 complement the galvanostatic cycling results. Impedance studies were carried out on FeCo 2 O 4 at various voltages during the first cycle and after 10 cycles, and the data have been interpreted.