ZnFe2O4 and MgxCu0.2Zn0.82–xFe1.98O4 (where x = 0.20, 0.25, 0.30, 0.35, and 0.40) nanoparticles were synthesized by sol–gel assisted combustion method. X-ray diffraction (XRD), FTIR spectroscopy, Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Brunauer–Emmett–Teller (BET) surface area studies were used to characterize the synthesized compounds. ZnFe2O4 and the doped compounds crystallize in Fd3m space group. The lattice parameter of ZnFe2O4 is calculated to be a = 8.448(3) Å, while the doped compounds show a slight decrease in the lattice parameter with an increase in the Mg content. The particle size of all the compositions are in the range of ∼50–80 nm, and the surface area of the compounds are in the range of 11–12 m2 g–1. Cyclic voltammetry (CV), galvanostatic cycling, and electrochemical impedance spectroscopy (EIS) studies were used to investigate the electrochemical properties of the different compositions. The as-synthesized samples at 600 °C show large-capacity fading, while the samples reheated at 800 °C show better cycling stability. ZnFe2O4 exhibits a high reversible capacity of 575 mAh g–1 after 60 cycles at a current density of 100 mA g–1. Mg0.2Cu0.2Zn0.62Fe1.98O4 shows a similar capacity of 576 mAh g–1 after 60 cycles with better capacity retention.
