In the current study, three distinct synthesis techniques, the gel, co-precipitation, and solid-state method, were employed to synthesize (MgFe2O4)x/ZnO1-x hetero-nanocomposites with varying magnesium ferrite contents (x = 0.03%, 0.06%, and 0.09%). To study the effect of the addition of magnesium ferrite nanoparticles on the structural, morphological, thermal, and electrochemical properties of zinc oxide. X–ray diffraction (XRD), Rietveld refinement technique, Fourier transform infrared (FT-IR) spectroscopy, field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and cyclic voltammetry (CV) were used to investigate the samples. The formation of the spinel cubic structure and hexagonal wurtzite structure of the prepared magnesium ferrite/zinc oxide nanocomposites was confirmed by X-ray diffraction, and no extra phases were detected. The Rietveld-refined X-ray diffraction data revealed spinel cubic and hexagonal wurtzite structures with the P63mc and Fd-3m space group, respectively. The crystallite size decreased from 16 to 15 nm upon the substitution of magnesium ferrite nanoparticles, confirming the formation of nano-crystalline MgFe2O4/ZnO nanocomposites. FT-IR spectra were used to verify the absorption bands of MgFe2O4, ZnO, and their composites. FE-SEM images revealed the presence of a slight agglomeration of nanoparticles and a non-uniform size distribution. TEM analysis revealed nearly spherical morphologies for all prepared samples, with an average particle size of 19-22 nm. There is variation in the crystallite size as estimated from the instruments, which may be due to strain. The electrochemical behavior was investigated using cyclic voltammetry (CV) with a 0.5 M KCl aqueous solution as the electrolyte. The MgFe2O4/ZnO nanocomposite exhibited superior rate performance and cycle stability compared to the other samples when their electrochemical performance was analyzed using cyclic voltammetry (CV). According to the physical results, nanocomposite electrodes exhibited enhanced electrochemical performance, high reversibility, and cycle stability, with specific capacitances ranging from 1.87 F/g (0.01 V) to 7.63 F/g (0.002 V), making them promising candidates for pseudocapacitors.