In this work, Ni0.5Zn0.5Fe2O4 is synthesized as binder-based (NZF) and binder-free electrodes (NZF@NF). The binder-free electrode is directly synthesized on nickel foam via facile hydrothermal techniques. The crystalline phase of both of these electrodes is examined through X-ray diffraction. Their morphology is investigated by scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (TEM), which revealed the well-defined nanostructure with the shape like thin hexagonal platelets. The chemical composition is verified by energy dispersive spectroscopy (EDS). Their electrochemical properties are analyzed by cyclic voltammetry (CV), galvanostatic charge−discharge (GCD), and electrochemical impedance spectroscopy (EIS). The NZF@NF electrode has outperformed the binder-based NZF electrode in terms of electrochemical performance owing to the 3D interconnected structure of the nickel foam. The NZF@NF electrode has delivered a high specific capacity of 504 F g−1 at the current density of 1 A g−1, while its counterpart has delivered a specific capacity of 151 F g−1 at the same current density.