| Summary: | The design and development of electrode materials for energy-storage applications is an area of prime focus around the globe because of the shortage of natural resources. In this study, we developed a method for preparing a novel three-dimensional binder-free pseudocapacitive NiZn<sub>2</sub>O<sub>4</sub> active material, which was grown directly over nickel foam (NiZn<sub>2</sub>O<sub>4</sub>@3D-NF), using a simple one-step hydrothermal process. The material was characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Cyclic voltammetry, galvanostatic charge–discharge, and electrochemical impedance spectroscopy techniques were employed to evaluate the pseudocapacitive performance of the NiZn<sub>2</sub>O<sub>4</sub> active material in a three-electrode assembly cell. The prepared NiZn<sub>2</sub>O<sub>4</sub>@3D-NF electrode exhibited an excellent specific capacitance, of 1706.25 F/g, compared to that of the NiO@3D-NF (1050 F/g) electrode because it has the bimetallic characteristics of both zinc and nickel. The NiZn<sub>2</sub>O<sub>4</sub>@3D-NF electrode showed better cyclic stability (87.5% retention) compared to the NiO@3D-NF electrode (80% retention) after 5000 cycles at a fixed current density, which also supports the durability of the NiZn<sub>2</sub>O<sub>4</sub>@3D-NF electrode. The characteristics of NiZn<sub>2</sub>O<sub>4</sub>@3D-NF include corrosion resistance, high conductivity, an abundance of active sites for electrochemical reaction, a high surface area, and synergism between the bimetallic oxides, which make it a suitable candidate for potential application in the field of energy storage.
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