The nanostructure of metal oxides attracts great attention in the field of supercapacitors because of fast charge transport process. The hydrothermal method is used for development of NiCo2O4nanostructure on carbon cloth as current collector backbone. The stepwise study of various structural, morphological and electrochemical properties of NiCo2O4electrode is studied. The ultrasonic treatment is used to obtain nanowire-like morphology of NiCo2O4 which exhibits hierarchical nanostructure, which provides surface properties such as high surface area and appropriate pore capacity. NiCo2O4 nanostructure with specific capacitance of 1460 F g-1 with high electrochemical stability of 84% after 3000 cycles in 3 M KOH aqueous electrolyte at 100 mV s-1. The electrochemical property shows NiCo2O4is one of the potential candidates for energy storage application. The specific capacitance and energy density for NiCo2O4@CC//NiCo2O4@CC symmetric supercapacitor device is of 124 F g-1 and 16.18 Wh.kg-1, respectively at current density of 5 mA.

Transition metal molybdates are one of the most prominent materials for energy storage devices. The present investigation establishes a strong correlation between the structure and electrochemical performance of NiMoO ₄ through Density Functional Theory (DFT). Initially, the NiMoO ₄ microspheres are directly deposited on nickel foam using a hydrothermal method by tuning experimental parameters. When employed as electrode materials, the NiMoO ₄ microspheres deliver a specific capacity of 168.9 mAh g ⁻¹ at 1 A g ⁻¹ . In addition, the material retains 80% capacity over 7000 charge‐discharge cycles with 98.3% coulombic efficiency, implying its excellent stability. DFT calculations are used to determine specific capacity and potassium ion diffusion for 5 layers of [110] planes of NiMoO ₄ . The potential energy landscape is created for [110] plane using the potassium atom minimum hopping algorithm and atomic simulation environment. The DFT results clearly align with the theoretical capacity of 203 mAh g ⁻¹ close to the experimental results. A hybrid supercapacitor (HSC) is also developed with NiMoO ₄ //AC cell delivers a specific energy of 56.3 Wh kg ⁻¹ at a specific power of 421 W kg ⁻¹ with negligible capacity loss over 15 000 cycles. This investigation offers the development of battery‐type electrodes for hybrid supercapacitors using the fundamental understanding of ion‐diffusion in the materials’ structure.