Bifunctional NiCo‐CuO Nanostructures: A Promising Catalyst for Energy Conversion and Storage

Abstract This investigation explores the potential of co‐incorporating nickel (Ni) and cobalt (Co) into copper oxide (CuO) nanostructures for bifunctional electrochemical charge storage and oxygen evolution reactions (OER). A facile wet chemical synthesis method is employed to co‐incorporate Ni and Co into CuO, yielding diverse nanostructured morphologies, including rods, spheres, and flake. The X‐ray diffraction (XRD) and Raman analyses confirmed the formation of NiCo‐CuO nanostructure, with minor phases of nickel oxide (NiO) and cobalt tetraoxide (Co 3 O 4 ). High‐resolution Transmission Electron Microscope (HRTEM) also confirms the diverse morphologies and the minor phases of oxides. Synchrotron X‐ray absorption spectroscopy revealed higher charge states of Cu, Ni, and Co in the NiCo‐CuO nanostructure, enhancing its charge storage and OER. Site‐selective X‐ray absorption near edge structure analysis elucidated the spatial distribution of Cu, Ni, and Co in the nanostructure. Furthermore, extended X‐ray absorption fine structure spectroscopy provided insights into the local atomic structures, revealing increased coordination numbers and interatomic distances in the NiCo‐CuO nanostructure. In situ Raman analysis discloses the transformation of Co 3 O 4 into cobalt hydroxide (Co(OH) 2 ) and cobalt oxide (CoO) into cobalt oxyhydroxide (CoOOH) The NiCo‐CuO nanostructures exhibited superior specific capacitance, favorable Tafel behavior, and low overpotential positioning as promising bifunctional materials for energy storage and conversion applications. This work contributes to the development of efficient CuO nanocatalysts.