Insights into the Electrochemical Synthesis and Supercapacitive Behaviour of 3D Copper Oxide-Based Nanostructures

In this study, nanostructured copper oxide-based films with crystallite size below 10 nm were electrochemically synthesized on copper foil and foam electrodes and investigated for their supercapacitive behaviour. The synthesis was carried out via cyclic voltammetry (CV) for up to 1000 cycles in an alkaline electrolyte. By tuning the upper vertex potential (−0.3 V to 0.65 V vs. Ag/AgCl), both phase composition (Cu2O, Cu(OH)2, CuO) and morphology (grains, nanoneedles, nanoplatelets) were precisely controlled, demonstrating the versatility of this approach. The kinetics of oxide/hydroxide film formation on foil and foam electrodes were analysed based on EIS data that were interpreted in the frame of equivalent electric circuits and their changes with potential. The capacitive properties of the synthesized films were evaluated using CV in the potential range of 0 V–0.65 V, and the optimized CuO film synthesized on Cu foam exhibited a high specific capacitance of 1380 mF cm⁻2. An energy density of 0.061 mWh cm−2 and power density of 1.28 mW cm−2 were obtained at 10 mA cm−2 discharge current. Charge–discharge cycling at 100 mV s−1 for 1000 cycles indicated an initial capacitance increase followed by stable retention, highlighting the structural integrity and electrochemical stability of the films obtained on 3D foam. These findings provide valuable insights into the controlled electrochemical synthesis of copper oxide nanostructures and their potential for high-performance capacitor applications.