Calcination Strategy for Scalable Synthesis of Pithecellobium-Type Hierarchical Dual-Phase Nanostructured Cu(x)O to Columnar Self-Assembled CuO and Its Electrochemical Performances

[Image: see text] The search for low-cost environmentally benign promising electrode materials for high-performance electrochemical application is an urgent need for an applaudable solution for the energy crisis. For this, the present attempt has been made to develop a scalable synthetic strategy for the preparation of pure and dual-phase copper oxide self-hybrid/self-assembled materials from a copper oxalate precursor using the calcination route. The obtained samples were characterized by means of various physicochemical analytical techniques. Notably, we found that the BET surface area and pore volume of copper oxides measured by N(2) adsorption–desorption decrease with the elevation of calcination temperature. From the XRD analysis, we observed the formation of a Cu(2)O cubic phase at low temperatures and a CuO monoclinic phase at high temperatures (i.e., 450 and 550 °C). FTIR and RAMAN spectroscopy were employed for bonding and vibrational structure analysis. The self-assembled dual-phase copper oxide particle as a pithecellobium-type hierarchical structure was observed through SEM of the sample prepared at 350 °C. The surface morphological structure for the samples obtained at 450 and 550 °C was a bundle-like structure developed though columnar self-assembling of the particles. All the above techniques confirmed the successful formation of Cu(2)O/CuO nanoparticles. Afterward, the electrochemical properties of the as-synthesized copper oxides reinforced by introducing carbon black (10% wt) were explored via cyclic voltammetry, electrochemical impedance spectroscopy, and galvanometric charge–discharge analysis. The Cu(2)O system exhibits the maximum specific capacitance performance value of 1355 F/g, whereas in the CuO system (at 450 and 550 °C), it possesses values of 903 and 724 F/g at a scan rate of 2 mV/s. This study reveals that the electrochemical properties of Cu(2)O are better than those of the CuO nanoparticles, which could be ascribed to the high surface area and morphology. The present assessment of the electrochemical properties of the developed material could pave the way to a low-cost electrode material for developing other high-performance hybrid electrodes for supercapacitor or battery applications.