Oxalate-mediated synthesis of hybrid nickel cobalt-based nanostructures for boosting water and urea electrooxidation efficiency

The utilization of urea during electrolysis presents an appealing option for anodic oxidation, offering environmental benefits by converting waste into energy. The present work focuses on synthesizing mixed transition metal oxide (MMO) nanostructures composed of nickel rich nickel cobaltite electrode materials. Interesting, cobalt rich nickel cobaltite have been widely studied; however, the nickel-rich nickel cobaltite remains relatively unexplored. For stabilization of nickel rich nickel cobaltite, we have designed a process for synthesizing three-dimensional (3D) Ni-Co oxalate as a precursor via the coprecipitation method using diammonium oxalate monohydrate as a precipitating agent. The as obtained precursor was further subjected to thermal decomposition which results in the formation of Ni2CoO4. Microstructural analysis of Ni-Co oxalate indicates that oxalate-assisted synthesis leads to anisotropic ultrafine nanoparticle growth, forming hierarchically arranged 3D microflowers. Interestingly, the use of NaOH as a precipitating agent induces a significant change in the morphology of Ni2CoO4, (nanoparticles). Furthermore, the effect of morphology changes over the electrochemical performance was investigated. Ni2CoO4 microflower demonstrates an overpotential of 330mV@25mA/cm2 for O2 and -190 mV@10mA/cm2 for H2 production during water oxidation in 1M KOH, exhibiting excellent stability for up to 24h. During urea oxidation, the potential required by Ni2CoO4 microflowers was 1.31V@10mA/cm2. Ni2CoO4 nanoparticles' performance is significantly poor during water and urea oxidation compared to the microflower counterpart. Therefore, this work provides detailed insights into designing MMOs with high porosity, increased exposed active sites, and unique structural features that enhance electrocatalytic activity.