<p>Green synthesis is a sustainable and environmentally friendly approach for designing efficient electrode materials to meet the growing demand for supercapattery electrodes. In this work, Aloe vera-assisted synthesis of phase-pure spinel NiCo₂O₄ nanomaterial was achieved through a simple and eco-friendly route. Synchrotron XRD confirmed excellent crystallinity and phase purity, while FTIR identified characteristic metal-oxygen bonds together with Aloe vera-derived organic functionalities. FESEM and TEM provided morphological insights, while BET analysis, confirming mesoporosity with a surface area of 18.61 m² g⁻¹, and average pore diameter of ~ 14.7&#xa0;nm. Synchrotron XPS revealed mixed Ni/Co oxidation states and abundant oxygen vacancies, which promote enhanced redox activity and rapid charge-transfer kinetics. The Alv-NiCo₂O₄ electrode exhibited high specific capacitance (609.6&#xa0;F g⁻¹ at 5 mV s⁻¹; 471.1&#xa0;F g⁻¹ at 1&#xa0;A g⁻¹), excellent rate capability, and long-term durability, retaining 97% capacitance and 99.6% coulombic efficiency over 5000 charge-discharge cycles at 20&#xa0;A g⁻¹. These findings demonstrate that Aloe vera-derived NiCo₂O₄ is a cost-effective, sustainable, and high-performance green electrode for supercapattery applications.</p>