<p>α-NaVOPO₄ has emerged as a highly promising cathode material for sodium-ion batteries, thanks to its impressive theoretical capacity (144.9 mAh g⁻¹) and elevated operating voltage. However, its practical application is hindered by poor electronic conductivity. In this study, small particle size and exceptional uniformity of α-NaVOPO₄ were successfully synthesized using a two-step hydrothermal method. This approach preserves the intrinsic advantages of α-NaVOPO₄ while improving particle microstructure, effectively boosting the electrochemical performance of the cathode. The successful synthesis of pure-phase α-NaVOPO₄, along with its desired structural and morphological properties, was rigorously confirmed through X-ray diffraction and scanning electron microscopy. To assess the material’s sodium storage performance, its electrochemical behavior was evaluated in a Na||NaVOPO₄ half-cell, employing both galvanostatic charge/discharge cycling and cyclic voltammetry for comprehensive analysis.</p>