Layered NaCrO₂ is considered a promising cathode material for sodium-ion batteries (SIBs) due to its high theoretical capacity and structural simplicity. However, its practical application is hindered by capacity fading and poor rate performance, pr...
Layered NaCrO₂ is considered a promising cathode material for sodium-ion batteries (SIBs) due to its high theoretical capacity and structural simplicity. However, its practical application is hindered by capacity fading and poor rate performance, primarily caused by sluggish Na⁺ kinetics, phase transitions, and interfacial deterioration during prolonged cycling. In this study, we systematically investigated the effect of varying H₂/Ar atmospheric heat treatments during the synthesis of NaCrO₂. Structural and surface analyses using XRD, SEM, TEM, Raman, and XPS revealed that hydrogenation induced beneficial oxygen vacancies without altering the particle morphology. Electrochemical studies demonstrated that the NCO-25 sample achieved the highest reversible capacity of 106 mAh g⁻¹ at 2 C after 300 cycles, significantly outperforming the bare NCO sample (52 mAh g⁻¹). This superior performance is attributed to the abundant oxygen vacancies, which facilitated rapid electron/ion transport and enhanced structural stability. Quantitative analysis revealed that both diffusion-controlled and capacitive-controlled processes contributed to the electrochemical sodium storage behavior of the electrode. Furthermore, the NCO-25//HC full cell exhibited excellent cycling stability, retaining 86.3% of its initial capacity after 300 cycles. This study offers new insights into synthetic reduction engineering for Na-based cathodes and provides a promising pathway for optimizing the performance of NaCrO₂ and related layered oxide materials in sodium-ion batteries.