Biomass-derived hard carbon (HC) represents a promising anode candidate for sodium-ion batteries, owing to its disordered structure and abundant micropores. This study systematically investigates three chemical oxidation strategies (NaClO, H
2 SO
4 and H
2 O
2 +NaOH) applied to cotton stalk-derived
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Biomass-derived hard carbon (HC) represents a promising anode candidate for sodium-ion batteries, owing to its disordered structure and abundant micropores. This study systematically investigates three chemical oxidation strategies (NaClO, H
2 SO
4 and H
2 O
2 +NaOH) applied to cotton stalk-derived HC carbonized at 1300 °C. The NaClO-treated sample delivers the optimal overall electrochemical performance, achieving a high discharge capacity of 330.2 mAh g
−1 at 0.1 C, a high initial Coulombic efficiency (ICE) of 81.7%, and a capacity retention of 81.9% after 1000 cycles at 2 C (from 226.0 to 185.1 mAh g
−1 ). This superiority is attributed to the formation of a three-dimensional hierarchical pore network and optimal oxygen functional groups. The H
2 SO
4 treatment yields a discharge capacity of 323.2 h g
−1 , an ICE of 75.3%, and a capacity retention of 77.1% after 1000 cycles (from 183.5 to 141.5 mAh g
−1 ), benefiting from structural densification. The H
2 O
2 +NaOH treatment delivers a capacity of 269.8 mAh g
−1 and an ICE of 74.2%, exhibiting a distinct activation behavior likely due to its thin pore walls and abundant open mesopores. Overall, all treated samples significantly outperformed the pristine HC, which exhibits a discharge capacity of 320.3 mAh g
−1 , an ICE of 68.0%, and a retained capacity of 90.4 mAh g
−1 after 1000 cycles at 2 C.
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