Dual Enhancement of Electrochemical Ozone Production and Chlorine Evolution Reaction over Sulfur‐Doped 3D Ni‐Sb‐SnO 2 Electrodes

ABSTRACT Electrochemical ozone production (EOP) and chlorine evolution reaction (CER) are promising green and efficient oxidation technologies for water treatment. However, conventional electrode materials demonstrate limited electrocatalytic activity, hindering their practical application. To address these limitations, this study introduced sulfur into the Ni‐Sb‐SnO 2 (DLS‐NATO/TiF) to modulate the electronic structure, constructing a high‐performance electrocatalyst for both EOP and CER. The results demonstrated that the DLS‐NATO/TiF achieved a Faradaic efficiency (FE) of 50.10% for EOP and 95.70% for CER under acidic conditions. In situ characterization and theoretical calculation revealed that the EOP process predominantly followed the lattice oxygen mechanism on the electrocatalyst. Sulfur doping facilitated lattice oxygen migration, stabilizing OOH * and O 2 * intermediates and lowering the reaction energy barrier, thereby enhancing EOP activity. In addition, sulfur incorporation reduced the overpotential at oxygen sites by tuning Cl * adsorption strength, which optimized the CER reaction pathway. Moreover, the electrocatalyst integrated into a continuous‐flow stacked cell achieved sterilization rates of 97.50% for E. coli and 99.89% for S. griseus, demonstrating significant potential for water treatment.