LAUSR

Ni–Sb–SnO₂ (NATO) has demonstrated significant practical advantages for electrochemical ozone production (EOP) and wastewater treatment. However, its limited lifetime poses challenges for environmental applications. In this study, bilayer electrocatalysts (NATO/C‐ATO) with an inner layer doped with carbon material were synthesized by electrodeposition combined with multiple quenching processes. It exhibited excellent EOP activity and stability under acidic conditions, achieving a current efficiency of 34.4% and an accelerated lifetime of 121 h. Additionally, a continuous flow stacked electrolyzer was designed via a combination of flow field simulation and experimental validation. Compared to conventional batch reactors, this design intensifies the mass and heat transfer processes in operation, enabling the production of ozonated water at a high concentration of 36.6 mg h−1 and the rapid degradation of organic pollutants. This work provides new insights into the design of efficient electrocatalysts and application equipment for advanced oxidation processes.