The reactive oxygen species (ROS) contribute to photodegrading tetracycline (TC), which determines the overall efficiency of photocatalysts. Superoxide radical (·O₂^–) is one of the excellent ROS for photodegrading TC by carbon nitride. However, achieving hierarchical carbon nitride with efficient, stabile, and selective production of ·O₂^– via O₂ photoreduction is a great challenge. Herein, a carbon nitride oxide nest (CNON₆) with carbon/nitrogen vacancies (C-v, N-v) and oxygen substitution (O-s) was prepared via tailoring surface microenvironment. The CNON₆ can photodegrade 82% of TC within 2 min under visible light, and the pseudo-first-order kinetic constant is 1.22 min⁻¹, 24-fold higher than that of CN. The superior photoactivity is attributed to a unique surface microenvironment, which N-v increased photoelectric conversion efficiency, C-v enhanced O₂ adsorption and O-s induced ·O₂^– evolution with ∼ 100% selectivity. Moreover, PVDF membrane-supported CNON₆ (11.33 cm², 0.88 mg/cm²) can completely remove TC from wastewater at a rate of 2.62 mg/h in a simulated industrial continuous flow cell. The cost-effectiveness assessment was $6.36/kg/h, implying the CNON₆/PVDF has a bright application prospect in wastewater treatment. This work developed a surface microenvironment tailor strategy to design photocatalysts for efficient degradation of TC.

活性氧 (ROS) 有助于光降解四环素 (TC)，这决定了光催化剂的整体效率。超氧自由基(·O ₂ ^– )是一种用于氮化碳光降解TC的优良ROS。^{然而，通过}O _{2光还原实现高效、稳定和选择性地产生·O 2}的分级碳氮化物是一个巨大的挑战。在此，通过定制表面微环境制备了具有碳/氮空位（Cv，Nv）和氧取代（Os）的氮氧化物巢（CNON _{6 ）。}CNON ₆在可见光下2 min内可光降解82%的TC，准一级动力学常数为1.22 min^-1，比 CN 高 24 倍。优异的光活性归因于独特的表面微环境，其中 Nv 提高了光电转换效率，Cv 增强了 O ₂吸附，Os 诱导了·O ₂ ^–释放，选择性约为 100%。此外，PVDF 膜负载的 CNON ₆ (11.33 cm ² , 0.88 mg/cm ² ) 可以在模拟工业连续流通池中以 2.62 mg/h 的速率完全去除废水中的 TC。成本效益评估为 $6.36/kg/h，意味着 CNON ₆/PVDF在废水处理中具有广阔的应用前景。这项工作开发了一种表面微环境定制策略来设计光催化剂以有效降解 TC。