UiO-66-Derived Self-Supporting Carbon Nanofiber Membrane with Enriched Zr Sites and Oxygen Vacancies for Enhanced Electro-Fenton Degradation

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Abstract
To address the pressing need for efficient azo dye wastewater treatment, a novel self-supporting electro-Fenton (EF) cathode (Zr-C/NFME) was fabricated via electrospinning and programmed carbonization using UiO-66 as a precursor. UiO-66-derived Zr–O bonds facilitate the uniform exposure of Zr sites. Combined EPR and O 1s XPS analyses verify the dynamic generation of oxygen vacancies during reaction, which promotes interfacial electron transfer, accelerates the Fe3+/Fe2+ redox cycle, and enhances the in-situ H2O2 activation. EPR and quenching tests reveal that ·OH dominates degradation, with ·O2- playing a synergistic role. Benefiting from these integrated advantages, Zr-C/NFME achieves 94.7% removal of methyl orange (MO) within 30 min, demonstrating broad pH adaptability, applicability to diverse dyes, and stable performance over 5 consecutive cycles. TOC and COD removal rates reach 40.7% and 43.5% after 1 h. DFT and LC-MS identified azo bonds, tertiary amines, and sulfonic groups as primary radical attack sites, and ECOSAR assessment confirms reduced ecotoxicity of intermediates. This study provides a novel strategy for designing high-performance, stable self-supporting EF cathodes with promising application in organic wastewater remediation.

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