Synergistic Photo‐Electro‐Fenton Oxidation of Antibiotics Using a Ferrocene‐Functionalized <scp>MXene</scp> (Ti ₃ C ₂ T _x ) Electrode

The persistence of antibiotics such as tetracycline in aquatic systems poses severe environmental and health risks by potential antimicrobial resistance. To address this, a hybrid photo‐electro‐Fenton oxidation system based on MXene‐derived electrodes was developed for efficient tetracycline degradation. The integration of photo, electro, and Fenton processes synergistically enhances hydroxyl radical (•OH) generation and charge‐carrier separation, ensuring superior removal efficiency. The cathode was synthesized via a Schiff base formation method, which facilitates functionalization of Ti 3 C 2 T x MXene with ferrocene, as confirmed by X‐ray diffraction, X‐ray photoelectron spectroscopy, and UV–visible spectrometry. The Ti 3 C 2 –TiO 2 photoanode was fabricated by electrochemical oxidation of Ti 3 C 2 T x . The photocatalytic properties of anatase TiO 2 , when combined with Ti 3 C 2 T x , create a Schottky junction that significantly improves charge separation, thereby enhancing the photo‐electrocatalytic activity of the system. The hybrid photo‐electro‐Fenton (PEF) system demonstrates a substantial enhancement in tetracycline removal efficiency (∼90%) compared to unmodified Ti 3 C 2 T x ‐based electrodes (∼46%). Furthermore, the Ti 3 C 2 –TiO 2 Schottky photoanode showed enhanced removal efficiency over a commercial P25‐based photoanode for photocatalytic degradation. Through this hybrid PEF oxidation system, the removal efficiencies achieved above 90% in neutral and acidic pH, indicating significant efficacy for the advanced oxidation process. The transformation products formed during the PEF process were analyzed with liquid chromatography coupled with high‐resolution mass spectrometry, showing breakdown of tetracycline and decreasing ecotoxicity with increasing treatment time. Moreover, the MXene‐derived electrode system demonstrates stability and consistent degradation performance over numerous cycles, making it a promising material for environmental remediation applications.