1：Experimental Design and Method Selection:

The study employs a coupled photocatalytic system where TiO2 with in situ generated oxygen vacancies (OVs) catalyzes both nitrobenzene reduction and benzyl alcohol oxidation under visible light. Theoretical models include density functional theory (DFT) for electronic structure calculations and experimental characterizations to validate OVs formation and carrier dynamics.

2：Sample Selection and Data Sources:

Anatase TiO2 microspheres synthesized via microwave-assisted method; commercial reagents like benzyl alcohol, nitrobenzene, and benzotri?uoride used without purification; data from XRD, SEM, TEM, BET, UV-vis, EPR, TRPL, and electrochemical measurements.

3：List of Experimental Equipment and Materials:

Equipment includes microwave oven (Initiator 8 EXP, Biotage Corp), XRD (Rigaku MiniFlex 600), SEM (JSM6700), TEM (JEM2010), BET analyzer (Micromeritics ASAP 2020), UV-vis spectrometer (Shimadzu UV-2600), EPR spectrometer (Bruker-BioSpin E500), TRPL system (Coherent Libra Regenerative Amplifier with BBO crystal), gas chromatograph (Agilent 7890A), GC-MS (430 GC Varian), electrochemical station (ZM6ex, Zahner). Materials include TiCl4, methanol, acetic acid, NaF, benzyl alcohol, nitrobenzene, benzotri?uoride, n-dodecane, triethanolamine, CCl4, Na2SO4, TBAPF6, CH3CN.

4：Experimental Procedures and Operational Workflow:

Synthesis of TiO2 via microwave reaction; photocatalytic tests in N2 atmosphere with light irradiation (300-W Xenon Illuminator System, CM 1 filter); sample characterization before and after reaction; electrochemical measurements on FTO electrodes; DFT calculations for surface interactions and electronic properties.

5：Data Analysis Methods:

Conversion and yield calculations from GC data; EPR and TRPL for OVs and carrier lifetime; Mott-Schottky and photocurrent for semiconductor properties; DFT for energy levels and adsorption mechanisms.