1：Experimental Design and Method Selection:

The study used a one-step magnetron sputtering method to synthesize TiO2 films with controlled morphology and defects. The rationale was to leverage sputtering advantages such as substrate temperature control, ion impinging effects, and O2 partial pressure variation to achieve desired nanostructures and defects.

2：Sample Selection and Data Sources:

TiO2 thin films were deposited on quartz glass substrates (2 cm × 4 cm). Samples T1, T2, and T3 were prepared with different O2 flow rates and substrate temperatures.

3：List of Experimental Equipment and Materials:

Equipment includes RF magnetron sputtering system, high-purity Ti target (

4：999%, 2-inch diameter), Cu foil (999% pure), quartz glass substrates, Ar and O2 gases (999% purity), ultrasonic cleaner, annealing furnace, Xe lamp (300 W), calibrated Si photodiode, and various characterization tools (XRD, AFM, SEM, TEM, XPS, EPR, PL spectroscopy). Materials include deionized water, acetone, ethanol, methanol. Experimental Procedures and Operational Workflow:

Substrates were cleaned ultrasonically with deionized water, acetone, and ethanol. Sputtering was performed with specific RF power, substrate temperature, O2 flow rate, and sputtering time. Post-deposition annealing at 500°C for 6 hours was done to enhance crystallinity. Photocatalytic tests involved immersing films in methanol aqueous solution or pure water under Xe lamp irradiation, with gas evolution measured over time.

5：Data Analysis Methods:

XRD for phase identification, AFM and SEM for morphology, TEM for crystal structure, XPS for chemical composition, EPR for defect analysis, PL for carrier dynamics, and hydrogen generation rates were calculated from gas evolution data. Apparent quantum efficiency was evaluated using a specific equation.