1：Experimental Design and Method Selection:

The study involved the hydrothermal synthesis of TiO2 nanofibers, followed by thermal reduction under H2/Ar to introduce oxygen vacancies. Cyanide-assisted heat-treatment was used for oxygen vacancy rearrangement. Fe-containing polyoxometalates were then coupled with the defect-rearranged TiO2 to construct Fenton-like photocatalysts.

2：Sample Selection and Data Sources:

Commercial p25 TiO2 was used as the starting material. The performance of the catalysts was evaluated by degrading organic pollutants under simulated solar light.

3：List of Experimental Equipment and Materials:

Instruments included XRD, FE-SEM, HR-TEM, XPS, UV-vis DRS, ESR, fluorescence spectrometer, and HPLC. Materials included NaOH, HCl, FeCl3, H3PW12O40?xH2O, and organic pollutants.

4：Experimental Procedures and Operational Workflow:

The synthesis involved hydrothermal reaction, thermal reduction, cyanide-assisted heat-treatment, and impregnation method for catalyst fabrication. Photocatalytic activity was assessed by measuring the degradation of pollutants under light irradiation.

5：Data Analysis Methods:

The degradation efficiency was calculated by C/C0, where C was the concentration of pollutant at each irradiated time interval and C0 was the initial concentration. ESR and PL spectra were used to analyze reactive species and charge transfer behavior.