1：Experimental Design and Method Selection:

A photo-assisted deposition method was used to synthesize MoS2/TiO2 composites, with characterization via XRD, Raman, SEM, TEM, XPS, UV-vis DRS, PL, and ESR. Photocatalytic activity was tested under visible light.

2：Sample Selection and Data Sources:

TiO2 nanoparticles were commercially available, and MoS2 was deposited on TiO2 using (NH4)2[MoS4] and EDTA in deionized water. Samples were labeled based on irradiation time (5 to 60 min).

3：List of Experimental Equipment and Materials:

Equipment included SEM (HITACHI S-4800), TEM (FEI Tecnai G2 F30 S-Twin), XRD (Bruker D8 Advance), XPS, Raman microscope (Renishaw 300), UV-vis spectrophotometer (Shimadzu UV-2550), PL spectrofluorometer (FS5 from Edinburgh Instruments), ESR spectrometer (Bruker E500), and a 500 W xenon lamp with 420 nm cutoff filter. Materials included TiO2 powder, (NH4)2[MoS4], EDTA, MB, 2-CP, t-BuOH, BQ, and TA.

4：Experimental Procedures and Operational Workflow:

Synthesis involved dissolving precursors, adding TiO2, ultrasound, nitrogen saturation, sunlight irradiation for varying times, washing, drying, and calcination. Photocatalytic tests involved adding catalyst to pollutant solution, dark equilibration, visible light irradiation, sampling, centrifugation, and concentration measurement via UV-vis. Radical trapping used scavengers, and ESR/PL for active species detection.

5：Data Analysis Methods:

Data were analyzed using UV-vis for concentration changes, XRD for crystal structure, Raman for bonding, XPS for composition, and ESR/PL for radical identification. Statistical analysis of degradation efficiencies was performed.