1：Experimental Design and Method Selection:

A facile hydrothermal method was used to synthesize 3D flower-like Fe2O3/MoS2 heterostructures, and a surface modification method involving hydrolysis of tetraethylorthosilicate (TEOS) was employed to coat the composites with amorphous Si-oxyhydroxides (SiOxH).

2：Sample Selection and Data Sources:

Samples included bare Fe2O3 nanoparticles, Fe2O3/MoS2 nanocomposites with varying Mo:Fe ratios (2MF, 3MF, 4MF, 6MF), and SiOxH-coated Fe2O3/MoS

3：Methyl blue (MB) solution (20 mg/L) was used as the photocatalytic indicator. List of Experimental Equipment and Materials:

Equipment included a Rigaku D/MAX 2500PC diffractometer for XRD, JSM-6700F SEM, JEM-2100F HRTEM, ESCALAB Mk II XPS spectrometer, fluorescence spectrophotometer for PL spectra, and a 300 W xenon lamp (CEL-HXUV300) with AM

4：5 filter for photocatalytic measurements. Materials included ferric chloride hexahydrate, sodium acetate, Na2MoO4·2H2O, CH4N2S, TEOS, ethanol, deionized water, NaOH, and H2OExperimental Procedures and Operational Workflow:

Fe2O3 nanoparticles were synthesized hydrothermally at 200°C for 24h. Fe2O3/MoS2 composites were prepared by adding Fe2O3 to a solution with Na2MoO4·2H2O and CH4N2S, followed by hydrothermal treatment at 200°C for 24h. SiOxH coating was achieved by hydrolyzing TEOS in a suspension with Fe2O3/MoS2, ethanol, and NaOH, stirred for 24h at room temperature and dried. Photocatalytic tests involved degrading MB solution under simulated solar irradiation, with air bubbling and magnetic stirring; photo-Fenton reaction included adding H2O2 to adjust pH to

5：4h. Fe2O3/MoS2 composites were prepared by adding Fe2O3 to a solution with Na2MoO4·2H2O and CH4N2S, followed by hydrothermal treatment at 200°C for 24h. SiOxH coating was achieved by hydrolyzing TEOS in a suspension with Fe2O3/MoS2, ethanol, and NaOH, stirred for 24h at room temperature and dried. Photocatalytic tests involved degrading MB solution under simulated solar irradiation, with air bubbling and magnetic stirring; photo-Fenton reaction included adding H2O2 to adjust pH to Data Analysis Methods:

4.0. 5. Data Analysis Methods: XRD patterns were analyzed for phase identification, SEM and TEM for morphology, XPS for surface chemistry, PL spectra for carrier transfer, and UV-visible spectrometry for degradation efficiency by monitoring absorbance at 664 nm.