1：Experimental Design and Method Selection:

A facile hydrothermal method was used with surfactant assistance (F68) to synthesize monodispersed hierarchical hollow MoS2 microspheres. The design rationale was to achieve structures with large surface area, strong light absorption, and rich catalytic sites.

2：Sample Selection and Data Sources:

Chemicals like ammonium molybdate, thioacetamide, and F68 were used. Samples included hierarchical hollow MoS2 microspheres, MoS2 particles (without F68), and commercial MoS2 for comparison.

3：List of Experimental Equipment and Materials:

Equipment included a Teflon-lined stainless steel autoclave, vacuum oven, magnetic stirrer, xenon lamp (500 W and 300 W), UV/vis/NIR spectrophotometer (Hitachi U-4100), electrochemical workstation (CHI 760E), XRD (Philips X'Pert Pro), SEM (JEOL-6610-LV), TEM (JEOL JEM-2100), BET equipment (Micromeritics ASAP 2020), and fluorescence spectrophotometer (F280). Materials included ammonium molybdate, thioacetamide, F68, RhB, H2O2, Nafion solution, and various electrodes.

4：0). Materials included ammonium molybdate, thioacetamide, F68, RhB, H2O2, Nafion solution, and various electrodes. Experimental Procedures and Operational Workflow:

4. Experimental Procedures and Operational Workflow: Synthesis involved hydrothermal reaction at 180°C for 8 h. Photocatalytic tests involved degrading RhB with H2O2 under white light irradiation, with sampling and centrifugation at intervals. Photoelectrochemical tests used a three-electrode cell with specific electrodes and electrolyte.

5：Data Analysis Methods:

Data were analyzed using UV/vis spectroscopy for concentration measurements, BET for surface area, XRD for phase purity, SEM/TEM for morphology, PL spectra for charge carrier analysis, and kinetic models for degradation rates.