1：Experimental Design and Method Selection:

A two-step hydrothermal method was used to synthesize TiO2 nanoplates and MoS2 nanosheets, followed by hydrothermal synthesis of MoS2/TiO2 composites with varying MoS2 content (5, 10, 30, 50 wt%). The design rationale was to create a heterostructure to improve charge separation and light absorption.

2：Sample Selection and Data Sources:

Samples included pure TiO2, pure MoS2, and MoS2/TiO2 composites with different MoS2 loadings. Data were obtained from characterization techniques and photocatalytic tests.

3：List of Experimental Equipment and Materials:

Equipment included D2 PHASER diffractometer (Bruker), Quanta 200 SEM, JEOL 2100 TEM, Micromeritics TriStar II BET analyzer, UH4150 spectrophotometer (HITACHI), FT-IR spectrometer (Thermo Electron), LS55 fluorescence spectrometer (Perkin Elmer), LC-MS (Agilent 5977A), Lambda 35 UV-vis spectrophotometer (Perkin Elmer), gas chromatograph (GC7890B, Agilent), Parstat 2273 Electrochemical workstation (Princeton Applied Research). Materials included tetrabutyl titanate, hydrofluoric acid, sodium molybdate dehydrate, thioacetamide, deionized water, ethanol, RhB, methanol, Na2SO4, etc.

4：Experimental Procedures and Operational Workflow:

TiO2 was synthesized by hydrothermal treatment of Ti(OBu)4 and HF at 180°C for 24 h. MoS2 was synthesized by hydrothermal reaction of Na2MoO4·2H2O and C2H5NS at 200°C for 24 h. MoS2/TiO2 composites were prepared by mixing precursors with TiO2 and hydrothermal treatment at 200°C for 24 h. Characterization involved XRD, SEM, TEM, BET, UV-vis DRS, FT-IR, PL, XPS, EDX. Photocatalytic tests included RhB degradation under 400W metal halide lamp and hydrogen production under 300W xenon arc lamp, with photoelectrochemical measurements using a three-electrode system.

5：Data Analysis Methods:

XRD patterns were analyzed for crystal structure, BET for surface area, UV-vis DRS for band gap calculation using Tauc plot, photocatalytic kinetics using pseudo-first-order model, EIS using Randles-Ershler equivalent circuit, and statistical analysis of photocurrent and hydrogen production rates.