1：Experimental Design and Method Selection:

A two-step synthesis method was used to fabricate exfoliated MoS2@ZIF-8 hybrids. Exfoliated MoS2 was prepared by sonication in methanol, and then encapsulated into ZIF-8 by adding it during ZIF-8 synthesis. The rationale was to combine the visible-light absorption of exfoliated MoS2 with the porous structure of MOFs for improved photocatalytic performance.

2：Sample Selection and Data Sources:

MoS2 bulk powder and methanol were purchased from Sigma-Aldrich. Zinc nitrate hexahydrate and 2-methylimidazole were used for ZIF-8 synthesis. Samples included exfoliated MoS2 (EM), ZIF-8, and the composite MZ (MoS2@ZIF-8).

3：8). List of Experimental Equipment and Materials:

3. List of Experimental Equipment and Materials: Equipment included an ultrasonic bath, probe sonicator, centrifuge, vacuum dryer, scanning electron microscope (Hitachi S-4800), X-ray diffractometer (Bruker D8 Discover), Raman microscope (Renishaw), XPS system (PerkinElmer PHI 5440 ESCA), BET surface area analyzer (ASAP2020, Micromeritics), gas-sorption system (Quantachrome Autosorb), solar light simulator (Newport Oriel Sol1ATM 94021A), and gas chromatography (Agilent 7890A). Materials included MoS2 powder, methanol, zinc nitrate hexahydrate, 2-methylimidazole, and de-ionized water.

4：Experimental Procedures and Operational Workflow:

For exfoliated MoS2 synthesis, 100 mg MoS2 was sonicated in methanol for 1 h in an ultrasonic bath and 1 h with probe sonication, with temperature kept below 277 K. The top two-thirds were collected. For MZ synthesis, zinc nitrate was added to exfoliated MoS2 solution, then mixed with 2-methylimidazole, stirred for 12 h, centrifuged at 10,000 rpm for 5 minutes, and vacuum-dried. Characterization involved SEM, XRD, EDS, XPS, BET, and UV-Vis spectroscopy. Photocatalytic tests used a reactor with N2 carrier gas, water-methanol vapor, and visible light irradiation (Xe lamp, AM 1.5 G, 100 mW cm-2), with hydrogen production measured by GC every 15 min.

5：5 G, 100 mW cm-2), with hydrogen production measured by GC every 15 min. Data Analysis Methods:

5. Data Analysis Methods: XRD patterns were compared to standard references (PDF#37-1742 for MoS2 and literature for ZIF-8). BET surface area was calculated from N2 adsorption isotherms. XPS spectra were analyzed for chemical states. UV-Vis spectra were used to determine band gaps via Tauc's plot. Hydrogen evolution rates were quantified from GC measurements.