1：Experimental Design and Method Selection:

A two-step solvothermal method followed by an in situ photodeposition process was used to synthesize 1D Cd1?xZnxS@O-MoS2/NiOx nanohybrids. The design rationale involves tuning Zn-doping content, O-MoS2 layer growth, and NiOx deposition to optimize band alignments, active sites, and charge separation.

2：Sample Selection and Data Sources:

Samples include Cd1?xZnxS solid solutions (x = 0, 0.05, 0.10, 0.15), O-MoS2 nanosheets, and their hybrids. Data were acquired through various characterization techniques.

3：05, 10, 15), O-MoS2 nanosheets, and their hybrids. Data were acquired through various characterization techniques. List of Experimental Equipment and Materials:

3. List of Experimental Equipment and Materials: Chemicals from Sinopharm Chemical Reagent Co., Ltd. (analytical grade), autoclaves, ovens, ultrasonication equipment, and characterization instruments (e.g., XRD, SEM, TEM, UV-vis spectrometer, electrochemical workstation).

4：Experimental Procedures and Operational Workflow:

Synthesis involved solvothermal reactions in ethylenediamine and DMF, photodeposition under light irradiation, washing, drying, and characterization. Photocatalytic HER tests were conducted in a Labsolar-6A system with a Xe lamp and gas chromatograph.

5：Data Analysis Methods:

Bandgap energies calculated from UV-vis spectra using Tauc plots, CBM potentials determined using empirical formulas, photocurrent and EIS measurements for charge separation analysis, and AQY calculated based on H2 evolution and photon counts.