| Summary: | Semiconductor-based photocatalyst materials play an important role in solar hydrogen production. In the present work, we achieved the successful synthesis of a CeO<sub>2</sub>/MoS<sub>2</sub> composite using a facile hydrothermal method. For the preparation of the CeO<sub>2</sub>/MoS<sub>2</sub> composite, the hydrothermal process was carried out at a temperature of 120 °C for 24 h, and its performance in hydrogen production was tested. The CeO<sub>2</sub>/MoS<sub>2</sub> composite was characterized using XRD, XPS, Raman spectroscopy, SEM, and optical investigation. The optical study showed that after forming a composite with MoS<sub>2</sub>, the absorption edge of CeO<sub>2</sub> is shifted from the ultraviolet to the visible light region. Bandgap values decreased from 2.93 for CeO<sub>2</sub> to 2.34 eV for the CeO<sub>2</sub>/MoS<sub>2</sub> composite. In photocatalytic hydrogen production, Na<sub>2</sub>SO<sub>3</sub>–Na<sub>2</sub>S was used as a sacrificial agent. The CeO<sub>2</sub>/MoS<sub>2</sub> composite exhibited superior photocatalytic hydrogen production performance compared to CeO<sub>2</sub> and MoS<sub>2</sub>. The CeO<sub>2</sub>/MoS<sub>2</sub> composite achieved higher charge separation efficiency, faster charge transfer, more active sites available for redox reactions, and greater affinity towards the reactant ions due to such properties its hydrogen evolution rate has reached 112.5 μmol/h. The photostability of the CeO<sub>2</sub>/MoS<sub>2</sub> composite was tested in up to four cycles, with each cycle being four hours.
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