In this work, a low-cost, high-yield hydrothermal treatment was used to produce nanozeolite (Zeo), nanoserpentine (Serp), and Zeo/Serp nanocomposites with weight ratios of 1:1 and 2:1. At 250 °C for six hours, the hydrothermal treatment was conducted. Various methods are used to explore the morphologies, structures, compositions, and optical characteristics of the generated nanostructures. The morphological study revealed structures made of nanofibers, nanorods, and hybrid nanofibril/nanorods. The structural study showed clinoptilolite monoclinic zeolite and antigorite monoclinic serpentine with traces of talcum mineral and carbonates. As a novel photoelectrochemical catalyst, the performance of the Zeo/Serp (2:1) composite was evaluated for solar hydrogen generation from water splitting relative to its constituents. At −1 V, the Zeo/Serp (2:1) composite produced a maximum current density of 8.44 mA/g versus 7.01, 6.74, and 6.6 mA/g for hydrothermally treated Zeo/Serp (1:1), Zeo, and Serp, respectively. The Zeo/Serp (2:1) photocatalysts had a solar-to-hydrogen conversion efficiency (STH) of 6.5% and an estimated hydrogen output rate of 14.43 mmole/h.g. Consequently, the current research paved the way for low-cost photoelectrochemical catalytic material for efficient solar hydrogen production by water splitting.
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