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CuO thin films with broccoli-like structure were prepared using a facile hydrothermal method to construct photocathodes for water-splitting application. The morphological, structural, and optical properties of thin films were characterized and measured using several techniques, including X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), photoluminescence (PL), and ultraviolet-visible spectroscopy (UV-Vis). The thickness, structure, and morphology of CuO thin films can be controlled by varying the precursor concentration (Cp) and reaction temperature (Tr), which are also discussed. Moreover, the electrical properties of CuO thin films were also measured in the three-electrode system. The photocurrent density of photocathodes, when synthesized by a 0.5 M solution at 150 °C for 12 h, was 0.5 mA/cm2 at −0.6 V vs. Ag/AgCl, which is 1.8 times higher than that of photocathodes synthesized in a 0.1 M solution at 100 °C with the same reaction time. In addition, increasing the reaction temperature and precursor concentration aided in the enhancement of the IPCE and APCE values, which peaked at a wavelength range of 330–400 nm.

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