In this study, the synthesis of hybrid photocatalysts of Zn-Al-In mixed metal oxides were activated by using visible light, derived from Zn-Al-In layered double hydroxide (ZnAlIn-LDH), and these nanocomposites demonstrated high efficiency for photocatalytic H2 production under UV light when using methanol as a sacrificial agent. The most active photocatalytic material produced 372 μmol h−1 g−1 of H2. The characterization of these materials included X-ray diffraction (DRX), infrared spectroscopy (FTIR), X-ray fluorescence spectroscopy (XRF), X-ray spectroscopy (XEDS), scanning electron microscopy analysis (SEM), transmission electron microscopy (TEM), diffuse reflectance spectroscopy, and N2- physisorption. In addition, the materials were characterized by photoelectrochemical techniques to explain the photocatalytic behavior. Subsequently, the photocatalytic performance for the water-splitting reactions under visible irradiation was evaluated. The ZnAlIn-MMOs with an In/(Al + In) molar ratio of 0.45 exhibited the highest photocatalytic activity in tests under visible light, attributed to the efficient separation and transport of photogenerated charge carriers originating from the new nanocomposite. This discovery indicates a method for developing new types of heteronanostructured photocatalysts which are activated by visible light.
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