Partially Reduced Ni-NiO-TiO₂ Photocatalysts for Hydrogen Production from Methanol–Water Solution

The study compares the photocatalytic behavior of TiO2, NiO-TiO2, and Ni-NiO-TiO2 photocatalysts in photocatalytic hydrogen production from methanol–water solution. TiO2 and NiO-TiO2 photocatalysts with theoretical NiO loading of 0.5, 1.0, and 3.0 wt. % of NiO were prepared by the sol–gel method. The Ni-NiO-TiO2 photocatalysts were prepared by partial reduction of NiO-TiO2 in hydrogen at 450 °C. The Ni-NiO-TiO2 photocatalysts showed significantly higher hydrogen production than the NiO-TiO2 photocatalysts. The structural, textural, redox, and optical properties of all of the prepared photocatalysts were studied by using XRD, SEM, N2- adsorption, XPS, H2-TPR, and DRS. Attention is focused on the contribution of Ni loading, the surface composition (Ni2+, the lattice O2− species, and OH groups), the distribution of Ni species (dispersed NiO species, crystalline NiO phase, and the metallic Ni0 species), oxygen vacancies, TiO2 modification, the TiO2 crystallite size, and the specific surface area