Background: In this work, we investigated the effect of nickel on the photocatalytic properties of TiO 2 nanostructures. The photocatalysts were obtained in a two-stage procedure. First, the sol-gel method was used for obtaining TiO 2 and Ni-TiO 2 at 1.0 wt% of Ni, which was then followed by hydrothermal treatment under highly alkaline conditions with NaOH at 110°C.Results: The obtained powders were thermally treated at 400°C. The main crystalline phase was anatase for all the samples, and a lower E g value was estimated for the Ni/TiO 2 sample (3.13 eV). The specific BET areas were obtained from N 2 isotherms at 77 K, being 141 and 153 m 2 /g for pure TiO 2 and 1.0% Ni-TiO 2 samples, respectively. Scanning electron microscopy confirmed the rod shape of the particles with diameters between 10 and 20 nm and length between 100 and 400 nm. X-ray photoelectron spectroscopy analysis showed the presence of oxygen vacancies and surface hydroxyl oxygen species in all samples, but in a higher ratio for the Ni/TiO 2 -HT-400 sample. The photocatalytic test was performed using two different radiation sources: 254 nm and a simulated solar lamp (300 W), for the photoreduction of 4-nitrophenol to 4-aminophenol, which was followed by UV-vis spectroscopy.Conclusions: The Ni/TiO 2 -HT-400 sample showed a high efficiency, reaching 100% reduction after 15 min (simulated solar radiation) and 40 min (⊗ = 254 nm) after the first cycle, while for the second cycle these values decreased to 63% and 78%, respectively. The increase in the photocatalytic reduction of TiO 2 nanostructures was achieved mainly through the presence of oxygen vacancies along with the decrease in electron-hole recombination.
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