Different sol-gel synthesis methods were used to obtain four nanostructured mesoporous TiO 2 samples for an efficient photocatalytic degradation of the emerging contaminant Nphenylurea under either simulated solar light (1 Sun) or UV light. Particularly, two TiO 2 samples were obtained by means of as many template-assisted syntheses, whereas other two TiO 2 samples were obtained by a greener template-free procedure, implying acidic conditions and, then, calcination at either 200°C or 600°C. In one case, anatase was obtained, whereas in the other three cases mixed crystalline phases were obtained. The four TiO 2 samples were characterized by X-ray powder diffraction (followed by Rietveld analysis); Transmission Electron Microscopy; N 2 adsorption/desorption at À 196°C; Diffuse Reflectance UV/Vis spectroscopy and ζ-potential measurements. A commercial TiO 2 powder (i. e., Degussa P25) was used for comparison. Differences among the synthesized samples were observed not only in their quantitative phase composition, but also in their nanoparticles morphology (shape and size), specific surface area, pore size distribution and pH IEP (pH at isoelectric point), whereas the samples band-gap did not vary sizably. The samples showed different photocatalytic behavior in terms of N-phenylurea degradation, which are ascribed to their different physico-chemical properties and, especially, to their phase composition, stemming from the different synthesis conditions.

Brookite positively affects solar photocatalysis, electrocatalysis and electrochemical applications by stabilizing photogenerated e−/h+ pairs. Brookite-related heterojunctions, cus Ti atoms, surface acidity and redox behaviour are crucial aspects.

Fe-doped titania photocatalysts (with 1, 2.5, and 3.5 wt. % Fe nominal content), showing photocatalytic activity under visible light, were prepared by a soft-template assisted sol–gel approach in the presence of the triblock copolymer Pluronic P123. An undoped TiO2 photocatalyst was also prepared for comparison. The photocatalysts were characterized by means of X-ray powder Diffraction (XRPD), Quantitative Phase Analysis as obtained by Rietveld refinement, Diffuse Reflectance (DR) UV−Vis spectroscopy, N2 adsorption/desorption at −196 °C, electrophoretic mobility in water (ζ-potential), and X-ray photoelectron spectroscopy (XPS). The physico-chemical characterization showed that all the samples were 100% anatase phase and that iron was present both in the bulk and at the surface of the Fe-doped TiO2. Indeed, the band gap energy (Eg) decreases with the Fe content, with Tauc’s plot determined values ranging from 3.35 (undoped TiO2) to 2.70 eV (3.5 wt. % Fe). Notwithstanding the obtained Eg values, the photocatalytic activity results under visible light highlighted that the optimal Fe content was equal to 2.5 wt. % (Tauc’s plot determined Eg = 2.74 eV). With the optimized photocatalyst and in selected operating conditions, under visible light it was possible to achieve 90% AO7 discoloration together with a TOC removal of 40% after 180 min. The kinetic behavior of the photocatalyst was also analyzed. Moreover, the tests in the presence of three different scavengers revealed that the main reactive species are (positive) holes and superoxide species. Finally, the optimized photocatalyst was also able to degrade phenol under visible light.

A reverse-micelle sol–gel method was chosen for the preparation of Fe-doped TiO2 samples that were employed in the photodegradation of the crystal violet dye under visible light irradiation in a batch reactor. The dopant amount was varied to assess the optimal photocatalyst composition towards the target dye degradation. The photocatalysts were characterized through a multi-technique approach, envisaging XRPD and QPA as obtained by Rietveld refinement, FE-SEM analysis, DR UV−vis spectroscopy, N2 adsorption/desorption isotherms measurement at −196 °C, ζ-potential measurement, and XPS analysis. The physical-chemical characterization showed that the adopted synthesis method allows obtaining NPs with uniform shape and size and promotes the introduction of Fe into the titania matrix, finally affecting the relative amounts of the three occurring polymorphs of TiO2 (anatase, rutile and brookite). By increasing the Fe content, the band gap energy decreases from 3.13 eV (with undoped TiO2) to 2.65 eV (with both 2.5 and 3.5 wt.% nominal Fe contents). At higher Fe content, surface Fe oxo-hydroxide species occur, as shown by DR UV-vis and XP spectroscopies. All the Fe-doped TiO2 photocatalysts were active in the degradation and mineralization of the target dye, showing a TOC removal higher than the undoped sample. The photoactivity under visible light was ascribed both to the band-gap reduction (as confirmed by phenol photodegradation) and to dye sensitization of the photocatalyst surface (as confirmed by photocatalytic tests carried out using different visible-emission spectra LEDs). The main reactive species involved in the dye degradation were determined to be positive holes.