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In this work, 3D-structured clay filters were prepared and coated with iron-doped titanium dioxide (Fe-TiO2) using 3D printing and sol–gel soaking and calcination techniques. Three-dimensional printing was employed to mold and shape the clay filters before annealing. The coated and uncoated filters were characterized for different properties, i.e., morphology, optical properties, and crystalline structure, using field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDS), UV/Vis diffused reflectance spectroscopy (DRS), and X-ray diffraction (XRD). The FESEM images show uniform coatings of round-shaped Fe-TiO2 on the tiny pore of the clay filter. The optical energy band gap of the obtained coating was around 2.8 eV, estimated by Tauc's plot, compared with 3.2 eV of pristine anatase TiO2. The XRD spectra data processed through XRD software revealed the coatings of TiO2 on the filter surface with the obtained phase of anatase. The photocatalytic performance of bare and coated filters was initially tested for the degradation of indigo carmine (IC) dye and the obtained results suggested the photocatalytic degradation of IC dye by the Fe-TiO2 clay filter compared with the bare filter. Afterward, the denitrification of nitrate NO3 at various concentrations was performed using Fe-TiO2-coated clay filters and analyzing the total nitrogen (TN) analysis and reduction of NO3 to nitrite (NO2−), nitrogen monoxide (NO), and nitrogen gas (N2). The TN analysis revealed up to 81% denitrification efficiency of the 30 ppm NO3 solution with the photocatalytic response of the Fe-TiO2-coated filter. The results revealed that the Fe-TiO2-coated clay filter has a high potential for denitrification applications under natural sunlight. [ABSTRACT FROM AUTHOR]

For the first time, Fe-doping (0.05, 1.0, and 2.5 wt.% Fe) was performed on a high-surface-area anatase/brookite TiO2 by adopting a simple template-free sol-gel synthesis followed by calcination at a mild temperature. The powders' textural and surface properties were characterized by following a multi-technique approach. XRD analysis showed that the anatase/brookite ratio slightly varied in the Fe-doped TiO2 (from 76.9/23.1 to 79.3/22.7); Fe doping noticeably affected the cell volume of the brookite phase, which decreased, likely due to Fe3+ ions occupying interstitial positions, and retarded the crystallite growth. N2 sorption at −196 °C showed the occurrence of samples with disordered interparticle mesopores, with an increase in the specific surface area from 236 m2 g−1 (undoped TiO2) to 263 m2 g−1 (2.5 wt.% Fe). Diffuse Reflectance UV-Vis spectroscopy showed a progressive decrease in the bandgap energy from 3.10 eV (undoped TiO2) to 2.85 eV (2.5 wt.% Fe). XPS analysis showed the presence of some surface Fe species only at 2.5 wt.% Fe, and accordingly, the ζ-potential measurements showed small changes in the pH at the isoelectric point. The photocatalytic degradation of simazine (a persistent water contaminant) both under UV and simulated solar light was performed as a probe reaction. Under UV light, Fe-doping improved simazine degradation in the sample at 0.05 wt.% Fe, capable of degrading ca. 77% simazine. Interestingly, the undoped TiO2 was also active both under UV and 1 SUN. This is likely due to the occurrence of anatase/brookite heterojunctions, which help stabilize the photogenerated electrons/holes. [ABSTRACT FROM AUTHOR]

The photocatalytic degradation of the emerging contaminant paracetamol in aqueous solution has been studied under 1 SUN (~1000 W m−2) in the presence of four commercial TiO2 powders, namely sub-micrometric anatase and rutile, and nanometric brookite and P25 (the popular anatase/rutile mixture used as a benchmark in most papers). The rutile powder showed low activity, whereas, interestingly, the anatase and the brookite powders outperformed P25 in terms of total paracetamol conversion to carboxylic acids, which, according to the literature, are the final products of its degradation. To explain such results, the physicochemical properties of the powders were studied by applying a multi-technique approach. Among the physicochemical properties usually affecting the photocatalytic performance of TiO2, the presence of some surface impurities likely deriving from K3PO4 (used as crystallization agent) was found to significantly affect the percentage of paracetamol degradation obtained with the sub-micrometric anatase powder. To confirm the role of phosphate, a sample of anatase, obtained by a lab synthesis procedure and having a "clean" surface, was used as a control, though characterized by nanometric particles and higher surface area. The sample was less active than the commercial anatase, but it was more active after impregnation with K3PO4. Conversely, the presence of Cl at the surface of the rutile did not sizably affect the (overall poor) photocatalytic activity of the powder. The remarkable photocatalytic activity of the brookite nanometric powder was ascribed to a combination of several physicochemical properties, including its band structure and nanoparticles size. [ABSTRACT FROM AUTHOR]

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. [ABSTRACT FROM AUTHOR]

The reaction of carboxylic groups in an ordered SBA-15, incorporated via co-condensation is studied by infrared spectroscopy. It is observed that they react reversibly with ammonia at room temperature, with the formation of carboxylate species and ammonium ions and so it is concluded that it is isolated and non interacting with each other.