Undoped and Fe-Doped Anatase/Brookite TiO<sub>2</sub> Mixed Phases, Obtained by a Simple Template-Free Synthesis Method: Physico-Chemical Characterization and Photocatalytic Activity towards Simazine Degradation

For the first time, Fe-doping (0.05, 1.0, and 2.5 wt.% Fe) was performed on a high-surface-area anatase/brookite TiO<sub>2</sub> by adopting a simple template-free sol-gel synthesis followed by calcination at a mild temperature. The powders’ textural and surface properties were character...

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Main Authors: Stefano Gervasi, Nicola Blangetti, Francesca S. Freyria, Salvatore Guastella, Barbara Bonelli
Format: Article
Language:English
Published: MDPI AG 2023-03-01
Series:Catalysts
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Online Access:https://www.mdpi.com/2073-4344/13/4/667
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author Stefano Gervasi
Nicola Blangetti
Francesca S. Freyria
Salvatore Guastella
Barbara Bonelli
author_facet Stefano Gervasi
Nicola Blangetti
Francesca S. Freyria
Salvatore Guastella
Barbara Bonelli
author_sort Stefano Gervasi
collection DOAJ
description For the first time, Fe-doping (0.05, 1.0, and 2.5 wt.% Fe) was performed on a high-surface-area anatase/brookite TiO<sub>2</sub> 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 TiO<sub>2</sub> (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 Fe<sup>3+</sup> ions occupying interstitial positions, and retarded the crystallite growth. N<sub>2</sub> sorption at −196 °C showed the occurrence of samples with disordered interparticle mesopores, with an increase in the specific surface area from 236 m<sup>2</sup> g<sup>−1</sup> (undoped TiO<sub>2</sub>) to 263 m<sup>2</sup> g<sup>−1</sup> (2.5 wt.% Fe). Diffuse Reflectance UV-Vis spectroscopy showed a progressive decrease in the bandgap energy from 3.10 eV (undoped TiO<sub>2</sub>) 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 TiO<sub>2</sub> 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.
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spelling doaj.art-55932380c6884bb7bc5ca81a3d62a33b2023-11-17T18:40:53ZengMDPI AGCatalysts2073-43442023-03-0113466710.3390/catal13040667Undoped and Fe-Doped Anatase/Brookite TiO<sub>2</sub> Mixed Phases, Obtained by a Simple Template-Free Synthesis Method: Physico-Chemical Characterization and Photocatalytic Activity towards Simazine DegradationStefano Gervasi0Nicola Blangetti1Francesca S. Freyria2Salvatore Guastella3Barbara Bonelli4Department of Applied Science and Technology and INSTM Unit of Torino-Politecnico, Corso Duca degli Abruzzi 24, I-10129 Torino, ItalyDepartment of Applied Science and Technology and INSTM Unit of Torino-Politecnico, Corso Duca degli Abruzzi 24, I-10129 Torino, ItalyDepartment of Applied Science and Technology and INSTM Unit of Torino-Politecnico, Corso Duca degli Abruzzi 24, I-10129 Torino, ItalyDepartment of Applied Science and Technology and INSTM Unit of Torino-Politecnico, Corso Duca degli Abruzzi 24, I-10129 Torino, ItalyDepartment of Applied Science and Technology and INSTM Unit of Torino-Politecnico, Corso Duca degli Abruzzi 24, I-10129 Torino, ItalyFor the first time, Fe-doping (0.05, 1.0, and 2.5 wt.% Fe) was performed on a high-surface-area anatase/brookite TiO<sub>2</sub> 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 TiO<sub>2</sub> (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 Fe<sup>3+</sup> ions occupying interstitial positions, and retarded the crystallite growth. N<sub>2</sub> sorption at −196 °C showed the occurrence of samples with disordered interparticle mesopores, with an increase in the specific surface area from 236 m<sup>2</sup> g<sup>−1</sup> (undoped TiO<sub>2</sub>) to 263 m<sup>2</sup> g<sup>−1</sup> (2.5 wt.% Fe). Diffuse Reflectance UV-Vis spectroscopy showed a progressive decrease in the bandgap energy from 3.10 eV (undoped TiO<sub>2</sub>) 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 TiO<sub>2</sub> 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.https://www.mdpi.com/2073-4344/13/4/667TiO<sub>2</sub> polymorphsanatase/brookite heterojunctionsFe-doped TiO<sub>2</sub>simazine degradationdetoxification
spellingShingle Stefano Gervasi
Nicola Blangetti
Francesca S. Freyria
Salvatore Guastella
Barbara Bonelli
Undoped and Fe-Doped Anatase/Brookite TiO<sub>2</sub> Mixed Phases, Obtained by a Simple Template-Free Synthesis Method: Physico-Chemical Characterization and Photocatalytic Activity towards Simazine Degradation
Catalysts
TiO<sub>2</sub> polymorphs
anatase/brookite heterojunctions
Fe-doped TiO<sub>2</sub>
simazine degradation
detoxification
title Undoped and Fe-Doped Anatase/Brookite TiO<sub>2</sub> Mixed Phases, Obtained by a Simple Template-Free Synthesis Method: Physico-Chemical Characterization and Photocatalytic Activity towards Simazine Degradation
title_full Undoped and Fe-Doped Anatase/Brookite TiO<sub>2</sub> Mixed Phases, Obtained by a Simple Template-Free Synthesis Method: Physico-Chemical Characterization and Photocatalytic Activity towards Simazine Degradation
title_fullStr Undoped and Fe-Doped Anatase/Brookite TiO<sub>2</sub> Mixed Phases, Obtained by a Simple Template-Free Synthesis Method: Physico-Chemical Characterization and Photocatalytic Activity towards Simazine Degradation
title_full_unstemmed Undoped and Fe-Doped Anatase/Brookite TiO<sub>2</sub> Mixed Phases, Obtained by a Simple Template-Free Synthesis Method: Physico-Chemical Characterization and Photocatalytic Activity towards Simazine Degradation
title_short Undoped and Fe-Doped Anatase/Brookite TiO<sub>2</sub> Mixed Phases, Obtained by a Simple Template-Free Synthesis Method: Physico-Chemical Characterization and Photocatalytic Activity towards Simazine Degradation
title_sort undoped and fe doped anatase brookite tio sub 2 sub mixed phases obtained by a simple template free synthesis method physico chemical characterization and photocatalytic activity towards simazine degradation
topic TiO<sub>2</sub> polymorphs
anatase/brookite heterojunctions
Fe-doped TiO<sub>2</sub>
simazine degradation
detoxification
url https://www.mdpi.com/2073-4344/13/4/667
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