Impact of the Precursor on the Physicochemical Properties and Photoactivity of TiO<sub>2</sub> Nanoparticles Produced in Supercritical CO<sub>2</sub>
The synthesis of TiO<sub>2</sub> nanoparticles (NPs) in supercritical media has been reported over the last two decades. However, very few studies have compared the physicochemical characteristics and photoactivity of the TiO<sub>2</sub> powders produced from different precur...
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2023-08-01
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author | Óscar Ramiro Andrade Rafael Camarillo Fabiola Martínez Carlos Jiménez Jesusa Rincón |
author_facet | Óscar Ramiro Andrade Rafael Camarillo Fabiola Martínez Carlos Jiménez Jesusa Rincón |
author_sort | Óscar Ramiro Andrade |
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description | The synthesis of TiO<sub>2</sub> nanoparticles (NPs) in supercritical media has been reported over the last two decades. However, very few studies have compared the physicochemical characteristics and photoactivity of the TiO<sub>2</sub> powders produced from different precursors, and even fewer have investigated the effect of using different ratios of hydrolytic agent/precursor (HA/P) on the properties of the semiconductor. To bridge this knowledge gap, this research focuses on the synthesis and characterization of TiO<sub>2</sub> NPs obtained in a supercritical CO<sub>2</sub> medium from four different TiO<sub>2</sub> precursors, namely diisopropoxytitanium bis (acetylacetonate) (TDB), titanium (IV) isopropoxide (TIP), titanium (IV) butoxide (TBO), and titanium (IV) 2-ethylhexyloxide (TEO). Further, the effect of various HA/P ratios (10, 20, 30, and 40 mol/mol) when using ethanol as a hydrolytic agent has also been analyzed. Results obtained have shown that the physicochemical properties of the catalysts are not significantly affected by these variables, although some differences do exist between the synthesized materials and their catalytic performances. Specifically, photocatalysts obtained from TIP and TEO at the higher HA/P ratios (HA/P = 30 and HA/P = 40) led to higher CO<sub>2</sub> photoconversions (6.3–7 µmol·g<sup>−1</sup>·h<sup>−1</sup>, Apparent Quantum Efficiency < 0.1%), about three times higher than those attained with commercial TiO<sub>2</sub> P-25. These results have been imputed to the fact that these catalysts exhibit appropriate values of crystal size, surface area, light absorption, and charge transfer properties. |
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spelling | doaj.art-2094c3f2412e4d0abfce41c3312ec9a22023-11-19T02:27:26ZengMDPI AGNanomaterials2079-49912023-08-011316232810.3390/nano13162328Impact of the Precursor on the Physicochemical Properties and Photoactivity of TiO<sub>2</sub> Nanoparticles Produced in Supercritical CO<sub>2</sub>Óscar Ramiro Andrade0Rafael Camarillo1Fabiola Martínez2Carlos Jiménez3Jesusa Rincón4Department of Chemical Engineering, Faculty of Environmental Sciences and Biochemistry, University of Castilla-La Mancha, 45071 Toledo, SpainDepartment of Chemical Engineering, Faculty of Environmental Sciences and Biochemistry, University of Castilla-La Mancha, 45071 Toledo, SpainDepartment of Chemical Engineering, Faculty of Environmental Sciences and Biochemistry, University of Castilla-La Mancha, 45071 Toledo, SpainDepartment of Chemical Engineering, Faculty of Environmental Sciences and Biochemistry, University of Castilla-La Mancha, 45071 Toledo, SpainDepartment of Chemical Engineering, Faculty of Environmental Sciences and Biochemistry, University of Castilla-La Mancha, 45071 Toledo, SpainThe synthesis of TiO<sub>2</sub> nanoparticles (NPs) in supercritical media has been reported over the last two decades. However, very few studies have compared the physicochemical characteristics and photoactivity of the TiO<sub>2</sub> powders produced from different precursors, and even fewer have investigated the effect of using different ratios of hydrolytic agent/precursor (HA/P) on the properties of the semiconductor. To bridge this knowledge gap, this research focuses on the synthesis and characterization of TiO<sub>2</sub> NPs obtained in a supercritical CO<sub>2</sub> medium from four different TiO<sub>2</sub> precursors, namely diisopropoxytitanium bis (acetylacetonate) (TDB), titanium (IV) isopropoxide (TIP), titanium (IV) butoxide (TBO), and titanium (IV) 2-ethylhexyloxide (TEO). Further, the effect of various HA/P ratios (10, 20, 30, and 40 mol/mol) when using ethanol as a hydrolytic agent has also been analyzed. Results obtained have shown that the physicochemical properties of the catalysts are not significantly affected by these variables, although some differences do exist between the synthesized materials and their catalytic performances. Specifically, photocatalysts obtained from TIP and TEO at the higher HA/P ratios (HA/P = 30 and HA/P = 40) led to higher CO<sub>2</sub> photoconversions (6.3–7 µmol·g<sup>−1</sup>·h<sup>−1</sup>, Apparent Quantum Efficiency < 0.1%), about three times higher than those attained with commercial TiO<sub>2</sub> P-25. These results have been imputed to the fact that these catalysts exhibit appropriate values of crystal size, surface area, light absorption, and charge transfer properties.https://www.mdpi.com/2079-4991/13/16/2328TiO<sub>2</sub>supercritical CO<sub>2</sub>semiconductor nanoparticles synthesisprecursorCO<sub>2</sub> photoreduction |
spellingShingle | Óscar Ramiro Andrade Rafael Camarillo Fabiola Martínez Carlos Jiménez Jesusa Rincón Impact of the Precursor on the Physicochemical Properties and Photoactivity of TiO<sub>2</sub> Nanoparticles Produced in Supercritical CO<sub>2</sub> Nanomaterials TiO<sub>2</sub> supercritical CO<sub>2</sub> semiconductor nanoparticles synthesis precursor CO<sub>2</sub> photoreduction |
title | Impact of the Precursor on the Physicochemical Properties and Photoactivity of TiO<sub>2</sub> Nanoparticles Produced in Supercritical CO<sub>2</sub> |
title_full | Impact of the Precursor on the Physicochemical Properties and Photoactivity of TiO<sub>2</sub> Nanoparticles Produced in Supercritical CO<sub>2</sub> |
title_fullStr | Impact of the Precursor on the Physicochemical Properties and Photoactivity of TiO<sub>2</sub> Nanoparticles Produced in Supercritical CO<sub>2</sub> |
title_full_unstemmed | Impact of the Precursor on the Physicochemical Properties and Photoactivity of TiO<sub>2</sub> Nanoparticles Produced in Supercritical CO<sub>2</sub> |
title_short | Impact of the Precursor on the Physicochemical Properties and Photoactivity of TiO<sub>2</sub> Nanoparticles Produced in Supercritical CO<sub>2</sub> |
title_sort | impact of the precursor on the physicochemical properties and photoactivity of tio sub 2 sub nanoparticles produced in supercritical co sub 2 sub |
topic | TiO<sub>2</sub> supercritical CO<sub>2</sub> semiconductor nanoparticles synthesis precursor CO<sub>2</sub> photoreduction |
url | https://www.mdpi.com/2079-4991/13/16/2328 |
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