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...

Full description

Bibliographic Details
Main Authors: Óscar Ramiro Andrade, Rafael Camarillo, Fabiola Martínez, Carlos Jiménez, Jesusa Rincón
Format: Article
Language:English
Published: MDPI AG 2023-08-01
Series:Nanomaterials
Subjects:
Online Access:https://www.mdpi.com/2079-4991/13/16/2328
_version_ 1797583607047389184
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
collection DOAJ
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.
first_indexed 2024-03-10T23:41:12Z
format Article
id doaj.art-2094c3f2412e4d0abfce41c3312ec9a2
institution Directory Open Access Journal
issn 2079-4991
language English
last_indexed 2024-03-10T23:41:12Z
publishDate 2023-08-01
publisher MDPI AG
record_format Article
series Nanomaterials
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
work_keys_str_mv AT oscarramiroandrade impactoftheprecursoronthephysicochemicalpropertiesandphotoactivityoftiosub2subnanoparticlesproducedinsupercriticalcosub2sub
AT rafaelcamarillo impactoftheprecursoronthephysicochemicalpropertiesandphotoactivityoftiosub2subnanoparticlesproducedinsupercriticalcosub2sub
AT fabiolamartinez impactoftheprecursoronthephysicochemicalpropertiesandphotoactivityoftiosub2subnanoparticlesproducedinsupercriticalcosub2sub
AT carlosjimenez impactoftheprecursoronthephysicochemicalpropertiesandphotoactivityoftiosub2subnanoparticlesproducedinsupercriticalcosub2sub
AT jesusarincon impactoftheprecursoronthephysicochemicalpropertiesandphotoactivityoftiosub2subnanoparticlesproducedinsupercriticalcosub2sub