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. 2023 Jun 25;13(13):1928.
doi: 10.3390/nano13131928.

Novel Sol-Gel Synthesis of TiO2 Spherical Porous Nanoparticles Assemblies with Photocatalytic Activity

Carla Calabrese  1 , Amélie Maertens  2 , Alessandra Piras  2   3 , Carmela Aprile  2 , Leonarda Francesca Liotta  1
Affiliations

Novel Sol-Gel Synthesis of TiO2 Spherical Porous Nanoparticles Assemblies with Photocatalytic Activity

Carla Calabrese et al. Nanomaterials (Basel). .

Abstract

For this study, the synthesis of TiO2 nanomaterials was performed via a novel sol-gel method employing titanium butoxide as a metal precursor, Pluronic F127 as a templating agent, toluene as a swelling agent, and acidic water or ethanol as the reaction solvents. The method was designed by tailoring certain reaction parameters, such as the sequence of toluene addition, magnetic stirring, the type of reaction solvent, and the calcination conditions. Analysis of the specific surface area and porosity was carried out via N2 physisorption, whereas the morphological features of the solids were investigated via transmission electron microscopy. The crystalline structure of both the dried powders and the calcined materials was evaluated using X-ray diffraction analysis. It transpired that the different phase compositions of the solids are related to the specific synthesis medium employed. Under the adopted reaction conditions, ethanol, which was used as a reaction solvent, promoted the local arrangement of dispersed anatase particles, the specific arrangement of which does not lead to rutile transformation. Conversely, the use of water alone supported high-particle packing, evolving into a rutile phase. The photodegradation of Rhodamine B was used as a target reaction for testing the photocatalytic activity of the selected samples.

Keywords: anatase; photocatalysis; porous nanoparticles; rutile; sol-gel synthesis; titanium.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Scheme 1
Scheme 1
Sol-gel synthesis of TiO2-based materials.
Figure 1
Figure 1
Adsorption-desorption N2 isotherms of TiO2-EtOH-C1 and TiO2-H2O-C1. Inset: pore size distribution.
Figure 2
Figure 2
TEM micrographs of TiO2-H2O-C1 (top) and TiO2-EtOH-C1 (bottom).
Figure 3
Figure 3
XRD patterns of reference and calcined materials.
Figure 4
Figure 4
Adsorption-desorption N2 isotherms of TiO2-EtOH-C2, TiO2-EtOH-C3 and TiO2-H2O-C3. Inset: pore size distribution.
Figure 5
Figure 5
XRD patterns of the reference and calcined materials.
Figure 6
Figure 6
TEM micrographs of TiO2-EtOH-C3.
Figure 7
Figure 7
TEM micrographs of TiO2-H2O-C3.
Figure 8
Figure 8
XRD patterns of the reference ICSD files, with the dried and calcined materials.
Figure 9
Figure 9
N2-adsorption-desorption isotherms of TiO2-EtOH-C3, TiO2-EtOH-C3′, and TiO2-EtOH-C3″. The inset displays the pore size distribution.
Figure 10
Figure 10
Three consecutive catalytic cycles of RhB degradation, carried out for the best solid (TiO2-EtOH-C3).
See this image and copyright information in PMC

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