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Structural and photocatalytic properties of sol–gel-derived TiO2 samples prepared by conventional and hydrothermal methods using a low amount of water

  • Original Paper: Nano-structured materials (particles, fibers, colloids, composites, etc.)
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Abstract

Titania is a versatile semiconductor widely used in many applications, including photocatalysis. Among the processing routes used to prepare titania, the sol–gel process deserves to be highlighted because it allows obtaining samples with tailored composition, particle size, and specific surface area. Such properties play a key role in the photocatalytic behavior of titania. In this study, we show that by adjusting the sol–gel parameters and drying/heat treatment conditions it is possible to control the co-existence of anatase and rutile in the synthesized sol–gel titania. The works found in the literature usually deal with the preparation of crystalline titania using water-rich solutions, which usually gives rise to anatase. However, we demonstrate that the lack of water in the starting solution favors the formation of both anatase and rutile; the co-existence of these two phases has been reported to improve the photocatalytic behavior of titania due to a band-gap alignment. Furthermore, we propose a sol–gel route based on a single-step hydrothermal procedure where nanoparticles with sizes of about 3 nm and surface areas up to 120 m2.g−1 are obtained. This study accounts for the knowledge regarding the preparation and use of sol–gel titania for photocatalysis applications. It is supported by a series of experimental techniques, including X-ray diffraction, N2 sorption, thermogravimetry, differential thermal analysis, Raman spectroscopy, transmission electron microscopy, selected area electron diffraction, and UV–Vis diffuse reflectance spectroscopy. The photoactivity of the prepared samples was evaluated in terms of the photodegradation of methylene blue under near-ultraviolet (UV-A) light.

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Highlights

  • Titania nanoparticles obtained from a sol–gel route based on a water-deficient starting solution.

  • Crystalline samples prepared by either heat-treatment or hydrothermal treatment.

  • The lack of water allows the preparation of anatase-rutile mixed titania.

  • Nanoparticles with sizes as small as 3 nm and specific surface areas up to 120 m2.g−1.

  • Photoactivty evaluated in terms of the degradation of methylene blue under UV-A light.

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Acknowledgements

EHMN is grateful for the financial support from CAPES (PROEX), FAPEMIG (RED-00102-16, RENOVAMIN), and CNPq (304415/2021-9). The authors thank the technical support from Taiane Guedes/INCT Acqua (Raman spectroscopy) and the UFMG microscopy center (TEM). CeNano2I/CEMUCASI (Prof. Herman Mansur and Dr. Alexandra Mansur) are also recognized for their technical support to this research (TG/DTA).

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Authors and Affiliations

  1. Departamento de Engenharia de Materiais, Centro Federal de Educação Tecnológica de Minas Gerais, Nova Suíça, Belo Horizonte, MG, CEP 30421-169, Brasil

    Maira Marra & Marcello Dumont

  2. Departamento de Engenharia Metalúrgica e de Materiais, Universidade Federal de Minas Gerais, Pampulha, Belo Horizonte, MG, CEP 31270-901, Brasil

    Hugo G. Palhares, Himad A. Alcamand & Eduardo H. M. Nunes

  3. Departamento de Engenharia Química, Universidade Federal de Minas Gerais, Pampulha, Belo Horizonte, MG, CEP 31270-901, Brasil

    Manuel Houmard

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  1. Maira Marra
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Marra, M., Dumont, M., Palhares, H.G. et al. Structural and photocatalytic properties of sol–gel-derived TiO2 samples prepared by conventional and hydrothermal methods using a low amount of water. J Sol-Gel Sci Technol 103, 97–107 (2022). https://doi.org/10.1007/s10971-022-05780-6

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