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In situ infrared spectroscopic ellipsometry as a tool to probe the formation of sol–gel based mesoporous films

  • Invited Paper: Characterization methods of sol-gel and hybrid materials
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Abstract

Probing the formation of sol–gel mesoporous films and characterizing them under environmental/in-operando conditions represents an important challenge to optimize their performances. Obtaining a complete picture of the system usually requires a combination of multiple techniques. In this work, we introduce in situ infrared (IR) ellipsometry equipped with an environmental chamber as a tool to follow simultaneously the evolution of structural, optical and chemical properties during the formation of sol–gel derived mesoporous films. As a case study, we investigate the formation of mesoporous TiO2 by comparing a conventional thermal treatment and a low-temperature annealing by UV irradiation. In both cases, the structural optical and chemical evolution could be monitored during the IR ellipsometric experiment. Interestingly, UV-annealing allows the fabrication of mesoporous TiO2 films at low temperatures enabling the formation of plasmonic mesoporous composites. At last, we critically discuss the advantages and drawbacks of IR ellipsometry for in situ investigations compared to conventional UV–visible ellipsometry by providing additional insights for future developments.

Graphical Abstract

Using Infrared ellipsometry to probe the structural, optical and chemical evolution during the formation of sol–gel derived mesoporous films.

Highlights

  • IR ellipsometry is used to characterize the formation of TiO2 based mesoporous films.

  • Structural, optical and chemical evolutions can be investigated during thermal or UV treatments.

  • UV-annealing is well suited to fabricate composite plasmonic mesoporous films.

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Acknowledgements

We thank D. Montero and the Institut des Matériaux de Paris Centre (IMPC FR2482) for servicing FEGSEM & EDX instrumentation and Sorbonne Université, CNRS and C’Nano projects of the Région Ile-de-France for funding.

Funding

This work was supported by the European Research Council (ERC) under European Union’s Horizon 2020 Programme (Grant Agreement no. 803220, TEMPORE). This project has also received funding from the EU-H2020 research and innovation programme under grant agreement No. 654360 having benefitted from the access provided by ELETTRA Trieste, Italy, within the framework of the NFFA-Europe Transnational Access Activity. The infrared ellipsometry was funded by the Région Ile-de-France in the framework of DIM ResPore and by the French state within the Investissements d’Avenir programme under reference ANR-11-IDEX-0004-02, within the framework of the Cluster of Excellence MATISSE.

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Authors and Affiliations

  1. Sorbonne Université, CNRS, Laboratoire Chimie de la Matière Condensée de Paris (LCMCP), F-75005, Paris, France

    Hajar Amyar, Caroline Byun, Cédric Boissiere & Marco Faustini

  2. Université Paris-Saclay, Institut d’Optique Graduate School, CNRS, Laboratoire Charles Fabry, 91127, Palaiseau, France

    Hajar Amyar & Mondher Besbes

  3. Centre de Nanosciences et de Nanotechnologies (C2N), CNRS UMR 9001, Université Paris-Saclay, Palaiseau, France

    Andrea Cattoni

  4. Institute of Inorganic Chemistry, Graz University of Technology, Graz, Austria

    Heinz Amenitsch

  5. Institut Universitaire de France (IUF), 75231, Paris, France

    Marco Faustini

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  1. Hajar Amyar
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  2. Caroline Byun
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Amyar, H., Byun, C., Besbes, M. et al. In situ infrared spectroscopic ellipsometry as a tool to probe the formation of sol–gel based mesoporous films. J Sol-Gel Sci Technol (2023). https://doi.org/10.1007/s10971-023-06169-9

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