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A detailed study of the mesoporous structure formation in the silica monolith with interconnected macropores

  • Original Paper: Nano- and macroporous materials (aerogels, xerogels, cryogels, etc.)
  • Published:
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Abstract

In this work, the phenomena occurring at the stage of solvent exchange treatment during the synthesis of porous silica monoliths are described using high-resolution scanning microscopy. Initially, the solution in the swollen gel network and macropores contains the tetraethoxysilane hydrolysis products, the structure-forming agent polyethylene oxide, and nitric acid. Solvent exchange treatment with a more basic solvent leads to the leaching of polyethylene oxide and promotes the polycondensation process. This results in the increase in crosslinking density, the decrease in the elasticity, and the swelling degree of the gel. The release of excess solvent in the dense gel leads to its fragmentation. The formed non-spherical fragments under basic conditions are immediately crosslinked within the skeleton of macropores. Therefore, the porous monolith macrostructure and the integrity of the block are preserved. This process is rather rapid. With further treatment, there is a slow dissolution and reprecipitation of silica from the particle surface resulting in their decrease and in an increase in the size and volume of mesopores formed between them.

Graphical Abstract

Mesoporous structure formation.

Highlights

  • Formation of mesopores occurs due to skeleton fragmentation and crosslinking of fragments

  • Fragmentation occurs with an increase in crosslink density in a gel that is not able to relax

  • Fragments are rapidly connected by siloxane bonds which preserves the integrity of the sample

  • During drying and heat treatment, a crust is formed on the surface of macropores.

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Acknowledgements

This work was carried out within the framework of the state assignment of the Ministry of Science and Higher Education of the Russian Federation (FSWM-2020-0037). The authors thank Dr. Mikhail Salaev (Tomsk State University) for language review.

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Author notes

  1. These authors contributed equally: A. N. Serkova, A. N. Salanov, T. I. Izaak

Authors and Affiliations

  1. Tomsk State University, 36 Lenin Ave., Tomsk, 634050, Russia

    O. Yu. Miskevich & T. I. Izaak

  2. Boreskov Institute of Catalysis SB RAS, 5 Lavrentiev Ave., Novosibirsk, 630090, Russia

    A. N. Serkova & A. N. Salanov

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  1. O. Yu. Miskevich
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Miskevich, O.Y., Serkova, A.N., Salanov, A.N. et al. A detailed study of the mesoporous structure formation in the silica monolith with interconnected macropores. J Sol-Gel Sci Technol 105, 748–757 (2023). https://doi.org/10.1007/s10971-023-06051-8

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  • DOI: https://doi.org/10.1007/s10971-023-06051-8

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