Abstract—This article describes the method for preparation of opal matrices by the sol–gel method, their drying in supercritical carbon dioxide, and the preparation of α-cristobalite with high temperature annealing. The conditions for the preparation of synthetic opal matrices and the concentration of reagents for this process are described. A supercritical operation mode of the drying of silica xerogel to produce porous matrices is proposed. The transition of SiO2 from an amorphous to a crystalline state by supercritical drying and annealing is shown. All processes were controlled by scanning electron microscopy, Raman spectroscopy, and X-ray diffraction.
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ACKNOWLEDGMENTS
Raman spectroscopic and X-ray powder diffraction studies were performed on the equipment of the Institute of Experimental Mineralogy of the Russian Academy of Sciences (Chernogolovka, Moscow Oblast, Russia). The authors thank T.N. Dokina (Institute of Experimental Mineralogy) for her help in carrying out and interpreting the X-ray powder diffraction studies. Electron microscopy was performed on the equipment of the Shared Facility Center at the Ivanovo State University of Chemistry and Technology (Ivanovo, Russia). The authors thank senior researcher Candidate V.M. Masalov (Institute of Solid State Physics, Russian Academy of Sciences, Chernogolovka, Moscow oblast, Russia) for his assistance in the synthesis of opal matrices. The authors are grateful to senior researcher Candidate O.V. Eliseeva (Krestov Institute of Solution Chemistry, Russian Academy of Sciences, Ivanovo, Russia) for carrying out the synthesis of opal matrices and fruitful discussion at all stages of the work.
Funding
The work was performed as part of a State Assignment (registration number 01201260481) and was supported by the Russian Foundation for Basic Research (grant no. 18-29-06008).
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Dyshin, A.A., Bondarenko, G.V. & Kiselev, M.G. α-Crystobalite Preparation via Supercritical Carbon Dioxide Drying of Opal Matrices Synthesized by Sol-Gel Method. Russ. J. Phys. Chem. B 13, 1182–1188 (2019). https://doi.org/10.1134/S1990793119070030
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DOI: https://doi.org/10.1134/S1990793119070030