Preparation and investigation of cerium-based nanocomposites are of scientific and practical interest due to their unique catalytic, optical, and adsorption properties. CeO2/SiO2 nanocomposite was synthesized via thermolysis of amorphized CeCl3∙7H2O on a fumed silica surface at 400–800 °С. According to XRD and TG data, the phase transition from crystalline to amorphous state during the preparation of the initial composite and a change in the thermal dehydration process of CeCl3∙7H2O on the silica surface are observed in comparison with individual cerium chloride at 100–250 °C. A cubic cerium dioxide with a crystallite size of 4 nm is formed in the silica matrix upon the thermolysis of the blend at 400 °С. With increasing temperature from 400 to 800 °С, a slight increase in the ceria crystallite size is observed. According to SEM data, the single-domain spherical-like CeO2 nanoparticles (4–11 nm) are uniformly distributed in the amorphous silica matrix in the composite synthesized at 400 °С. The size distribution of CeO2 estimated from XRD data is in agreement with HRTEM data. This study shows a pathway to control the formation of ceria nanocrystallites in the silica matrix that may be of interest from a practical point of view.
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