This article is devoted to the study of the processes of formation and growth of nanocrystals with the pyrochlore structure in the TiO2-Gd2O3 system. A mixture of an aqueous solution of gadolinium nitrate and a solution of titanium isopropoxide with polyethylene glycol in isopropyl alcohol was evaporated to a gel state, and then it was heat-treated using a one- or two-stage scheme. The study showed that the material being formed has a trabecular structure with a developed system of macropores. The use of the two-stage roasting method allows a uniform distribution of titanium and gadolinium atoms in the sample. Gadolinium titanate with a pyrochlore structure, which is formed using an aggregation mechanism at a temperature T = 700 °C from an X-ray amorphous precursor, is a variable composition compound. It has been shown that in terms of obtaining a monophasic product, the possibility of varying the size of nanocrystals, and defects in the pyrochlore structure, the most promising heat treatment mode is synthesis in the temperature range of 750–900 °C. In this case, the possibility of controlling the above characteristics of Gd2Ti2O7 nanoparticles can be implemented by varying the ratio of titanium- and gadolinium-containing precursors in the initial mixture, the duration of the isothermal exposure process.
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