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Nanocrystalline (RE2O3)x(SnO2)1−x (x = 0.02–0.15, RE = La, Sm, Gd, Ho, Yb, Y) powders were synthesized by a two-step hydrothermal process in the presence of urea, followed by the calcination between 400 and 1000 °C. The average crystallite size of the as-calcined samples decreased with the increase of dopant content, suggesting that doping an appropriate amount of RE into nanosized SnO2 could effectively inhibit the grain growth. Structure characterization revealed that (RE2O3)x(SnO2)1−x, except (Yb2O3)x(SnO2)1−x, appeared tetragonal SnO2 at low temperature, and segregated cubic RE2O3 upon calcination, and transformed into cubic RE2Sn2O7 over 800–1000 °C. The amount of the RE2Sn2O7 increased with the increase of RE dopant content. For (Yb2O3)x(SnO2)1−x (x = 0.02–0.15), only cassiterite SnO2 was observed at the high calcination temperature of 1000 °C, and the lattice parameter refinement revealed that both lattice parameter and lattice volume decreased linearly with the increase of Yb2O3 content.
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