Abstract: Nanocrystalline powders of ZrO₂-8mol%SmO_1.5(8SmSZ), ZrO₂-8mol%GdO_1.5 (8GdSZ), and ZrO₂-8mol%YO_1.5(8YSZ) were prepared by a simple reverse-coprecipitation technique. Differential thermal analysis/thermogravimetry (DTA/TG), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Raman spectroscopy, and high-resolution transmission electron microscopy (HRTEM) were used to study the phase transformation and crystal growth behavior. The DTA results showed that the ZrO₂ freeze-dried precipitates crystallized at 529, 465, and 467℃ in the case of 8SmSZ, 8GdSZ, and 8YSZ, respectively. The XRD and Raman results confirmed the presence of tetragonal ZrO₂ when the dried precipitates were calcined in the temperature range from 600 to 1000℃ for 2 h. The crystallite size increased with increasing calcination temperature. The activation energies were calculated as 12.39, 12.45, and 16.59 kJ/mol for 8SmSZ, 8GdSZ, and 8YSZ respectively.