Nanocrystalline powders of ZrO2–8mol%SmO1.5 (8SmSZ), ZrO2–8mol%GdO1.5 (8GdSZ), and ZrO2–8mol%YO1.5 (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°C 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°C 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.