The xerogels in the system 0.88 mol.% ZrO2 − 0.12 mol.% CeO2 were obtained by the method of coprecipitation in a neutral (pH = 7) and slightly alkaline (pH = 9) medium under the influence of ultrasound with the size of the agglomerates 70 – 230 nm. It is shown that the coprecipitation of hydroxides of zirconium and cerium at pH = 9 with the use of ultrasonic treatment facilitates the formation of a primary crystal is symbolic of the particles in the xerogel, whose size is ~ 5 nm, whereas the xerogel synthesized in a neutral environment consists only of the x-ray amorphous phase. The effect of pH-precipitation on deposition processes of dehydration of the xerogels and crystallization solid solution based on zirconia oxide in the metastable pseudocubic modification (с′-ZrO2) was discovered. It was found that in the temperature range 500 – 800 °C there is a phase transition с′-ZrO2 → t-ZrO2, the size of the crystallites of the formed tetragonal solid solutions is 8 and 11 nm. The method of low-temperature nitrogen adsorption were investigated dispersion properties and characteristics of the pore structure of the powders of the solid solution Zr0.88Ce0.12O2. It is determined that the specific surface area of t-ZrO2 samples obtained after firing at 800 °C is 117 and 178 m2/g, the total pore volume reaches 0.300 − 0.325 cm3/g, the pore size distribution is monomodal and is in the range of 2 − 8 nm. The effect of thermal “aging” at a temperature of 800 °C (40 h) on the structure and dispersion of the solid solution t-ZrO2 powders was studied.
