In the present work, we have studied for the first time the combined effect of both sonication and precipitation pH on the structure of amorphous zirconia gels synthesized from zirconium(IV) propoxide. The techniques of small-angle neutron and X-ray scattering (SANS and SAXS) and low temperature nitrogen adsorption provided the integral data on the changes in the microstructure and mesostructure of these materials caused by ultrasonic treatment.Amorphous ZrO 2 ·xH 2 O synthesized under ultrasonic treatment was found to possess a very structured surface, characterized by the surface fractal dimension 2.9-3.0, compared to 2.3-2.5 for the non US-assisted synthesis, and it was also found to possess a higher specific surface area, while the sizes of the primary particles remain unchanged.