Power ultrasound of 20 kHz was applied to the synthesis of silica spheres via the controlled hydrolysis of tetraethoxysilane (TEOS). Silica spheres of about 0.3 μm were agglomerated to form tolerably uniform, dense particles of about 2 μm through 90 min sonication. This agglomeration behavior was examined by laser diffraction particle size analysis and transmission electron microscopy. It was found that the agglomeration process involves (I) an incubation period in which no agglomeration occurs, (II) rapid formation of ramified particles, and (III) their densification. It was inferred that sonication enhances collision among silica spheres.