The present study is focused on fabrication of high-purity submicrometer alumina ceramic particles (predominantly in sub-100 nm range) from micrometer-sized feed (e.g., 70-80 μm) using sonofragmentation. The effects of various parameters such as ultrasonic frequency, feed concentration, sonication time, surfactant, and applied ultrasonic power on sonofragmentation were investigated. Sub-100 nm particle production by sonofragmentation was validated via three metrics, i.e., laser particle size analysis, high-resolution transmission electron microscopy, and turbidimetry. There is a significant change in color and shape of alumina ceramic particles as a result of sonofragmentation. Higher size reduction ratios are obtained at lower frequencies and at higher input power. Submicrometer particle generation increases as concentration of the feed particles increases, indicating that attrition by interparticle collision is a significant mechanism. The shape of the particles changes from angular to spherical as sonofragmentation time increases. Probe-type sonication produces fragmentation effects that are less uniform than those induced by tank-type ultrasonics. Surfactant plays a significant role in preventing agglomeration, especially as finer fragments are produced with prolonged sonication. © 2008 IEEE.