Preparation of iron oxide ( -Fe 2 O 3 ) nanoparticles was carried out via a sonochemical process. The process parameters such as temperature, sonication time and power of ultrasonication play important roles in the size and morphology of the final products. The iron oxide nanoparticles were characterized by transmission electron microscopy, X-ray powder diffraction, and thermogravimetric and differential thermal analyses. From transmission electron microscopy observations, the size of the iron oxide nanoparticles is estimated to be significantly smaller than 19 nm. X-ray diffraction data of the powder after annealing provide direct evidence that the iron oxide was formed during the sonochemical process. Preparation of iron oxide (-Fe 2 O 3) nanoparticles was carried out via a sonochemical process. The process parameters such as temperature, sonication time and power of ultrasonication play important roles in the size and morphology of the final products. The iron oxide nanoparticles were characterized by transmission electron microscopy, X-ray powder diffraction, and thermogravimetric and differential thermal analyzes. From transmission electron microscopy observations, the size of the iron oxide nanoparticles is estimated to be significantly smaller than 19 nm. X-ray diffraction data of the powder after annealing provide direct evidence that the iron oxide was formed during the sonochemical process.