In this study, the cubic antimony trioxide (Sb2O3) nanoparticles were successfully synthesized by ultrasonic-assisted solid-liquid reaction ball milling technique. And the synthetic process, using Sb powder as raw material, was conducted with an atmosphere of acetic acid aqueous solution at low temperature (<= 100 degrees C). Some controlled trials, including without the assistance of ultrasonic wave, different reaction solutions and diverse ultrasonic frequencies, were performed. The products were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that the Sb2O3 nanoparticles with uniform and ultrafine particle size were obtained within short reaction time under the coaction of both ultrasonic wave and ball milling. Furthermore, the catalytic capacity of the Sb2O3 nanoparticles for decomposition of H2O2 was measured during the oxidative decomposition of methylene blue (MB). The test exhibited rapid and efficient color removal in the degradation of MB. (C) 2017 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.