Two-dimensional （2D） metal halides have attracted increasing research attention in recent years. Antimony triiodide （SbI₃） is used in radiation detectors and optoelectronic devices due to its optical anisotropy， high refractive index， and second harmonic generation. However， the high price of SbI₃ limits its large-scale application. In this paper， SbI₃ was synthesized by the sonochemical method using antimony powder and iodine powder as raw materials for the first time. The effects of ultrasound time， solvent， Sb content， and antimony-iodine ratio were studied and finally SbI₃ crystals and films were prepared successfully from the synthesized powder. The results show that the SbI₃ powder with pure phase is obtained using methanol as the solvent， with a Sb to I₂ molar ratio of 2∶3.6 （a 20% molar excess of iodine） and the ultrasonic time of 100 min. A highly oriented SbI₃ crystal along the （006） plane is obtained by the sublimation method at 220 ℃ for 3 h. When preparing SbI₃ film by vapor transport deposition method， the deposition distance has a great influence on the morphology of the film. Increasing the deposition distance improves the density of the film， but the crystallization degree of the film decreases due to the decrease in temperature. Therefore， it is necessary to choose an appropriate deposition distance. Here， a dense and uniform SbI₃ film can be obtained at a deposition distance of 17.5 cm. The method of sonochemical synthesis of SbI₃ is simple， efficient， low cost， reproducible， and can be extended to the synthesis of other metal iodides such as AgI， CuI， BiI₃， Cs₃Bi₂I₉ and so on.