A simple and rapid microwave-assisted wet chemical route was developed for the preparation of Sb 2 Te 3 hexagonal single-crystalline nanoplates with edge length of hundreds of nanometers. The products were characterized with X-ray powder diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), and selected area electron diffraction (SAED) techniques. The reaction mechanism was proposed and the effects of alkali, solvents, and stimulating factors such as ultrasonic wave and solvothermal process were studied. The effects of some additives were also discussed, and PVP (polyvinyl pyrrolidone) was found to be able to regularize and diminish the nanoplates.