Uniform hollow antimony micron spheres were synthesized on a large scale using SbCl3 and dithizone as starting reagents in ethylenediamine at 140degreesC for 72 h. XRD and Raman results reveal that the as-obtained final product is pure Sb. FE-SEM and TEM observation reveals that the prepared hollow microspheres are composed of nanoparticles. The possible formation mechanism was briefly discussed.