Abstract: Organic ligands are widely used in the synthesis of metallic complexes, which can be burned and eliminated from the coordination sphere at high temperatures and remaining only oxide group. The reaction of Ethylenediaminetetraacetic acid (EDTA) as an organic ligand and antimony trichloride in a domestic microwave leads to formation of antimony-EDTA complex. Then, the resulting compound was calcined and got nano antimony oxide. The product was characterized by powder x-ray diffraction (XRD), fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM) and UV–vis diffuse reflectance spectrum (DRS). This technique is a simple, fast, environmental friendly and can draw a usable viewpoint for the synthesis of nanomaterials.