Colloids of the coordinated terbium oxide are prepared by colloids precipitation method with ligands of acetylacetone (acac) and 2,2-bipyridine and pH regulating agent of NaOH solution. The fluorescent properties and structure of nanoparticles of the coordinated terbium oxide are characterized by fluorescence spectra, ultraviolet-visible spectra and high-resolution transmission electron microscopy (HRTEM). The results show that the nano terbium oxide particles coordinated by acac and 2,2′-bipy can radiate intense green light under ultraviolet irradiation, and their fluorescence spectrum presents typical characteristic emission peaks of Tb3+ ions. The HRTEM and selected area electron diffraction (SED) results show that the nanoparticles are terbium oxide with the size of 6 nm.