Abstract: To synthesize pure γ-La₂S₃ at lower temperature, lanthanide complex La(Et₂S₂CN)₃·phen, containing La-S bond, was chosen as the precursors to decompose. The obtained samples were characterized by X-ray power diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) with an energy dispersive spectrometer and UV-Vis diffuse reflectance spectra. The decomposition mechanism of the lanthanide complex was studied by thermogravimetric analyses (TGA). The results show that the obtained samples are cubic phase particles with sizes among 20–50 nm and the band gap is 2.97 eV, which is bigger than that of its bulk crystal. TG/DTG results indicate that La(Et₂S₂CN)₃·phen decomposed to γ-La₂S₃ via La₄(Et₂S₂CN)₃ as an intermediate product.