The electrochemical behavior of UO 2 F 2 in LiF-NaF-KF (46.5-11.5-42 mol%, FLiNaK) melt on Pt electrode was investigated at 550 • C by cyclic voltammetry (CV) and square wave voltammetry (SWV). UO 2 F 2 was prepared by the reaction of UF 4 powder and oxygen at 650 • C, and ascertained by X-ray diffraction (XRD) and Raman spectroscopy. It was found that the reduction of UO 2 2+ in FLiNaK exhibited two steps both with one exchanged electron: UO 2 2+ + e − → UO 2 + and UO 2 + + e − → UO 2 , with the CV reduction peak at about 2.02 V and 1.49 V (vs. K + /K), respectively. Both of them were reversible and diffusion-controlled. By means of potentiostatic electrolysis, the product of UO 2 was obtained and the separation ratio of uranium from UO 2 F 2 -FLiNaK melt was approximately 54.5% at 550 • C, which were characterized by XRD and the inductively coupled plasma atomic emission spectrometer (ICP-AES).