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Electrochemical behavior of dysprosium (Dy) ions in LiF-DyF3 (24 mol％) was investigated by cyclic voltammetry, chronoamperometry and chronopotentiometry. Dy-Cu alloy samples were prepared by constant-potential electrolysis in LiF-DyF3 (24 mol％) at the Cu electrode. The Cu5Dy and Cu phases were characterized by an X-ray diffractometer and a scanning electron microscope equipped with an energy dispersive spectrometer. The results show that the reduction of Dy(III) ions in a LiF-DyF3 (24 mol％) molten salt system is found to be a quasi-reversible diffusion-controlled process which occurs via a one-step reaction involving the transfer of three electrons. The electro-crystallization processes of the Dy metal at the W electrode and the mode of nucleation confirm that progressive nucleation is dominant at high concentrations of Dy ions in the LiF-DyF3 salt. At lower concentrations, the instantaneous nucleation of Dy with three-dimensional growth of the nuclei is dominant.