The cathodic reduction reaction of Dy(III) ions on inert molybdenum electrode in fused 3LiCl–2KCl eutectic in the temperature range 723–843 K in inert atmosphere was studied by electrochemical methods. On cyclic voltammogram in the investigated “electrochemical window”, one cathode current peak at potential of –3.19 ± 0.11 V and the corresponding anode current peak at potential of –2.95 ± 0.11 V vs. the reference chlorine electrode were fixed. Therefore, the recovery process proceeds by the reaction Dy3+ + 3ē → Dy. Analyzing of cyclic voltammograms showed that the potential of the current peak shifts to the negative region with increasing of scan rate, and the current of the cathode peak is directly proportional to the square root of the polarization rate. It was found that the increasing of scan rate led to a natural increase of the irreversibility of the cathode process. The number of electrons (n) of the electrode reaction for reduction Dy(III) ions was determined by the square-wave voltammetry method. The calculated value is equal to n = 2.93 ± 0.05. According to the theory of cyclic voltammetry, the cathode recovery process proceeds irreversibly, in one stage, and is controlled by the charge transfer rate. The dependence of the apparent standard potential of the Dy(III)/Dy couple vs. the temperature was determined by the chronopotentiometry method at zero current. Experimental values are described by the linear equation: \[E_{{{{{\text{Dy}}\left( {{\text{III}}} \right)} \mathord{\left/ {\vphantom {{{\text{Dy}}\left( {{\text{III}}} \right)} {{\text{Dy}}}}} \right. \kern-\delimiterspace} {{\text{Dy}}}}}}^{{\text{*}}} = - \left( {{\text{3}}{\text{.401}} \pm {\text{0}}{\text{.009}}} \right) + \left( {{\text{6}}{\text{.2}} \pm {\text{0}}{\text{.1}}} \right) \cdot {\text{1}}{{{\text{0}}}^{{ - 4}}} \cdot T \pm {\text{0}}{\text{.007}}\,\,{\text{V}}\. The apparent standard Gibbs energy change, enthalpy, and entropy of the dysprosium trichloride formation reaction from its elements in fused 3LiCl–2KCl eutectic and the activity coefficient of DyCl3 were calculated.