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Lanthanides possess extremely similar properties because their radius only changes slightly due to lanthanide contraction.

High temperature processing is an important method for recovering long‐lived elements from spent nuclear fuel. Electrolysis is the key technology for high temperature processing. The electrochemical behaviors of Sn2+, Nd3+ and the mechanisms of Sn‐Nd alloy formation were investigated on a Mo electrode at 873 K by conducting a series of electrochemical techniques. The results showed the deposition of Nd on inert electrode is a two‐step process in LiCl‐KCl‐SnCl2 (2.0 wt.%) melt system. Subsequently, the electrochemical extraction of Nd from molten chlorides were carried out on the Mo electrode at temperature of 873 K by the potentiostatic electrolysis at −1.2 V for 40 hr. Besides, the extraction efficiency is 97.6%. A series of potentiostatic electrolysis were carried out at potential range between −1.0 and − 1.4 V. The NdSn3 alloy was obtained by electrolysis at −1.2 V. This deposition potential is consistent with the predicted results of the mathematical model. The micro‐chemical analysis and morphology analysis of the deposits was characterized by energy dispersive spectrometry (EDS) with scanning electron microscopy (SEM) equipped. The composition of the deposits was analyzed by X‐ray diffraction (XRD) and inductive coupled plasma atomic emission spectrometer (ICP‐AES).