The electrochemical reduction and nucleation process of Si 4+ on an electrical steel electrode in the eutectic LiF-NaF-KF molten salt were investigated at 750°C, by means of cyclic voltammetry and chronoamperometry technique. Silicon was electrodeposited on steel, and Fe 3 Si was formed by the diffusivity of silicon on the electrode surface. The electrochemical reduction of Si 4+ process in single-step charge transfer and the cathode process was reversible. The electrocrystallization process of silicon is controlled by progressive three-dimensional mechanism. The diffusion coefficient was calculated to be 5.42×10 −7 cm 2 /s by chronopotentiometry at experimental conditions.

The electrochemical behavior of silicon was investigated in a molten salts system including saturation silicon dioxide. Silicon was electrodeposited and MoSi 2 was formed on the employed molybdenum working electrode by the diffusivities of silicon and the substrate metals. Transient electrochemical techniques such as cyclic voltammetry and chronoamperometry were used to study the reaction mechanism at the molybdenum electrode. Cyclic voltammograms showed the possibility of electrodeposition of Si at À0.64 V versus Pt reference electrode in a NaCl-KClNaF-SiO 2 system at 1073 K (800°C). The electrodeposition of Si is single-step charge-transfer process and the cathode process is irreversible. Chronoamperometry studies indicated that electrocrystallization of Si is controlled by progressive nucleation with a three-dimensional growth mechanism.

With the continuous development of society, the number of spent lithium-ion batteries has also increased, and the recovery of valuable metals such as Ni, Co, and Li has become the main research direction of many scholars. In this paper, the extraction process of lithium that enters the molten salt after LiCoO2 electrolysis is studied. Oxalic acid and phosphate are added to molten salt containing lithium ions to realize the two-part precipitation method to extract lithium. The influence of pH value, temperature, reaction time, and oxalic acid (or phosphate) addition on the process of oxalic acid calcium removal and phosphate lithium precipitation is analyzed. The results show that the calcium removal rate of oxalic acid has reached 99.72% (Initial conditions: PH = 7.0, T = 70 °C, t = 1.5 h, n(H2C2O4):n(Ca2+) = 1.2:1). The precipitation of Li3PO4 obtained in the phosphate extraction experiment of lithium is as high as 88.44% (Initial conditions: PH = 8.0, T = 70 °C, t = 1.5 h, n(actual dosage of Na3PO4):n(theoretical dosage of Na3PO4) = 1.2:1). The obtained lithium phosphate crystals show regular spherical particles, which can be seen by SEM.

The electrochemical reduction mechanism of Mn in LiMn2O4 in molten salt was studied. The results show that in the NaCl-CaCl2 molten salt, the process of reducing from Mn (IV) to manganese is: Mn (IV)→Mn (III)→Mn (II)→Mn. LiMn2O4 reacts with molten salt to form CaMn2O4 after being placed in molten salt for 1 h. The reaction of reducing CaMn2O4 to Mn is divided into two steps: Mn (III)→Mn (II)→Mn. The results of constant voltage deoxidation experiments under different conditions show that the intermediate products of LiMn2O4 reduction to Mn are CaMn2O4, MnO, and (MnO)x(CaO)(1−x). As the reaction progresses, x gradually decreases, and finally the Mn element is completely reduced under the conditions of 3 V for 9 h. The CaO in the product can be removed by washing the sample with deionized water at 0 °C.

With the widespread use of lithium-ion batteries, the cumulative amount of used lithium-ion batteries is also increasing year by year. Since waste lithium-ion batteries contain a large amount of valuable metals, the recovery of valuable metals has become one of the current research hotspots. The research uses electrometallurgical technology, and the main methods used are cyclic voltammetry, square wave voltammetry, chronoamperometry and open circuit potential. The electrochemical reduction behavior of Ni3+ in NaCl-CaCl2 molten salt was studied, and the electrochemical reduction behavior was further verified by using a Mo cavity electrode. It is determined that the reduction process of Ni3+ in LiNiO2 is mainly divided into two steps: LiNiO2 → NiO → Ni. Through the analysis of electrolysis products under different conditions, when the current value of LiNiO2 is not less than 0.03 A, the electrolysis product after 10 h is metallic Ni. When the current reaches 0.07 A, the current efficiency is 77.9%, while the Li+ in LiNiO2 is enriched in NaCl-CaCl2 molten salt. The method realizes the separation and extraction of the valuable metal Ni in the waste lithium-ion battery.