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Materials 2022, 15, 3956 5 of 11 Figure 4. XRD patterns of the products at different electro-deoxidation times. Figure 5. SEM images and EDX analysis of the products electrolysis for (a,b) 8 h and (c,d) 24 h. Figure 5. SEM images and EDX analysis of the products electrolysis for (a,b) 8 h and (c,d) 24 h. Table 1. ΔGθθ of possible reaction in the electrolysis process at 1073 K. Table 1. ∆G of possible reaction in the electrolysis process at 1073 K. Possible Reactions θ ΔGθ1073 K (kJ/mol) No. (1) (2) (3) PossibleReactions ∆G 1073K(kJ/mol) −1045.43 −1045.43 −86.94 −21.29 No. (1) (2) (3) Ca2+ + O2− = CaO Ca2+ + O2− = CaO CaO + TiO2 = CaO·TiO2 −86.94 −21.29 CaO + TiO2 = CaO·TiO2 Ti + CaTiO3 = 2TiO + CaO Ti + CaTiO3 = 2TiO + CaO 3.3. Electro-Deoxidation Thermodynamics of Titanium Oxides in Molten Salt Systems 3.3. Electro-Deoxidation Thermodynamics of Titanium Oxides in Molten Salt Systems The main phases in TiO2 electro-deoxidation products include Ti4O7, Ti2O3, TiO, and The main phases in TiO2 electro-deoxidation products include Ti4O7, Ti2O3, TiO, and Ti. When graphite was used as the anode material, the main anode product in molten salt Ti. When graphite was used as the anode material, the main anode product in molten electrolysis was CO2 [25]. In order to simplify the calculation, CO2 was considered as the salt electrolysis was CO2 [25]. In order to simplify the calculation, CO2 was considered as only gas component in the anode product. Table 2 listed ΔGθ and E of TiO2 electro-deoxi- the only gas component in the anode product. Table 2 listed ∆Gθ and E of TiO2 electro- dation reactions at 1073 K. The theoretical decomposition potentials of TiO2 deoxidized to deoxidation reactions at 1073 K. The theoretical decomposition potentials of TiO2 de- Ti4O7 is 0.34 V, which is lower than TiO2 deoxidized to Ti2O3, TiO, and Ti. Therefore, the oxidized to Ti4O7 is 0.34 V, which is lower than TiO2 deoxidized to Ti2O3, TiO, and Ti. reaction (4) is preferentially carried out under the voltage driving force, and the first step Therefore, the reaction (4) is preferentially carried out under the voltage driving force, and reaction controlled by electrochemistry produces Ti4O7 [26]. the first step reaction controlled by electrochemistry produces Ti4O7 [26]. Table 2. ∆Gθ and E of TiO2 electro-deoxidation reactions at 1073 K. Reactions 8TiO2 + C = 2Ti4O7 + CO2 (g) 4TiO2 + C = 2Ti2O3 + CO2 (g) 2TiO2 + C = 2TiO + CO2 (g) TiO2 + C = Ti + CO2 (g) ∆Gθ1073 K (kJ/mol) 32.82 39.57 56.09 353.86 E (V) No. −0.34 (4) −0.41 (5) −0.58 (6) −0.92 (7) Table 3 listed ∆Gθ and E of Ti4O7, Ti2O3, and TiO electro-deoxidation reactions at 1073 K. The results show that E of Ti4O7 deoxidized to Ti2O3 is 0.48 V, which is lower than Ti4O7 deoxidized to TiO and Ti. Therefore, the second step reaction controlled by electrochemistry was Ti4O7 deoxidized to Ti2O3. In the same way, the third step reaction was Ti2O3 deoxidized to TiO. Finally, TiO deoxidized to Ti. According to the products obtained at different electrolysis times and electro-deoxidation thermodynamics analysis, the molten salt electrolysis from TiO2 to titanium is a multi-step electrochemical reaction process, which can be summarized as: TiO2→Ti4O7→Ti2O3→TiO→Ti.PDF Image | Electrochemical Mechanism of Molten Salt Electrolysis
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