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Materials 2022, 15, 3956 6 of 11 Table 3. ∆Gθ and E of Ti4O7, Ti2O3, and TiO electro-deoxidation reactions at 1073 K. Reactions 2Ti4O7 + C = 4Ti2O3 + CO2 (g) Ti4O7 + 1.5C = 4TiO + 1.5CO2 (g) Ti4O7 + 3.5C = 4Ti + 3.5CO2 (g) 2Ti2O3 + C = 4TiO + CO2 (g) Ti2O3 + 1.5C = 2Ti + 1.5CO2 (g) 2TiO+C=2Ti+CO2 (g) ∆Gθ1073 K (kJ/mol) 46.31 95.76 337.44 72.60 314.29 241.68 E (V) −0.48 −0.99 −3.50 −0.75 −1.09 −1.25 No. (8) (9) (10) (11) (12) (13) 3.4. Analysis of Electrochemical Deoxidation of TiO2 in NaCl-CaCl2 System Then, 3 wt.% TiO2 was added to NaCl-CaCl2 binary molten salt system, and then the samples from the upper, middle, and lower crucibles were taken for XRD analysis after being heated to 1073 K for 4 h. The XRD patterns (Figure 6) show that no other substances were found in the samples taken from the upper and middle crucibles and TiO2 was deposited in the bottom of the crucible. It indicates that there is no chemical dissolution of TiO2 in the molten salt system. CaTiO3 cannot be formed spontaneously, because there salt system. Figure 6. XRD patterns of the binary salt samples taken from upper, middle, and lower crucibles. Figure 6. XRD patterns of the binary salt samples taken from upper, middle, and lower crucibles. Figure 7 displays the CV curves of NaCl-CaCl2 system before and after TiO2 addition. There is no redox peak found in the CV curve of NaCl-CaCl2 system without 3 wt.% TiO2; it demonstrates that the electrochemical properties of the binary molten salt electrolyte are stable, and the trace impurities in the salt have no influence on the experiment. CV curve of NaCl-CaCl2 system with 3 wt.% TiO2 shows that there are four reduction peaks, a, b, c, and d, which appear in the reduction process, and one oxidation peak d’ appears in the oxidation process. The asymmetric CV curve of NaCl-CaCl2 system without 3 wt.% TiO2 and |ipa/ipc|̸=1 prove that the existence of reduction was an irreversible process. According to the four reduction peaks on the CV curve, the reduction of TiO2 to titanium metal may be divided into four steps, which was consistent with the above thermodynamic calculation results. Figure 7. CV curves of NaCl-CaCl2 system before and after 3 wt.% TiO2 addition with 0.7 V/s vs. Pt scan rate. Materials 2022, 15, x FOR PEER REVIEW 7 of 11 is no electro-deoxidation reaction conducted to produce oxygen ions in the binary molten Figure8displaystheCVcurvesofNaCl-CaCl-TiO systemwithdifferentscanrates.PDF Image | Electrochemical Mechanism of Molten Salt Electrolysis
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