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Materials 2022, 15, 3956 4 of 11 Materials 2022, 15, x FOR PEER REVIEW In anode: In cathode: CO2 + O2− = CO2− 3 CO2− +4e− = C+3O2− 3 5 of 11 3.2. Electro-Deoxidization of the Cathode Precursor Figure 4 presents the XRD patterns of the products at different electro-deoxidation time. It can be seen from the product electrolyzed for 0 h that TiO2 is the main component of the cathode precursor, which indicates that the little carbon did not react with TiO2 in the sintering process. The product electrolyzed for 8 h shows the intermediate valence titanium oxides (Ti4O7, Ti2O3, TiO) and CaTiO3 are the main phases of the product after 8 h electrolysis. CaTiO3 is generated by the reaction between TiO2 and calcium ions in molten salt and oxygen ions extracted from TiO2. Table 1 lists the possible reaction ∆GΘ in the electrolysis process at 1073 K. Reaction (1) has an extremely negative ∆GΘ(−1045.43 kJ/mol) at 1073 K, indicating that the formation of CaO betweent Ca2+ and O2− extracted from TiO2 is easy to proceed. The ∆Gθ of CaTiO3 generated by the reaction of CaO and TiO2 was −86.94 kJ/mol, demonstrating that the reaction could occur spontaneously. Literatures show that there is a high concentration of oxygen in the material at this stage; that is, CaTiO3 will be spontaneously formed when calcium ions and oxygen ions existed in the molten salt [24]. The diffraction peak of titanium detected in the product electrolyzed for 8 h indicates that titanium metal can be reduced after 8 h of electrolysis. Compared with the product of electrolysis for 8 h, the diffraction peak of titanium in the product of electrolysis for 24 h is significantly increased (shown in the XRD pattern of the product electrolyzed for 24 h), indicating that the reduction of titanium metal is further carried out with the extension of the electrolysis time. Figure 5 presents SEM images and EDX analysis of the products electrolysis for 8 h and 24 h. Combined with XRD data analysis in Figure 4, they show that CaTiO3 was formed in the products electrolysis for 8 h during the electrolysis process, shown in reaction (2). The main phase is the intermediate valence titanium oxides, and the CaTiO3 phase almost disappears in the products electrolysis for 24 h, which is due to the spontaneous decomposition between CaTiO3 and titanium, shown in reaction (3). The deposited carbon can react with the metal on the cathode, resulting in high carbon content in the cathode product. It can be explained by the following two reactions. Figure 4. XRD patterns of the products at different electro-deoxidation times. Figure 4. XRD patterns of the products at different electro-deoxidation times.PDF Image | Electrochemical Mechanism of Molten Salt Electrolysis
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