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Materials 2022, 15, 3956 3 of 11 Materials 2022, 15, x FOR PEER REVIEW 3 of 11 (SEM) (S-4800, Hitachi, Tokyo, Japan) and energy dispersive X-ray spectroscopy (EDX). The acceleration voltage of SEM is 20 kV and the working distance (WD) is 10 mm. V A RE WE Argon gas cylinders Furnace Argon outlet Cooling water inlet Cooling water outlet Argon inlet CE Electrochemical workstation Computer Temperature controller Figure 2. Schematic diagram of the electrochemical experimental platform. Figure 2. Schematic diagram of the electrochemical experimental platform. 3. Results and Discussion 2.4. Characterization 3.1. Calculation of the Theoretical Decomposition Potentials The electrolytic voltage was supplied by DC power supply (DP310, MESTEK, China). Alkaline metal molten salts with low melting point, wide electrochemical window, The phase composition of the solid precursors and cathodic products were determined by and good electrical conductivity are commonly used as electrolytes for electrochemical X-ray diffraction (XRD) (Noran7, Thermo Fisher, Waltham, MA, USA). Each scan was 5°– preparation of metals. The Gibbs free energy of the possible reactions can be calculated by 90° and step size is 0.02°. The morphology and chemical composition of the solid precur- sHorSsCantdhecarmthodiycnparomdiuccstsowftewreacrhea.rTachtertihzedorbeytiscalndniencgoemlepcotrsointimonicprostceonptyia(lSsE(ME) (oSf-the metal 4m80o0l,tHenitasachltis, TaonkdyoT,iOJapawne)raencdaelcnuerlgaytedisbpyertshiveefoXl-lroawyisnpgecetrqousacotipoyn(E[2D2X,2)3.]T:he accel- 2 eration voltage of SEM is 20 kV and the working distance (WD) is 10 mm. 3. Results and Discussion −∆GΘ E= nF (1) 3.1. Calculation of the Theoretical Decomposition Potentials crucible Thermocouple where ∆GΘ (kJ/mol) is the standard Gibbs free energy change; n and F represent the electron Alkaline metal molten salts with low melting point, wide electrochemical window, transfer number and Faraday’s constant (96,485 C/mol), respectively. The theoretical and good electrical conductivity are commonly used as electrolytes for electrochemical decomposition potentials and reactions that occurred in the electro-deoxidation cell from preparation of metals. The Gibbs free energy of the possible reactions can be calculated by 773 K to 1273 K are listed in Figure 3. The results show that the theoretical decomposition HSC thermodynamics software. The theoretical decomposition potentials (E) of the metal mpolttentsialtsoanfdTTiOiO22awnedretchaelcubliantaerdybysatlhteafroellopwoisnigtiveqeulyatcionrr[e2l2a,2te3]d: withtemperature. The theoreticaldecompositionpotentialsofNaClandCaCl is−3.29Vand−3.23V,respectively, −ΔGΘ 2 which is much higher than that of TEiO=2. It indicates that the experiment vo(l1ta)ge of 3 V, Materials 2022, 15, x FOR PEER REVIEW nF 4 of 11 conducted in a two-electrode system, is sufficient to electro-deoxidize TiO2 to titanium Θ whiethreoΔuGt th(ekJe/mlecotlr) oislythte dsteacnodmarpdoGsitbibosnf.ree energy change; n and F represent the elec- tron transfer number and Faraday’s constant (96,485 C/mol), respectively. The theoretical decomposition potentials and reactions that occurred in the electro-deoxidation cell from 773 K to 1273 K are listed in Figure 3. The results show that the theoretical decomposition potentials of TiO2 and the binary salt are positively correlated with temperature. The the- oretical decomposition potentials of NaCl and CaCl2 is −3.29 V and −3.23 V, respectively, which is much higher than that of TiO2. It indicates that the experiment voltage of 3 V, conducted in a two-electrode system, is sufficient to electro-deoxidize TiO2 to titanium without the electrolyte decomposition. Figure3.Theorreetitcicaallddeceocmompopsoitsiiotniopnopteontteinaltsiaalnsdanredarcetiaocntsiooncscuorcrceudrirnedthienetlheecterole-dcterox-ideaotixoindationcell cell from 773 K to 1273 K. VVT T II from 773 K to 1273 K. 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 valencePDF Image | Electrochemical Mechanism of Molten Salt Electrolysis
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