Zhuxian Q, Liman F, Grjotheim K, Kvande H (1987) Formation of metal fog during molten salt electrolysis observed in a see-through cell. Okabe TH, Suzuki RO, Oishi T, Ono K (1991) Thermodynamic properties of dilute titanium-oxygen solid solution in beta phase. Xie HW, Zhao HJ, Qu JK, Song QS, Ning ZQ, Yin HY (2019) Thermodynamic considerations of screening halide molten salt electrolytes for electrochemical reduction of solid oxides/sulfides. Suzuki RO, Ono K (2002) A new concept of sponge titanium production by calciothermic reduction of titanium oxide in the molten CaCl 2. Kumamoto K, Kishimoto A, Uda T (2020) Low temperature electrodeposition of titanium in fluoride-added LiCl–KCl–CsCl molten salt. Zhu F, Li L, Cheng X, Ma S, Jiang L, Qiu K (2020) Direct electrochemical reduction of low titanium chlorides into titanium aluminide alloy powders from molten eutectic KCl–LiCl–MgCl 2. Wu J, Song J, Zhu H, Shu Y, He J (2019) Equilibrium between metallic titanium and titanium ions in MgCl 2–LiCl molten salt. Lu X, Ono T, Takeda O, Zhu H (2019) Production of fine titanium powder from titanium sponge by the shuttle of the disproportionation reaction in molten NaCl–KCl. ![]() Suzuki RO (2005) Calciothermic reduction of TiO 2 and in situ electrolysis of CaO in the molten CaCl 2. Song Y, Dou Z, Zhang TA, Liu Y (2020) Research progress on the extractive metallurgy of titanium and its alloys. Suzuki RO, Natsui S, Kikuchi T (2021) Recent studies on titanium refining: 2017–2020. Therefore, synthesis of calcium hydride due to contact with precipitated Ca is highly probable, in addition to the H 2 generation observed in the form of bubbles. The H 2 generation estimated from the Coulombic efficiency was miniscule when the ratio of H 2 generation to the total amount of electricity contributing to the electrochemical reaction was calculated from the directly observed bubble volume. Moreover, we established that the cathodic current density increased with respect to the same potential. The H 2 gas generation occurred simultaneously with the electrochemical deposition of Ca when the H 2O content increased. The impact of residual H 2O on the cathodic reaction was estimated by electrolyzing H 2O-containing CaCl 2 at 1173 K in Ar atmosphere using high-speed imaging, which visualized the H 2 bubbles occurring around the cathode, to analyze the incomplete removal of H 2O in CaCl 2. The H 2 generated during the electrolysis of H 2O present in molten CaCl 2 inhibits metallothermic reduction by metallic Ca.
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