Zirconium, a critical rare metal with exceptional corrosion resistance and nuclear applications, is conventionally produced via the energy-intensive Kroll process. The electrolysis of ZrC_xO_y soluble anodes has been extensively investigated due to its advantages in having a short process flow and resulting in high-quality products. In particular, during the electrolysis of zirconium oxycarbide with a C:O molar ratio of 1:1, gaseous CO can be released, and no residual anodes are generated, which is extremely appealing. In this regard, this paper explores the feasibility of preparing zirconium metal through high-temperature vacuum reduction to produce zirconium oxycarbide using ZrO₂ as the raw material, followed by direct molten-salt electrolysis. Firstly, the reduction products were characterized using an X-ray diffractometer (XRD) and a scanning electron microscope (SEM). The results showed that under a vacuum of <10 Pa at 1750 °C, the reduction products mainly consisted of ZrC_xO_y and a small amount of ZrO₂, and they exhibited good electrical conductivity (0.0169 Ω·cm). Subsequently, the cyclic voltammetry test results of the reduction products revealed the reversible redox behavior of ZrC_xO_y. There were characteristic oxidation peaks at −0.53 V and −0.01 V (vs. Pt), corresponding to the formation of Zr²⁺ and Zr⁴⁺, respectively, and a reduction peak at −1.51 V, indicating the conversion from Zr²⁺ to Zr. Finally, β-zirconium metal with a purity of 99.2 ± 0.3 wt.% was obtained through potentiostatic electrolysis, and its quality met the R60704 grade specified in ASTM B551-12 (2021). This study offers a novel approach for the short-flow preparation of zirconium metal, which is conducive to expanding its applications.

Titanium metal is primarily produced via the Kroll process, which is characterized by a semi-continuous production flow and a lengthy process cycle, resulting in high production costs. Researchers have explored alternative methods for titanium production, including molten salt electrolysis, such as the Fray–Farthing–Chen (FFC), Ono Suzuki (OS), and University of Science and Technology Beijing (USTB) processes, aiming to achieve more economical production. Among these, the USTB process, a representative of soluble anode electrolysis, has shown significant promise. However, controlling oxygen concentration in titanium produced by soluble anode electrolysis remains a challenge. This study proposes a novel approach to enhance deoxidation efficiency in soluble anode electrolysis for titanium production by introducing yttrium chloride (YCl₃) into the molten salt electrolyte. Thermodynamic analysis and experimental validation demonstrate that the theoretical deoxidation limit for titanium can reach below 100 ppm under Y/YOCl/YCl₃ equilibrium. We report the successful synthesis of titanium powder with an oxygen concentration of 6000 ppm from titanium-carbon-oxygen solid solution. Under optimized conditions, the purity of the titanium powder reached 99.42%, demonstrating a new approach for producing high-purity titanium. This method, based on soluble anode electrolysis, offers a potential alternative to the conventional Kroll process. The research elucidates the fabrication process and analytical methods for titanium-carbon-oxygen solid solution, and employs a combination of analytical techniques, including XRD, SEM-EDS, and ONH Analyzer, for characterization of the electrolytic product, encompassing phase analysis, microstructure, and oxygen concentration testing.