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The USTB process with a consumable TiCxOy anode is considered as a low-cost and eco-friendly method for Ti production. However, the dendritic Ti products have disadvantages of high oxygen and salt contents. Here, a liquid Zn cathode was proposed to prepare Ti–Zn alloys from a casting TiC0.5O0.5 anode via a one-step electrolysis process in a NaCl–KCl molten salt. Cyclic voltammetry and square-wave voltammetry were used to investigate the electrochemical dissolution of Ti ions from a consumable TiC0.5O0.5 anode and subsequent reduction behavior on cathode. The results indicate that the reduction potential of Ti on a liquid Zn cathode is more positive than that on a solid W cathode. Ti2+ from the casting TiC0.5O0.5 anode was one-step reduced to Ti on the liquid Zn cathode. A quasi-reversible process was confirmed via diffusion-controlled mass transfer, and the diffusion coefficient of Ti2+ toward the liquid Zn electrode was 4.35 × 10−5 cm−2 s−1. The concentration of Ti2+ in molten salt is more stable during electrolysis with a liquid Zn cathode. Ti–Zn alloys were successfully prepared at a current density of 0.3 A cm−2 using a casting TiC0.5O0.5 anode and a liquid Zn cathode. Metallic Zn was confirmed to be a promising liquid cathode to prepare Ti–Zn alloys via the USTB process. [ABSTRACT FROM AUTHOR]