Titanium was prepared from TiCl₄ in molten NaCl-KCl-NaF salt. The product of the reaction of TiCl₄ with NaF was identified using X-ray diffraction, and its electrochemical behavior was studied using cyclic voltammetry and square wave voltammetry. The electrochemical deposition of titanium was investigated during the addition of TiCl₄ to NaCl-KCl-NaF melts. The results indicate that Na₂TiF₆ was first obtained through the reaction of NaF with TiCl₄ in the NaF-KCl-NaCl melt, and Na₂TiF₆ was decomposed to Na⁺ and [TiF₆]²⁻ in the melts. [TiF₆]²⁻ was then sequentially reduced to [TiF₆]³⁻ and Ti at the cathode, accompanied by chlorine gas emission at the anode and fluoride formation at the cathode.