Titanium was prepared from TiCl
4 in molten NaCl-KCl-NaF salt. The product of the reaction of TiCl
4 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 TiCl
4 to NaCl-KCl-NaF melts. The results indicate that Na
2TiF
6 was first obtained through the reaction of NaF with TiCl
4 in the NaF-KCl-NaCl melt, and Na
2TiF
6 was decomposed to Na
+ and [TiF
6]
2− in the melts. [TiF
6]
2− was then sequentially reduced to [TiF
6]
3− and Ti at the cathode, accompanied by chlorine gas emission at the anode and fluoride formation at the cathode.
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