This work proposed a process to prepare titanium subchlorides by using titanium and titanium tetrachloride as raw materials in an equimolar ratio of KCl-NaCl melt. According to the reactions Ti4++Ti 2Ti2+, Ti4+ +Ti2+ 2Ti3+, different molar ratio of Ti2+/Ti3+ titanium subchlordie salts could be prepared by controlling the ratio of raw materials. And the concentration of Ti2+ can be measured by the molar mass of hydrogen based on the reaction, Ti 2+ +H+ ⇌ Ti3+ +1/2H2. The total titanium chloride concentration was measured by the Diantipyryl Methane Photometric method. The prepared titanium subchloride was used as electro-activation ions for the titanium deposits in KCl-NaCl melts at 720° C.