In the CaCl2 molten salt, TiFe alloy was prepared by electroanalysis using titanium concentrate as the cathode. XRD and SEM analyses of products were performed. The electrolytic products at different temperatures were compared. Results show that the temperature has significant effects on diffused alloying process, and the phases and structures of electrolytic products are different. At 850 oC, the final electrolytic product is the TiFe2 and Ti discrete ball-type structure with the particle size of 1 μm, while at 900 oC the final product is the TiFe space net structure with the particle size of 3 μm