Electrodeposition of Al on Ti substrate from a dimethylsulfone (DMSO2) bath and subsequent annealing were conducted to examine the feasibility of the process for the fabrication of TiAl3 oxidation-resistance layer. A dense, uniform Al layer adhere to Ti substrate could be obtained by performing anodic dissolution of the Ti substrate in the DMSO2 bath prior to the electrodeposition of Al. Annealing of the Ti substrate with the Al layer at 650-1000 degrees C in vacuum yielded TiAl3 layer on the Ti substrate.