Abstract: The structure and properties of of the Ti-Al composite electrode materials prepared by the hot-pressing diffusion bonding method was analyzed by SEM, EDS, four-probe method and electrochemical workstation. The results show that the metallurgical bonding of Ti and Al can be achieved by the method of hot-pressing diffusion sintering with static pressure of 6 MPa, bonding temperature of 550℃ and holding time in Ar higher than 90 min. Change process of the diffusion reactive layer with temperature is TiAl→TiAl₂→TiAl₃. The electrochemical properties of the composite electrode materials is also much better than pure Ti anode, and the effects of preparation conditions and the resistivity on electrochemical properties are consistent. Under the same condition, the polarization potential of composite materials will fall by 37-54 mV in polarization potential of pure Ti, and the current density can be increased by more than 59.29%, while the resistivity is only 1/10 of pure Ti.