The Ti-Al composite electrode materials was prepared by hot press diffusion bonding in this article, and by the scanning electron microscopy (SEM), the energy dispersive spectroscopy (EDS), four-probe method, electrochemical workstation test means were used to test the structure and properties of the samples. The results show that the method of hot pressing diffusion sintering can achieve metallurgical bonding of Ti and Al with static pressure of 6MPa, holding times of 120min, in Ar and bonding temperature higher than 550°C,as well resistivity of the composite had dropped significantly, it was only 1/10 of pure Ti. The electrochemical properties of the composite electrode materials is also much better than pure Ti anode, and preparation conditions on electrochemical properties and the resistivity is consistent with law. This also shows that the conductivity of metal matrix will directly affect the catalytic properties of electrode materials for electrochemical. Therefore, changes in the composition of the electrode base material and structure not only reduces the cost and improve the performance of the electrode, also reached the purpose of energy saving.