Abstract: Multiple film preparation of Ti-Ni on Mo and Mo-Ti-Ni on SiO2 substrate with the method of electron beam physical vapor deposition was studied. The depth of every layer of the film was measured by using ion beam analysis method, and the hydrogenation characters of the samples were analyzed as well. It is found that the Ti-Ni film hydrogenated temperature is lower and hydrogenated ratio is higher than Ti film which shows a higher activity. The Mo-Ti-Ni film can still combine tightly with the SiO2 substrate after hydrogenation, while the substrate is cleaned more carefully. It is more difficult for the 50 nm Ti film to be hydrogenated because of the high temperature during the film preparation, which may induce a deeper diffusion among Ti, Mo and Ni to generate a thicker transition zone between Ti and Mo or Ti and Ni.