Abstract: The product of ball milling Ti and Ni powders of two kinds of ratio(Ti:Ni=50:50,Ti:Ni=65:35) has been investigated by XRD and XPS analyses. It is found that most part of the ball milling product is amorphous alloy. The slightly crystallization is attributed to the high ambient temperature and long milling time. The oxidation of the product's surface is thought to be caused by cleaning the stirring rod and the container during the milling process. The properties of hydrogen storage of the product are studied. It is found that the product is easy to activiate. The quantity of absorbed hydrogen increases with inceasing Ti content,and there is no plateau over 1 atm in P-C-T curves.