Surface treatment of Ni-Ti fibers were processed by using various chemical solutions, including the hydrochloric acid, the mixture solvent of hydrofluoric-nitric acid and the solvent of potassium dichromate-vitriol. Scan electric microscopy (SEM) and fiber pull-out test were adopted to characterize the corrosive effect of the chemicals and the shear strength of the fiber/resin interface. The results showed that the surface of the alloy fiber is corroded most seriously after acid treatment with the mixture of hydrofluoric acid and concentrated nitrate. Tensile test result also shows that the maximum interfacial bonding strength is obtained by treatment with this acid. The effect of the cross-link agent in epoxy was also discussed.