Abstract: In order to enhance the tensile strength, impact strength and flexural strength of NiTi fiber/resin composites, surface treatment of NiTi fiber was conducted using nitric acid, silanes coupling agent, triisocyanate coating and the combined treatment of low-temperature plasma and silanes coupling agent, and the surface adhesion strength between the fiber and resin matrix enhanced. Experimental results indicated that after treating NiTi fiber with different processes, the maximum ILSS of NiTi fiber/epoxy corresponded to an increase of 10.90% to 44.74%. The tensile strength, impact strength and flexural strength of NiTi fiber/epoxy in which NiTi fiber was prepared by silanes coupling agent after treated with low-temperature plasma had an increase of 88.81%, 98.43% and 45.55% respectively, and the treated fiber and resin was bond well in SEM pictures.