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Atomic probe tomography (APT) samples with Al/Ni multilayer structure were successfully prepared by using a focused ion beam (FIB), combining with a field emission scanning electron microscope, with a new single-wedge lift-out method and a reduced amorphous damage layer of Ga ions implantation. The optimum vertex angle and preparation parameters of APT sample were discussed. The double interdiffusion relationship of the multilayer films was successfully observed by the local electrode APT, which laid a foundation for further study of the interface composition and crystal structure of the two-phase composites. [ABSTRACT FROM AUTHOR]