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Ta/TaN bi-layer structure is currently used in the ultra-large scale integrated circuits (ULSI) interconnect as barrier for copper because of its good adhesion to both SiO₂ and Cu wire. In this work Cu, Ta and TaN layers were prepared by sputtering technology. X-ray diffraction, Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS) as well as transmission electron microscopy (TEM) were applied to characterize the thin film thermal stability and microstructure evolution. The results show that the Ta/TaN bi-layer structure has much better diffusion barrier properties than pure Ta or pure TaN film. A mechanism was proposed to explain the better thermal stability of the Ta/TaN bi-layer structure based on the correlation between TaN layer thickness and TaN crystallization kinetics. The microstructure evolution for Ta/TaN bi-layer structure during annealing was described.