X-ray diffraction and transmission electron microscopy, along with electrical and film stress measurements, were used to evaluate the effectiveness of 40-nm-thick amorphous Ta2N and microcrystalline TaN diffusion barriers, both single and multilayered, against Cu penetration. Failure of the single-layered Ta2N diffusion barrier upon annealing is initialized by crystallization/grain growth, mainly helped by frozen-in compressive stress (3–4 GPa) to transform itself into a columnar structure with a comparable grain size to the thickness of the barrier. However, when subjected to annealing, the Ta2N/TaN alternately layered diffusion barrier with an optimum bilayer thickness (10 nm) remains almost stress-free (0–0.7 GPa) and transforms itself into an equiaxed structure with grain sizes of only ⩽3 nm. Such quasisuperlattice films can present lengthening and complex grained structures to effectively block Cu diffusion, thus acting as much more effective barriers than Ta2N (and TaN) single-layered films.

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