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Nanocomposite Nb–Al–N films prepared by magnetron sputtering have been studied. It has been found that, in the films, there are two stable crystalline structural states, namely, NbNz and B1–Nb1 - xAlxNyO1 – y, and an amorphous like component related to aluminum oxynitride upon reactive magnetron sputtering. The substructure characteristics are sensitive to the current supplied to an Al target and related to the Knoop nanohardness and hardness, which change within in the ranges of 29–33.5 and 46–48 GPa, respectively. Ab initio calculations for the NbNz and Nb2AlN phases and NbN/AlN heterostructures have been performed to interpret the obtained results for the first time.
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