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First results in the field of synthesis and research of the multicomponent (Ti-Zr-Hf-V-Nb)N nanostructured coatings are presented in the paper. Influence of processes of spinodal segregation and mass-transfer on single-layered or multilayered crystal boundary (second phase) forming were explored. Superhard nanostructured coatings were investigated before and after annealing at the temperature 600°C using unique methods (slow positron beam, proton microbeam particle induced X-ray emission-μ, Rutherford backscattering-analysis, scanning electron microscopy with energy dispersive X-ray spectroscopy, X-ray diffraction analysis was performed using DRON-4 and nanoindentor). Diffraction spectra were taken point-by-point, with a scanning step 2Θ=0.05 to 0.1°. We detected that positron trapping by defects was observed on the nanograins boundaries and interfaces (vacancies and nanopores which are the part of triple and larger grain's boundary junction). The 3D distribution maps of elements obtained by the proton microbeam (particle induced X-ray emission-μ) together with the results obtained by slow positron microbeam gave us comprehensive information about physical basis of the processes, connected with diffusion and spinodal segregation in superhard coatings.
