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Using X-ray microanalysis and scanning electron microscopy Zn-Ni-SiO2 plating containing SiO2 nanoparticles were studied. It was found that X-ray irradiation of the electrolyte leads to the increased Ni concentration in ZnNi-SiO2(X) lms and the grain size is also increasing (the grain size is twice that in the unirradiated case). A thickness of Zn-Ni-SiO2(X) plating is 20 µm and a thickness of the Zn-Ni-SiO2 plating is about 15 µm. The surface morphology was studied using AFM method. Increasing Ni concentration and Ni5Zn21 phase due to X-Ray irradiation of the electrolyte leading to the improved mechanical properties of the coating.

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First results in the eld of synthesis and research of the multicomponent (TiZrHfVNb)N nanostructured coatings are presented in the paper. Inuence 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 diraction analysis was performed using DRON-4 and nanoindentor). Diraction 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 diusion and spinodal segregation in superhard coatings.