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This paper investigates the microstructure, physical, chemical and mechanical of superhard nanocomposite of Ti-Hf-Si-N. The coatings were grown by C-PVD method. Profiles of elements and vacancy-type defects (S-parameter measurements of the Doppler broadening of the annihilation peak DBAP) in the studied coatings were investigated. Defined and calculated the elastic modulus E, hardness H, friction, adhesion. Wear rate was determined as a function of the bias potential supplied to the substrate and the pressure in the chamber. The developed coatings have hardness of 37.8 to 48 GPa, the friction coefficient of 0.48 to 0.15, the grain size of the solid solution from 3.9 to 10.8 nm (depending on deposition conditions). It was found that positrons are trapped by defects at the junction of three or more nanograins interfaces. In some cases, there was formed two phases in coatings: a solid solution (Ti, Hf)N with different volume content of Hf in a solid solution, and an amorphous phase α-Si3N4 (the layer between the nanograins).