The Ni(Cr)-Cr3C2-Cr7C3-TiC composite powder was prepared by SHS (Self-propagating High-temperature Synthesis) process using elemental powders as starting materials. As-prepared powder was ground by a high-energy mill. The morphology of as-prepared and ground powders was analyzed by SEM method; the microstructure of powders was also observed by light microscopy. The X-ray diffraction methods were applied for the structure analysis of the studied samples. The Rietveld method appeared to be very useful in the verification of the qualitative phase composition and in the determination of phase abundance in the studied material. The parameters of diffraction line profiles were determined by PRO-FIT Toraya procedure. The crystallite sizes and lattice distortions were analyzed using Williamson-Hall method. It was found that during high-energy milling a significant decrease of crystallite size to nanoscale is observed only for Ni(Cr) phase.

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