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A series of Co-rich CoxFeyNiz alloys was successfully produced using the mechanical alloying method. To check the stability of their structure thermal treatment was applied subsequently. Mössbauer spectroscopy and X-ray diffraction were used to investigate some structural and micro-magnetic properties of mechanosynthesized as well as thermally treated alloys. X-ray diffraction measurements proved that during mechanical alloying solid solutions with b.c.c. or f.c.c. lattices were formed, while thermal processing in some cases provided to decomposition into the mixture of b.c.c. and f.c.c. phases. Mössbauer spectra were fitted using hyperfine magnetic field distribution method. The average value of hyperfine magnetic field induction ranged from 31.5 to 35.5 T. In the case of some thermally treated samples, shapes of distributions reflect two-phase character of the alloys. For this reason curves of distribution were numerically fitted using two Gaussian functions, which were attributed to the suitable phases. The area of individual components was calculated.