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Mechanical alloying method was used to prepare nanocrystalline Co50Fe40Ni10, Co52Fe26Ni22 and Co65Fe23Ni12 alloys. X-ray diffraction proved that during milling Co–Fe-based solid solution with b.c.c. lattice was formed in the case of Co50Fe40Ni10, while for Co52Fe26Ni22 and Co65Fe23Ni12 compositions Co–Ni-based solid solutions with f.c.c. lattice were obtained. Mössbauer spectroscopy revealed similar values of the average hyperfine magnetic fields for all alloys, e.g. 32.17, 32.24 and 31.21 T for Co50Fe40Ni10, Co52Fe26Ni22 and Co65Fe23Ni12 alloys, respectively. Magnetization measurements allowed to determine the effective magnetic moment, Curie temperature, saturation magnetization and coercive field for the obtained alloys.
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