Mechanical alloying method was used to prepare nanocrystalline Co52Fe26Ni22 alloy. X-ray diffraction was applied for determination of the structure of the alloy. During milling Co-based solid solution with f.c.c. lattice was formed. After 80 h of synthesis the lattice parameter was equal to 0.3575 nm while the average grain sizes and the mean level of internal strains were about 24 nm and 0.72%, respectively. Mossbauer spectroscopy was adopted to characterize the local atomic order of the Co52Fe26Ni22 alloy. In the nearest neighbourhood of Fe-57 isotopes there are at least six Co atoms, three Ni atoms and three Fe atoms giving the hyperfine magnetic field equal to 32.45(1) T. Magnetization measurements allowed to determine the effective magnetic moment of the Co52Fe26Ni22 alloy to be equal to 1.63 mu(B) per formula unit. Curie temperature of the obtained alloy is equal to 1000 K. (C) 2004 Kluwer Academic Publishers.