Crystallization of amorphous precursors: Fe 31 Ni 50 Zr 7 B 12 , Fe 31 Ni 40 Co 10 Zr 7 B 12 and Fe 31 Ni 30 Co 20 Zr 7 B 12 was studied by the Mössbauer spectroscopy and X-ray diffraction. The nanocrystalline phases were formed by annealing the amorphous alloys at temperatures of 440-770°C. The crystallization temperatures were determined by DSC measurements. Addition of Co atoms into FeNiZrB alloy resulted in the formation of FeCo phase with large hyperfine field of 35 T. Formation of FeCo and (FeNiCo) 23 B 6 phases was followed by the Mössbauer measurements and confirmed by XRD measurements. The size of nanograins was estimated from XRD measurements using the Scherrer formula.