Nickel-rich amorphous precursors with chemical composition of Ni64Fe16Zr7B12Au1 were produced by melt-spinning technique and then heat treated at temperatures ranging from 435to600°C for 1h to form a nanostructure. Properties of the amorphous and the nanocrystalline samples were investigated by the differential scanning calorimetry, the x-ray diffraction (XRD), the vibrating sample magnetometry, and Mössbauer techniques. The annealing favors the emergence of cubic FexNi23xB6 crystalline grains (1025nm in diameter). Magnetic measurements made at 4.21100K reveal rather high value of saturation magnetization (nearly 60 and 40Am2kg at 4.2K and room temperature, respectively) in amorphous as well as in nanocrystalline states. These facts are consistent with 300KFe57 Mössbauer effect results which are well supported by the calculations of Ni and Fe magnetic moments in Ni23B6 and Fe23B6 phases, using the spin polarized tight binding linear muffin-tin orbital method. However, anomalous high magnetic moments of Fe atoms were found in some inequivalent positions in the crystal structure.

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