Nanosize amorphous Fe-Ni-P-B alloy powders have been made by chemical reduction. The crystallization processes of the alloys have been studied by X-ray diffraction (XRD). The crystallization processes of different alloys vary with composition and chemical short-range order, which is determined by prepared conditions. A new kind of oxide phase (N-phase) has been found and determined by a double tilting method in transmission electron microscopy (TEM). This phase belongs to a body centered orthogonal lattice with a = 5.3 Angstrom, b = 8.5 Angstrom, c = 12.7 Angstrom.
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