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Mechanically alloyed FexNi77-xCu1Nb2P14B6 soft magnetic materials have been prepared with different atomic compositions. The alloy structures are investigated by X-ray absorption fine structure (XAFS). The results show that mechanical alloying (MA) can drive the FexNi77-xCu1Nb2P14B6 powder mixture to produce amorphous alloy while the atomic concentration of Fe element is about and over 40%. On the contrary, the MA FexNi77-xCu1Nb2P14B6 is a solid solution with a fcc-like structure in the region of lower Fe atomic concentration (<22%), preserving a medium-range order around Ni and Fe atoms. Moreover, we have found that the local structure geometry of Fe atom is similar to that of Ni atom for all the MA FexNi77-xCu1Nb2P14B6 samples. It indicates that the local structures of Fe and Ni atoms in a FexNi77-xCu1Nb2P14B6 sample only depend on the x value of element Ni after ball milling.

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