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Nanostructural γ-Ni-28Fe alloy (nano γ-Ni-28Fe) was successfully prepared by mechanochemical alloying(MCA). The relationship between the microstructure and the synthesis conditions was investigated by using XRD, TEM, SEM as well as BET analyzer. The results show that nano γ-Ni-28Fe alloy is composed ora gamma phase (FCC structure). Its grain size is about 20 nm at reduction temperature below 600 ℃. The magnetic measurements indicate that the saturation magnetization ofnano γ-Ni-28Fe alloy to its decrease of the grain size and chemical composition in nano γ-Ni-28Fe alloy.