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A nanostructured surface layer was formed in Fe-30 wt pct Ni alloy by surface mechanical attrition treatment (SMAT). The microstructure of the surface layer after SMAT was investigated using optical microscopy, X-ray diffraction, and transmission electron microscopy. The analysis shows that the nanocrystallization process at the surface layer starts from dislocation tangles, dislocation cells, and subgrains to highly misoriented grains in both original austenite and martensite phases induced by strain from SMAT. The magnetic properties were measured for SMAT Fe-30 wt pct Ni alloy. The saturation magnetization (M _s ) and coercivity (H _c ) of the nanostructured surface layers increase significantly compared to the coarse grains sample prior to SMAT. The increase of M _s for SMAT Fe-30 wt pct Ni alloy was attributed to the …