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A porosity-free and contamination-free surface layer with grain sizes ranging from nanometer to micrometer in Fe samples was obtained by surface mechanical attrition treatment (SMAT) technique. Mechanical and wear properties of the surface layer in the SMATed and annealed Fe samples were measured by means of nanoindentation and nanoscratch tests, respectively. Experimental results showed that the hardness of the surface layer in the SMATed Fe sample increased evidently due to the grain refinement. The elastic noduli of the surface layers in the SMATed and annealed Fe samples were unchanged, independent of grain size in the present grain size regime. Compared with the original Fe sample, the wear resistance enhanced and the coefficient of friction decreased in the surface layer of the SMATed Fe sample.