Abstract: The spark plasma sintering (SPS) technology was used to realize the preparation of the iron-nickel alloy layer on the surface of pure iron with nickel powder paving on the iron surface. The surface nano-layer and graded structure obtained by the pre-surface mechanical attrition treatment (pre-SMAT) on the pure iron surface effectively promotes the diffusion of iron and nickel during SPS, and the thickness and bonding strength of the alloy layer improves. By XRD, SEM, EDS, hardness, and friction and wear tests, the morphologies and composition were characterized, and the mechanical properties of the iron-nickel alloy layer were tested.The results show that after SMAT+SPS, an iron-nickel alloy layer with the thickness of about 50 μm on the pure iron sample has been prepared. And in the depth direction, the nickel content shows a gradient change. However, the alloy layer depth on the surface of pure iron without SMAT pretreatment is just 25 μm.Therefore, the method can achieve a significant increase in the thickness of the alloy layer. After SMAT pretreatment, the hardness of the surface alloy layer increases, the wear mass loss of surface and the depth of the plough groove reduce. The bonding strength increases.The wear resistance obviously improves.