The evolutions of microstructure of Fe0.85Ni0.15 products, which were prepared by mechanical alloying (MA) with and without process control agent (PCA), were studied using X-ray diffraction and scanning electron microscopy respectively. After MA without PCA (dry method) for 30h, Fe0.85Ni0.15 nanocrystalline alloy powders with bcc-Fe(Ni) phase were obtained; however, powders milled with PCA (wet method) from 20 to 90h, were unalloyed Fe-Ni mixtures with balanced morphology. It seems that dry method works efficiently in nanocrystalline alloying while wet method postpones MA but functionally fines the morphology of materials. Finally, the results were discussed considering the MA kinetics.