TheballmillingofFe-24MnandFe-24Mn-6Simixedpowdershasbeenperformedbythehighenergyballmillingtechnique.ByemployingX-raydiffractionandMoessbauermeasurements.Theccmpositionevolutionduringthemillingprocesshasbeeninvestigated.TheresultsindicatetheformationofparamagneticFe-MnorFe-Mn-Sialloyswithametastablefccphaseasfinalproducts.whichimplythattheFeandMnproceedaco-diffusionmeenanismthroughthesurfaceoffragmentedpowders.Thethermalstabilityandcompositionevolutionoftheas-milledalloyswerediscussedcomparingwiththebulkalloy,.