The structured powders of Fe and FeNi3 effectively by mechanical alloying (MA) method were prepared.It was found that wet milling can reduce ferrite particle size.Four dispersing agents were used for ferrite powders by settling rate method and the PVP was selected to use in wet milling.In the Fe system, wet milling process with 1 wt%PVP and without PVP were compared.After wet milling, the structured powders of ferrite were bound with epoxy to fabricate microwave absorbing composite.The return loss was measured by free space method.