Surface morphology, physical-chemical properties of skeletal iron catalysts prepared by leaching of the rapidly quenched(RQ) and naturally quenched(NQ) Fe-Al alloys with an aqueous solution of NaOH were characterized by using a series of techniques including XRD, BET, XPS, SEM, H2 and CO-TPD. It was found that the RQ skeletal iron catalyst exhibits a smaller particle size, larger specific surface area and pore volume than the NQ one. The H2 and CO-TPD experiments showed that the RQ skeletal iron exhibits stronger affinity for H2 and milder affinity for CO compared with the NQ one. But the NQ skeletal catalyst shows a better thermal stability than the RQ catalyst.