Mechanical alloying using high-energy ball mill and subsequent spark plasma sintering (SPS) process was applied to Al-Fe-Cr and Al-Fe-Mo powder mixture to investigate effects of Cr and Mo addition on thermal stability of Al-Fe, and thereby to enhance its thermal stability up to 500circC. Various analytical techniques including micro-Vickers hardness test, SEM, TEM, X-ray diffractometry and corrosion test were carried out. It was found that addition of Cr and Mo to Al-Fe system played a role of grain growth inhibitor of matrix Al and some precipitates such as Al_3Fe during SPS and subsequent heat treatment. The inhibition of grain growth resulted in increased Vickers hardness and thermal stability up to 500circC comparing to those of Al-Fe alloy system.