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 . 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 during SPS and subsequent heat treatment. The inhibition of grain growth resulted in increased Vickers hardness and thermal stability up to comparing to those of Al-Fe alloy system.