Fe-aluminides have the potential to replace many types of stainless steels that are currently used in structural applications. Once commercialized, it is expected that they will be twice as strong as stainless steels with higher corrosion resistance at high temperatures, while their average production cost will be approximately 10% of that of stainless steels. Self-propagating, high-temperature Synthesis (SHS) has been used to produce intermetallic and ceramic compounds from reactions between elemental constituents. The driving force for the SHS is the high thermodynamic stability during the formation of the intermetallic compound. Therefore, the advantages of the SHS method include a higher purity of the products, low energy requirements and the relative simplicity of the process. In this work, a Fe-aluminide intermetallic compound was formed from high-purity elemental Fe and Al foils via a SHS reaction in a hot press. The formation of iron aluminides at the interface between the Fe and Al foil was observed to be controlled by the temperature, pressure and heating rate. Particularly, the heating rate plays the most important role in the formation of the intermetallic compound during the SHS reaction. According to a DSC analysis, a SHS reaction appeared at two different temperatures below and above the metaling point of Al. It was also observed that the SHS reaction temperatures increased as the heating rate increased. A fully dense, well-bonded intermetallic composite sheet with a thickness of 700 μm was formed by a heat treatment at 665˚C for 15 hours after a SHS reaction of alternatively layered 10 Fe and 9 Al foils. The phases and microstructures of the intermetallic composite sheets were confirmed by EPMA and XRD analyses.