Iron aluminides exhibit good resistance to high-temperature oxidizing and sulphidizing
environments and have potential for structural applications at high temperatures under corrosive
environments. In this study, an Fe-Al intermetallic compound was prepared by multi-layered
roll-bonding of elemental Fe and Al foils. The process consisted of the accumulative roll-bonding
(ARB) for making a laminated Fe/Al sheet and the subsequent heat treatment promoting a
solid-phase reaction in the laminated Fe/Al sheet. Accumulated foils were rolled and bonded at
room temperature or 573 K. A pulsed electric current sintering (PECS) process was used for the
subsequent heat treatment. The microstructures produced at each processing stage were
characterized by optical microscopy and scanning electron microscopy (SEM) equipped with
energy-dispersive X-ray spectroscopy (EDS). Vickers microhardness testing was used for hardness
determination. A homogeneous intermetallic compound of Fe3Al or FeAl could be obtained after
the subsequent heat treatment for 1.8 ks at 873 K and for 3.6 ks at 1173 K.