The in-situ Fe based nanocomposite containing Fe-Al2O 3 particle is synthesized by reactive milling of Fe-Al 2O3-Al-Fe powder mixture in toluene medium followed by consolidation of powders using Spark Plasma Sintering process. Transmission electron microscopy investigation of consolidated Fe-Fe-Al2O 3 nanocomposites has shown heterogenous grain structure of Fe consisting of nano, submicron and micron size grains together with nanometer Fe-Al2O3 particles. The hardness of Fe-Al2O3 nanocomposites consolidated at 800°C is 795 MPa. © (2012) Trans Tech Publications.