Fe-40wt% TiB2 nanocomposites were fabricated by mechanical activation and spark-plasma sintering of a powder mixture of iron boride (FeB) and titanium hydride (TiH2). The powder mixture of (FeB, TiH2) was prepared by high-energy ball milling in a planetary ball mill at 700 rpm for 3 h followed by spark-plasma sintering (SPS) at various conditions. Analysis of the change in relative sintered density and densification rate during sintering showed that a self-propagating high-temperature synthesis reaction occurs to form TiB2 from FeB and Ti. A sintered body with relative density higher than 98% was obtained after sintering at 1150°C for 5 and 15 min. The microstructural observation of sintered compacts with the use of FE-SEM and TEM revealed that ultrafine particulates with approximately 5 nm were evenly distributed in an Fe-matrix. A hardness value of 83 HRC was obtained, which is equivalent to that of conventional WC-20 Co systems.