Fe-40Al-40Ni-20 and Fe-40Al-40Mn-20 (all in at.%) intermetallics were mechanically alloyed for 40 h and followed by hot-pressing at 650degreesC under 450 MPa for 1 h. As resulted from the X-ray diffraction studies, the ordered B2 structure was formed in the Fe-40Al-40Ni-20 alloy while in the case of Fe-40Al-40Mn-20 alloy, the disordered Fe(Al) solid solution was observed. The chemically homogenous rounded particles of size of about 5 mum were identified using scanning analytical electron microscopy in alloys after 40 h of milling. TEM studies of milled powders revealed a nanostructure in both alloys with grain size of about 20 nm. The hot pressing process of milled powders allowed to obtain compacts with the density of about 87 and 89% of the theoretical one for Fe-40Al-40Mn-20 and Fe-40Al-40Ni-20 alloys, respectively. The micro-hardness measurements have shown that the alloy with the Ni addition possesses the hardness of about 1200 HV20, whereas in the alloy with the Mn addition it is 1100 HV20. The TEM investigations allowed to identify a nanocrystalline structure of compacts with a mean grain size below 50 nm, with B2 ordered structure in both alloys. (C) 2004 Kluwer Academic Publishers.