A nanocrystalline iron-based powder has been prepared by microwave plasma method: Fe(CO)5 vapor was introduced into an argon discharge at ~1 kPa. A microwave 2.45 GHz generator was operated at 430 W. The reaction took place inside a quartz tube passing through a microwave waveguide. The microwave discharge (without and with Fe(CO)5) was characterized by optical emission spectroscopy. The synthesized nanopowder was passivated in situ with air. The asprepared nanopowder was characterized by TEM, XRD, Raman and Mössbauer spectroscopies. The nanopowder included α-Fe, α-Fe2O3, and Fe3O4 phases. The core-shell nanoparticles were observed under TEM: α-Fe cores had shells formed of Fe3O4 or carbon. The mean crystallite size of α-Fe was 36 nm (Scherrer formula). The synthesized nanopowder exhibited ferromagnetic behavior.