by Mossbauer Spectrometry B. Davida,∗, O. Schneeweiss, N. Pizurova, A. Rek, V. Kudrle, O. Ja2ek CEITEC IPM, Institute of Physics of Materials, ASCR, v.v.i., iokova 22, CZ 61662 Brno, Czech Republic Institute of Scienti c Instruments, ASCR, v.v.i., Kralovopolska 147, CZ 61264 Brno, Czech Republic DPE, Faculty of Science, Masaryk University, Kotla°ska 2, CZ 61137 Brno, Czech Republic CEITEC MU, Masaryk University, Kamenice 753/5, CZ 62500 Brno, Czech Republic A few micrometers thick nanocrystalline α-Fe layer with the mean crystallite size dXRD = 14 nm was deposited in low-pressure microwave plasma, using Fe(CO)5 vapour. Its nanocrystalline character was proved on its surface under SEM (surface was formed of deposited nanoparticles) and in its volume using TEM (deposited nanoparticles were stacked up, creating columns). No signi cant iron oxide phases were observed in the transmission Fe Mossbauer spectrum measured at 5 K nor in the surface-sensitive Fe conversion electron Mossbauer spectrum measured at 293 K.