Nanocrystalline iron samples were carburised with CO/CO₂ mixture at 400 - 550C. The product obtained contained 29% Fe3C, 35% Fe₃O₄ and 36% C as carbon fibres. The sample were characterised by XRD, TOC (total carbon, Multi N/C) and SEM after carburisation. This iron-carbon composite was used as a filler for PTMO - block - PET polymer, with low concentration (0.5%) of iron-carbon composite. Electron Spin Resonance investigations of the sample were carried out in the 4-300 K temperature range. At room temperature a strong symmetrical signal with g = 2.229 ⁺- 0.022 and linewidth of 150 mT dominates the spectrum. With the temperature decrease the intensity of the line is decreasing, but at temperature of about 90 K another line appears with g = 2.666 ⁺- 0.032. This low-temperature line is very anisotropic and its low-field shoulder spreads to negative magnetic fields. With decreasing temperature, the linewidth of this line decreases slightly, in contrast to the behavior of the high-temperature line. The intensity of the low-temperature line is approximately independent on temperature, while the intensity of the high-temperature line strongly depends on temperature. The difference in behavior of these two lines suggests that they originate from different magnetic centers. Based on detailed analysis we suggest that the line visible at higher temperatures arises form Fe₃O₄ (magnetite) nanoparticles, whereas the line visible below 90 K arises from Fe₃C (cementite) nanoparticles. The disappearance of the line from magnetite may be caused by the so-called blocking effect, i.e. the interaction between paramagnetic Fe₃O₄ nanoparticles and the polymer matrix.

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