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Polymer-derived SiCNFe ceramics is a prospective material that can be used as soft magnets in MEMS magnetic applications. The optimal synthesis process and low-cost appropriate microfabrication should be developed for best result. Homogeneous and uniform magnetic material is required for developing such MEMS devices. Therefore, the knowledge of exact composition of SiCNFe ceramics is very important for the microfabrication of magnetic MEMS devices. The Mössbauer spectrum of SiCN ceramics, doped with Fe (III) ions, and annealed at 1100 °C, was investigated at room temperature to accurately establish the phase composition of Fe-containing magnetic nanoparticles, which were formed in this material at pyrolysis and which determine their magnetic properties. The analysis of Mössbauer data shows the formation of several Fe-containing magnetic nanoparticles in SiCN/Fe ceramics, such as a-Fe, Fe_xSi_yC_z, traces of Fe-N and paramagnetic Fe³⁺ with octahedral oxygen environment. The presence of iron nitride and paramagnetic Fe³⁺ ions shows that the pyrolysis process was not completed in SiCNFe ceramics annealed at 1100 °C. These new observations confirm the formation of different Fe-containing nanoparticles with complex composition in SiCNFe ceramic composite.