Abstract-Polyelectrolyte/iron oxide nanoparticles composite nanocoatings are fabricated by polyionic assembly. They are characterized by atomic force microscopy, electron magnetic resonance, ellipsometry, and secondary ion mass spectrometry. The results obtained indicate that the number of magnetite nanoparticle lay ers in a film is related to its refractive index, thickness, and surface roughness. The electron magnetic resonance signal intensity is found to nonlinearly depend on the number of magnetic nanoparticle layers in a film.