We have performed a Mössbauer study on iron clusters that are formed in ytterbium films prepared by vapor co-deposition onto kapton substrates kept at room temperature. The film thicknesses were chosen in a range between 2.5 and 2.8 μm. XRD of the films reveals a mixture of fcc- and hcp-like ytterbium. Iron concentrations were between 0.3 and 5 at %. All samples reveal hyperfine spectra attributed to only two types of iron clusters with well defined hyperfine parameters. The clusters are supposed to be formed at boundaries of hcp- and fcc-like grains. In addition there is found a small contribution from monomeric iron. Spectra taken at 4.2 K reveal a complex distribution of magnetic hyperfine fields. The dynamic origin of the spectral shape is supported by susceptibility data revealing spin-freezing at temperatures below ca. 10 K. This proves that the iron clusters have sizes on the order of nm. © 2013 Springer Science+Business Media Dordrecht.