Nanocrystalline GeFe samples with Fe concentration varying from a few percent to about 86% were synthesized using an inert gas condensation method. The samples were compressed into thin disks in vacuum before exposure to air. Magnetization measurements found that the magnetization of the samples cannot be described by a simple Langevin function. Atomic force microscopy has been used to characterize the average size of the nanocrystals in the samples. For samples with a low concentration of Fe, atomic force microscopy images show distinct individual clusters with an average size of about 500 Å in diameter. For samples with a higher concentration of Fe, individual clusters cannot be distinguished, and atomic force microscope images show a mountain‐like, rugged morphology on the sample surfaces.