Using controlled N2/Ar sputtering gas mixtures, rf‐sputtered films were prepared from Fe, Ni, and Ni81Fe19targets, and their structure and orientation were studied by x‐ray diffraction. When no N2was introduced during sputtering, all the films were oriented in the highest density planes; i.e., in (110), (111), and (111) for &agr;‐Fe, Ni, and &ggr;‐Ni81Fe19, respectively. With increasing N2introduction, however, the orientation shifted to lower density planes, and eventually nitrides were formed. Multilayer films of metal and nitride were prepared with the Ni81Fe19target by repetitive supply of N2for short periods during sputtering. Strong orientation effects were observed depending on the number of layers grown. In addition, the x‐ray diffraction of these films presented evidence of epitaxial growth of the nitrides (Ni,Fe)4N on the alloy layers.