Time‐resolved high‐energy X‐ray diffraction studies of ultrathin Ni ferrite films on MgO(001)

Time‐resolved high‐energy X‐ray diffraction was used during growth of ultrathin NixFe3−xO4 films with varying Ni content (0 ≤ x ≤ 1.5) deposited on MgO(001) substrates by reactive molecular beam epitaxy, providing an insight into the growth dynamics of these films. In order to obtain structural information, reciprocal‐space maps were recorded and the temporal evolution of the Bragg peaks specific to the octahedral and tetrahedral lattice sites of the inverse spinel structure of NixFe3−xO4 was observed during growth of the films. A time delay, corresponding to a coverage of 1.2–1.8 nm, between the appearance of the Bragg reflections originating from octahedral sites and reflections originating exclusively from tetrahedral sites indicates that the ferrite films grow in two stages. In the initial growth phase, a rock salt interface layer is formed. Afterwards, a structural transition occurs and the films grow in an inverse spinel structure. The thickness of the initial rock salt phase was found to increase with Ni content and to be responsible for atypical strain in the thin films. Films with Ni contents x > 1 do not show a structural transition. These films remain in a (deficient) rock salt structure consisting of a mixed Ni–Fe oxide and do not form a spinel structure at all. They show an increased number of NiO clusters as detected by X‐ray photoelectron spectroscopy of the valence band, accompanied by a significant roughening of the films. Time‐resolved high‐energy X‐ray diffraction was used during growth of ultrathin NixFe3−xO4 films of varying Ni content (0 ≤ x ≤ 1.5) on MgO(001). For low Ni contents (x ≤ 1), the films grow initially in a rock salt phase followed by an inverse spinel structure, while overstoichiometric films (Ni contents x > 1) grow completely in a rock salt structure.