In this work, Tb0.32Dy0.67Fe1.92 thin films were prepared by DC magnetron sputtering and then annealed at 550 °C in vacuum. The structure of sputtering Tb0.32Dy0.67Fe1.92 thin films and their surface oxidation layers were characterized by anormalous X-ray diffraction. Diffraction peaks of rare-earth oxides, Tb2O3, Dy2O3 and other non-stoichiometric peaks were found. Since the structure of Tb2O3 is the same as Dy2O3, also the lattice constant is almost similar, the composition of Tb2O3 and Dy2O3 cannot be determined by standard XRD separately. By using synchrotron radiation anomalous X-ray scattering, the amount of Tb and/or Dy oxidized at different annealing conditions were determined. In addition, using the anomalous X-ray diffraction and electron probe micro-analyzer, the Fe clusters phase segregated from the bulk matrix without oxidation was also identified. These pure Fe cluster without oxidation might be due to the presentation of Dy and Tb matrix which protect Fe from oxidation.

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