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A (111) air-exposed surface of UO2 thin film (150 nm) on (111) YSZ (yttria-stabilized zirconia) before and after the Ar+ etching and subsequent in situ annealing in the spectrometer analytic chamber was studied by XPS technique. The U 5f, U 4f and O 1s electron peak intensities were employed for determining the oxygen coefficient kO = 2 + x of a UO2+x oxide on the surface. It was found that initial surface (several nm) had kO = 2.20. A 20 second Ar+ etching led to formation of oxide UO2.12, whose composition does not depend significantly on the etching time (up to 180 seconds). Ar+ etching and subsequent annealing at temperatures 100–380 °C in vacuum was established to result in formation of stable well-organized structure UO2.12 reflected in the U 4f XPS spectra as high intensity (~28% of the basic peak) shake-up satellites 6.9 eV away from the basic peaks, and virtually did not change the oxygen coefficient of the sample surface. This agrees with the suggestion that a stable (self-assembling) phase with the oxygen coefficient kO ≈ 2.12 forms on the UO2 surface.

Ageing mechanisms of the U-5\,\%wtNb system have been investigated on samples exposed to temperatures of 150$\,^{\circ}$C for up to 5000\,hours. A variety of surface and bulk analytic techniques have been used to investigate phase, chemical and crystallographic changes. Characterisation of microstructural evolution was carried out through secondary electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDS), electron backscatter diffraction (EBSD), transmission electron microscopy (TEM) and x-ray diffraction (XRD). This investigation suggests crystallographic defects such as twinning furthers the martensitic tendencies with ageing. Resizing of the lattice and shuffling of atoms results in a small progression from the $��''$ towards the $��'$ phase.

Ageing mechanisms of the U-7\%wtNb alloy have been investigated on samples exposed to temperatures of 150$^{o}$C for up to 5000\,hours. A variety of surface and bulk analytic techniques have been used to investigate microstructural, chemical and crystallographic changes. Characterisation of the alloy's evolving behaviour was carried out through secondary electron microscopy, energy dispersive x-ray spectroscopy, electron backscatter diffraction, transmission electron microscopy and x-ray diffraction. Vickers hardness testing showed evidence of a strong thermal hardening relationship with ageing. The mechanism responsible for these changes is thought to be a stress-induced isothermal martensitic transformation; a displacive reaction, in which correlated shuffling of atoms creates a phase change from $��^{o}$ to $��''$ without chemical species redistribution.

A (111) air-exposed surface of UO2 thin film (150 nm) on (111) YSZ (yttria-stabilized zirconia) before and after the Ar+ etching and subsequent in situ annealing in the spectrometer analytic chamber was studied by XPS technique. The U 5f, U 4f and O 1s electron peak intensities were employed for determining the oxygen coefficient kO = 2 + x of a UO2+x oxide on the surface. It was found that initial surface (several nm) had kO = 2.20. A 20 second Ar+ etching led to formation of oxide UO2.12, whose composition does not depend significantly on the etching time (up to 180 seconds). Ar+ etching and subsequent annealing at temperatures 100–380 °C in vacuum was established to result in formation of stable well-organized structure UO2.12 reflected in the U 4f XPS spectra as high intensity (~28% of the basic peak) shake-up satellites 6.9 eV away from the basic peaks, and virtually did not change the oxygen coefficient of the sample surface. This agrees with the suggestion that a stable (self-assembling) phase with the oxygen coefficient kO ≈ 2.12 forms on the UO2 surface.