Uranium trioxide behavior during electron energy loss spectroscopy analysis

• EEL spectra recorded as a function of UO3 sample thickness.
• The analysis was performed for the P and O edges.
• Reduction of UO3 into U4O9 and/or UO2 readily observed during TEM investigations.
• Reduction of UO3 was confirmed by electron diffraction.

A sample of uranium trioxide (UO3) was produced by focused ion beam (~10 μm×~10 μm×<0.5 μm) for transmission electron and electron energy loss (EEL) spectroscopy examinations in a transmission electron microscope (TEM). The EEL spectra were recorded as a function of the thickness for the P and O edges in the low energy range 0–350 eV and were compared to spectra of UO3 small grains attached to a TEM grid. The EEL spectrum was studied through a range of thicknesses going from ~60 to ~260 nm. The EEL spectra recorded for UO3 are compared with those recorded for UO2. The reduction of UO3 into U4O9 and/or UO2 is readily observed apparently during the TEM investigations and as confirmed by electron diffraction (eD). This redox effect is similar to that known for other redox sensitive oxides. Recommendations are suggested to avoid sample decomposition.