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We employed correlative atom probe tomography (APT) and transmission electron microscopy (TEM) to analyze the alumina scale thermally grown on the oxide dispersion-strengthened alloy MA956. Segregation of Ti and Y and associated variation in metal/oxygen stoichiometry at the grain boundaries and triple junctions of alumina were quantified and discussed with respect to the oxidation behavior of the alloy, in particular, to the formation of cation vacancies. Correlative TEM analysis was helpful to avoid building pragmatically well-looking but substantially incorrect APT reconstructions, which can result in erroneous quantification of segregating species, and highlights the need to consider ionic volumes and detection efficiency in the reconstruction routine. We also demonstrate a cost-efficient, robust, and easy-handling setup for correlative analysis based solely on commercially available components, which can be used with all conventional TEM tools without the need to modify the specimen holder assembly.
The application of safeguards measures by the International Atomic Energy Agency (IAEA) involves analytical measurements of samples taken during inspections of nuclear facilities. Thus constant development and advancement of analytical techniques is required. For quality control purposes, the IAEA has implemented a dedicated project to enhance its analytical capabilities by producing tailor-made reference materials for the analysis of uranium isotope signatures in (single) particles.
To this end, a particle production set-up was developed and implemented at Forschungszentrum Juelich capable to produce uranium oxide microparticles which are intended to be used as (certified) reference materials for particle analysis methods. A step towards the certification process is the evaluation of consistency of the size distribution and homogeneity. A monodisperse particle size distribution as well as the single phase triuranium octoxide structure was confirmed using SEM, µ-XRD and µ-Raman spectroscopy, respectively. Analysis performed on single uranium oxide microparticles confirmed consistency of the uranium isotopic ratios in comparison to the initial precursor solutions. To improve the homogeneity and particle handling, the particles are transferred into suspensions, for which the stability was investigated with respect to dissolution.
Synchrotron-based X-ray techniques are used increasingly to characterize actinide element speciation in heterogeneous media related to nuclear waste disposal safety. Especially techniques offering added temporal, spatial and energy resolved information are advancing our understanding of f-element physics and chemistry in general and of actinide element waste disposal in particular. Examples of investigations of uranium containing systems using both highly (energy) resolved X-ray emission spectroscopy (HRXES) techniques and spatially resolved techniques with focused X-ray beams are presented in this paper: polarization dependent partial fluorescence yield X-ray absorption near edge structure (PD-PFY-XANES) spectroscopic studies of a single Cs2UO2Cl4 crystal, which experimentally reveal a splitting of the σ, π, and δ components of the 6d valence states , and characterization of UO2/Mo thin films prepared on different substrates using a combination of techniques (2D and 3D micro- and nano-X-ray fluorescence, XANES and both holographic and ptychographic tomography).
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