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A multivariate statistical analysis method has been used to examine the information content of a series of EDX spectra acquired using a FEG‐STEM recorded across a segregated grain boundary in a ferritic steel. The spectra have been factored into a set of orthogonal information components (eigenspectra), each of which corresponds to an independent source of information. Two meaningful eigenspectra are identified: one is related to the segregation of P and Cr and the other to a combination of self‐absorption and coherent bremsstrahlung. Spectra are reconstructed from the meaningful eigenspectra to reduce noise and improve the sensitivity for detection of trace element segregation.

Zr alloys exhibit irradiation-induced growth and hardening which is associated with the defects and dislocation loops that form during irradiation. In this study, state-of-the-art in-situ synchrotron X-ray diffraction (SXRD) and transmission electron microscopy (TEM) techniques were used to investigate the stability of dislocation loops in two proton-irradiated Zr-Fe binary alloys in real time. Complementary data from both techniques show rapid annealing of a-loops occurs between 300°C and 450°C. Line profile analysis was performed on the SXRD patterns using the convoluted multiple whole profile analysis tool, to calculate the change in a-loop line density as a function of post-irradiation heat treatment temperature and time. At temperatures below 300°C, no significant decrease in a-loop density was detected when held for one hour at temperature. From this SXRD experiment, we calculate the effective activation energy for the annealing process as 0.46 eV. On-axis in-situ STEM imaging was used to directly observe a-loop mobility during heating cycles and confirm that a-loops begin to glide in the trace of the basal plane at ~200°C in a thin foil specimen. Such a-loop gliding events, leading to annihilation at the foil's surfaces, became more frequent between 300-450°C.