Abstract
The capabilities of field emitter electron microprobes to perform quantitative measurements at high spatial resolution are discussed. Using Fe-Cr-C particles in a bearing steel (SAE 52100) as example, a generic procedure was established to find the optimal analytical conditions (beam energy, beam current and acquisition time). The influence of these parameters on the accuracy, precision and spatial resolution was evaluated using experimental measurements and Monte Carlo simulations. A quantification procedure was developed for soft X-ray lines, taking into account the overlap of high order X-ray lines and background anomalies. The accuracy of Ka- and La-lines was verified using reference materials. A relationship between experimental and simulated X-ray intensities was determined to evaluate the measurement precision. The spatial resolution of each X-ray line was calculated from the simulated lateral and depth X-ray intensity distribution using simulations integrating experimentally measured beam diameters. The optimal analytical conditions for the studied sample were found to be 5 keV, 10 nA and 10 s acquisition time. Further specialized techniques to improve the spatial resolution are presented: focused ion beam preparation of thin lamella and wedge, and Monte Carlo based reconstruction. The feasibility of the latter to quantify features smaller than the X-ray emission volume was demonstrated.
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