Improving the accuracy of the sem-eds analysis of microparticle composition with reduced electron probe energy and surface smoothing with an ion beam

Abstract

The results of elemental analysis of the dioxide uranium bulk samples and microparticles of different sizes are collated. Analyses are performed with a scanning electron microscope equipped with an X-ray energy dispersive microanalyzer (INCA X-act, Oxford Instruments, United Kingdom). The concentrations were calculated using a preinstalled program for bulk samples based on the XPP Matrix Correction algorithm. Concentrations of uranium in bulk samples and in microparticles, which were measured at accelerating voltages 6–8 kV, are practically the same down to particle size of 0.5 µm if the analyzed surfaces have no evident roughness. It is shown that accuracy indicators can be significantly improved for the analysis of particles characterized by irregular shape and surface roughness, if their surfaces are smoothed previously by a focused ion beam. The uncertainty in determination the uranium concentration in dioxide uranium particles is reduced from 10% to 2% after smoothing of their surface by the ion beam.