QUANTITATIVE X-RAY FLUORESCENCE DETERMINATION OF ELEMENTAL COMPOSITION OF MICRO-CONSTITUENTS SMALLER THAN THE ELECTRON PROBE VOLUME

摘要

Often referred to as SEM-EDX, energy-dispersive spectroscopic analysis of characteristic fluorescence x-ray is a standard technique for semi-quantitative elemental composition analysis in scanning electron microscopy. It is quick and extremely useful for identification of phases in the sample microstructure, as long as the constituents are significantly larger than the probe volume from which the fluorescence x-rays originate. The probe volume ranges from a few to several microns, depending on the electron beam spot size and the acceleration voltage. We report on a new variant of an EDX technique developed to overcome this limitation and allow quantitative elemental analysis of smaller phase constituents, down to a size of several nanometers. This variant involves the calculation of compositions of individual phases from multiple analyses of areas containing phases of interest. This significantly increases the usefulness of EDX for quantitative analysis of new nano-structured materials.