New windowless EDS detectors designed specifically to collect low-energy X-rays (< 1 keV) and to work under ultra-low kV (< 3 kV) imaging conditions with the latest FE-SEMs offer new capabilities for elemental analysis. These capabilities include enhanced spatial resolution for the study of structures down to 10 nm or less, the characterization of surface features only 1-2 nm in thickness, the analysis of highly beam-sensitive or insulating materials, and much lower detection limits for light elements such as nitrogen and boron, as well as, for the first time, the detection of lithium. This offers an important breakthrough with potential for more detailed analysis of nano-materials, battery-and bio-materials, and semiconductors in the SEM.
We describe one approach to standardless quantification for energy-dispersive (ED) X-ray spectrometry that can achieved unnormalised results with an accuracy better than 5 %. This approach relies on a “factory” standards database, a model of the detector efficiency, calculated peak profiles, and a multi-step process to correct spectral artefacts and extract X-ray intensities from ED spectra. These processes and components, as well as the underlying equations involved in the quantification are detailed to illustrate the similarities between this approach and the classical standard-based k-ratio quantification. The accuracy was assessed by measuring and quantifying standard samples at different accelerating voltages (15 and 20 kV) and input count rates (50 and 200 kcps). In all cases, the measured, unnormalised concentrations yielded a centred distribution with a relative error less than 5 %. Excluding the analysis of light elements (B, C, O, N, F) improved the relative error to around 2 %
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