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This paper presents a novel 3D method to correct for absorption in energy dispersive X-ray (EDX) microanalysis of heterogeneous samples of unknown structure and composition. By using STEM-based tomography coupled with EDX, an initial 3D reconstruction is used to extract the location of generated X-rays as well as the X-ray path through the sample to the surface. The absorption correction needed to retrieve the generated X-ray intensity is then calculated voxel-by-voxel estimating the different compositions encountered by the X-ray. The method is applied to a core/shell nanowire containing carbon and oxygen, two elements generating highly absorbed low energy X-rays. Absorption is shown to cause major reconstruction artefacts, in the form of an incomplete recovery of the oxide and an erroneous presence of carbon in the shell. By applying the correction method, these artefacts are greatly reduced. The accuracy of the method is assessed using reference X-ray lines with low absorption.

An enhanced method to quantify energy dispersive spectra recorded in 3D with a scanning electron microscope (3D SEM–EDS) has been previously demonstrated. This paper presents an extension of this method using all the available X-ray lines generated by the beam. The extended method benefits from using high energy lines, that are more accurately quantified, and from using soft X-rays that are highly absorbed and thus more surface sensitive. The data used to assess the method are acquired with a dual beam FIB/SEM investigating a multi-element Ni-based superalloy. A high accelerating voltage, needed to excite the highest energy X-ray line, results in two available X-ray lines for several elements. The method shows an improved compositional quantification as well as an improved spatial resolution., Highlights • 3D SEM–EDS mapping of structures smaller than the X-ray generation volume is considered. • The influence of neighbouring voxels is corrected by a recursive quantification method. • The method is improved using all available X-ray lines. • The method is applied to simulated spectra and experimental dual beam FIB/SEM data. • The method is shown to improve both compositional accuracy and spatial resolution.