Enhanced Quantification for 3D Energy Dispersive Spectrometry: Going Beyond the Limitation of Large Volume of X-Ray Emission

Burdet, Pierre; Hébert, C.; Cantoni, Marco

doi:10.1017/s1431927614001688

Cited by 4 publications

(5 citation statements)

References 18 publications

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“…The system is ambiguous and convergence to a local minimum is likely. In [14] , the most unfavourable cases are avoided by grouping layers of similar composition together. The situation is improved, but inaccurate solutions still lead to an artefact of over-correction, as observed with simulated data ( Fig.…”

Section: Discussionmentioning

confidence: 99%

“…Described in [14] , the enhanced quantification for 3D EDS–SEM is revisited and augmented here. The standard quantification, called here bulk quantification, is first considered.…”

Section: Calculationmentioning

confidence: 99%

“…The mapping needs to contain information in all three dimensions and especially in the depth direction, the primary direction of the incident high energy electrons and thus the direction of the broadest X-ray distribution. Using 3D SEM–EDS data, a quantification method was developed for heterogeneous samples of unknown microstructure [14] . Called enhanced quantification, this method corrects the influence of the neighbouring voxel, applying recursively the XPP- φ ( ρz ) thin film quantification [10] .…”

Section: Introductionmentioning

confidence: 99%

“…The present work introduces a new version of the enhanced quantification for 3D SEM–EDS data proposed in [14] . This method is improved to take advantage of all available X-ray lines, benefiting from the higher quantification accuracy of the high energy X-ray lines and the improved spatial resolution of the low energy X-ray lines.…”

Section: Introductionmentioning

confidence: 99%

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Enhanced quantification for 3D SEM–EDS: Using the full set of available X-ray lines

2015

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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.

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Section: Discussionmentioning

confidence: 99%

“…Described in [14] , the enhanced quantification for 3D EDS–SEM is revisited and augmented here. The standard quantification, called here bulk quantification, is first considered.…”

Section: Calculationmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Enhanced quantification for 3D SEM–EDS: Using the full set of available X-ray lines

2015

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“…Indeed, by FIB thinning the samples and analyzing them at high voltages using a FEG-EPMA, Kubo et al (2013) demonstrated a spatial resolution in the range 40–200 nm for an InGaP/GaAs thin sample, with detection limits of 1,000–10,000 ppm and signal-to-noise ratio 13 times higher than that of a STEM-EDS system (on bulk samples such detection limits would be 2 to 3 orders of magnitude lower). Worth mentioning is also the development of three-dimensional microanalysis in dual-beam instruments (i.e., SEM equipped with both EDS and FIB), which will require more sophisticated quantification methods such as the one recently developed by Burdet et al (2014).…”

Section: A Look Into the Futurementioning

confidence: 99%

Electron Probe Microanalysis: A Review of the Past, Present, and Future

Rinaldi

Llovet

2015

Microsc Microanal

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The 50th anniversary of the application of electron probe microanalysis (EPMA) to the Earth Sciences provides an opportunity for an assessment of the state-of-the-art of the technique. Stemming from the introduction of the first automated instruments, the latest developments of EPMA and some typical applications are reviewed with an eye to the future. The most noticeable recent technical achievements such as the field-emission electron gun, the latest generation of energy and wavelength dispersive spectrometers, and the development of analytical methods based on new sets of first principle data obtained by the use of sophisticated computer codes, allow for the extension of the method to the analysis of trace elements, ultra-light elements (down to Li), small particles, and thin films, with a high degree of accuracy and precision and within a considerably reduced volume of interaction. A number of working examples and a thorough list of references provide the reader with a working knowledge of the capabilities and limitations of EPMA today.

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A novel 3D absorption correction method for quantitative EDX-STEM tomography

et al. 2016

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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.

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Enhanced Quantification for 3D Energy Dispersive Spectrometry: Going Beyond the Limitation of Large Volume of X-Ray Emission

Cited by 4 publications

References 18 publications

Enhanced quantification for 3D SEM–EDS: Using the full set of available X-ray lines

Enhanced quantification for 3D SEM–EDS: Using the full set of available X-ray lines

Electron Probe Microanalysis: A Review of the Past, Present, and Future

A novel 3D absorption correction method for quantitative EDX-STEM tomography

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