Intensity Measurement of Wavelength Dispersive X-Ray Emission Bands: Applications to the Soft X-Ray Region

Rémond, G.; Gilles, C.; Fialin, Michel; Rouer, Olivier; Marinenko, Ryna B.; Myklebust, Robert L.; Newbury, D. E.

doi:10.1007/978-3-7091-6555-3_4

Cited by 8 publications

(14 citation statements)

References 14 publications

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“…4.4. Chemical bonding X-ray emission lines that correspond to electron transitions involving outer valence electrons are known to be sensitive to chemical bond [24]. As a result, a shift in peak position as well as a change in peak distribution is observed when comparing X-ray lines of the same element in different chemical environments.…”

Section: Limitations Of Quantitative Proceduresmentioning

confidence: 99%

Uncertainty and capability of quantitative EPMA at low voltage – A review

Merlet

Llovet

2012

IOP Conf. Ser.: Mater. Sci. Eng.

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The use of electron probe microanalysis (EPMA) at low voltage allows improvements in the lateral resolution and surface sensitivity of the technique down to the sub-micrometre scale, and it is also useful in minimizing X-ray absorption (for the analysis of ultra-light elements), charging effects and secondary fluorescence. However, EPMA at low voltage is accompanied by a number of problems which may affect the accuracy of quantitative results. A large number of these problems arise from the need of using low-energy X-ray lines such as Land M-lines, which have low fluorescence yields, large uncertainties in the mass attenuation coefficients, and are affected by several spectroscopic difficulties (e.g., peak shifts and overlaps). Other factors that play an important role at low voltage are carbon contamination, surface oxidation, the quality of sample polishing, the influence of a conductive coating and the limitations of matrix correction procedures. In this paper, we illustrate the capabilities of EPMA at low voltage and we examine in detail the different sources of uncertainty that may affect the accuracy of quantitative results.

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Section: Limitations Of Quantitative Proceduresmentioning

confidence: 99%

Uncertainty and capability of quantitative EPMA at low voltage – A review

Merlet

Llovet

2012

IOP Conf. Ser.: Mater. Sci. Eng.

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“…In practice, only the convolution of these features with the spectral window (or energy response function) of the spectrometer will be seen. Thus the ability to observe the non-diagram satellite bands will depend on the resolution and sensitivity of the spectrometer as reported by Rémond et al [ 4 , 18 ] and Fialin et al [ 2 , 3 ] for x-ray emission spectra measured with EPMA’s equipped with WDS.…”

Section: Contributions Of X-ray Generation Mechanisms and Of Instrmentioning

confidence: 99%

“…In previous studies, Rémond et al [ 4 , 18 ] added Gaussian or pseudo-Voigt (equation [ 17 ] offsets to the main profiles to describe the high energy tail of x-ray emission peaks occurring at low Bragg angles. This approach based on the addition of high energy offsets, is supported by the results by Cauchois and Bonnelle [ 19 ] who showed that the asymmetrical diffraction pattern for a bent monochromator can be approximated by a sum of adjacent rectangular Darwin curves with decreasing amplitudes.…”

Section: Applications Of Least-square Fitting Techniques To Wds Spmentioning

confidence: 99%

“…In practice, specific calibration curves of peak widths as a function of wavelength must be obtained for emission lines belonging to the K, L, or M series since these lines of similar energy do not only exhibit shape changes but also have different peak widths [ 4 ]. These variations account for the contribution of the natural width to the observed peak width.…”

Section: Applications Of Least-square Fitting Techniques To Wds Spmentioning

confidence: 99%

“…A symmetrical peak never exists even for the case of atomic lines resulting from radiative transitions involving only core levels because of the presence of high and low energy satellites and instrumental distortions induced during measurement. While the approximation of the peak height for the x-ray intensity measurement remains valid in most analytical problems with the EPMA, this simplified approach is no longer sufficient in the presence of severe peak overlaps as is the case for L emission spectra of rare-earth elements [ 1 ] or when soft x-ray emissions are used in the analytical procedure [ 2 – 4 ].…”

Section: Introductionmentioning

confidence: 99%

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Decomposition of wavelength dispersive x-ray spectra

Rémond¹,

Myklebust²,

Fialin³

et al. 2002

J. Res. Natl. Inst. Stand. Technol.

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Line shapes of atomic lines and soft x-ray emission bands measured with a wavelength dispersive spectrometer (WDS) with the Electron Probe Micro Analyzer (EPMA) are reviewed. Least square fitting to pseudo-Voigt profiles of the digitally measured spectra are used to account for the presence of non-diagram features (high and low energy satellites) and instrumental induced distortions. The effect of line width and relative intensities on the quality of fits is illustrated. Spectral distortions resulting from the presence of absorption edges within the analyzed wavelength region are illustrated for the case of FeLα,β emission bands for pure Fe and iron oxides. For quantitative analysis, an analytical approach is presented where the measured soft x-ray emission bands are corrected for self absorption before extracting the intensities from the experimental data.

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Electron Probe Microanalysis of Ni Silicides Using Ni-L X-Ray Lines

et al. 2016

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We report electron probe microanalysis measurements on nickel silicides, Ni5Si2, Ni2Si, Ni3Si2, and NiSi, which were done in order to investigate anomalies that affect the analysis of such materials by using the Ni L3-M4,5 line (Lα). Possible sources of systematic discrepancies between experimental data and theoretical predictions of Ni L3-M4,5 k-ratios are examined, and special attention is paid to dependence of the Ni L3-M4,5 k-ratios on mass-attenuation coefficients and partial fluorescence yields. Self-absorption X-ray spectra and empirical mass-attenuation coefficients were obtained for the considered materials from X-ray emission spectra and relative X-ray intensity measurements, respectively. It is shown that calculated k-ratios with empirical mass attenuation coefficients and modified partial fluorescence yields give better agreement with experimental data, except at very low accelerating voltages. Alternatively, satisfactory agreement is also achieved by using the Ni L3-M1 line (Lℓ) instead of the Ni L3-M4,5 line.

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Intensity Measurement of Wavelength Dispersive X-Ray Emission Bands: Applications to the Soft X-Ray Region

Cited by 8 publications

References 14 publications

Uncertainty and capability of quantitative EPMA at low voltage – A review

Uncertainty and capability of quantitative EPMA at low voltage – A review

Decomposition of wavelength dispersive x-ray spectra

Electron Probe Microanalysis of Ni Silicides Using Ni-L X-Ray Lines

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