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Performing elemental microanalysis with high accuracy and high precision by scanning electron microscopy/silicon drift detector energy-dispersive X-ray spectrometry (SEM/SDD-EDS).

Newbury DE, Ritchie NW - J Mater Sci (2014)

Bottom Line: SDD-EDS throughput, resolution, and stability provide practical operating conditions for measurement of high-count spectra that form the basis for peak fitting procedures that recover the characteristic peak intensities even for elemental combination where severe peak overlaps occur, such PbS, MoS2, BaTiO3, SrWO4, and WSi2.Accurate analyses are also demonstrated for interferences involving large concentration ratios: a major constituent on a minor constituent (Ba at 0.4299 mass fraction on Ti at 0.0180) and a major constituent on a trace constituent (Ba at 0.2194 on Ce at 0.00407; Si at 0.1145 on Ta at 0.0041).Measurement of trace constituents with limits of detection below 0.001 mass fraction (1000 ppm) is possible within a practical measurement time of 500 s.

View Article: PubMed Central - PubMed

Affiliation: Materials Measurement Science Division, National Institute of Standards and Technology, Gaithersburg, MD 20899 USA.

ABSTRACT

Electron-excited X-ray microanalysis performed in the scanning electron microscope with energy-dispersive X-ray spectrometry (EDS) is a core technique for characterization of the microstructure of materials. The recent advances in EDS performance with the silicon drift detector (SDD) enable accuracy and precision equivalent to that of the high spectral resolution wavelength-dispersive spectrometer employed on the electron probe microanalyzer platform. SDD-EDS throughput, resolution, and stability provide practical operating conditions for measurement of high-count spectra that form the basis for peak fitting procedures that recover the characteristic peak intensities even for elemental combination where severe peak overlaps occur, such PbS, MoS2, BaTiO3, SrWO4, and WSi2. Accurate analyses are also demonstrated for interferences involving large concentration ratios: a major constituent on a minor constituent (Ba at 0.4299 mass fraction on Ti at 0.0180) and a major constituent on a trace constituent (Ba at 0.2194 on Ce at 0.00407; Si at 0.1145 on Ta at 0.0041). Accurate analyses of low atomic number elements, C, N, O, and F, are demonstrated. Measurement of trace constituents with limits of detection below 0.001 mass fraction (1000 ppm) is possible within a practical measurement time of 500 s.

No MeSH data available.


Related in: MedlinePlus

SDD-EDS spectrum of the MoS2 with E0 = 10 keV (red); residual spectrum after MLLSQ peak fitting (blue) (Color figure online)
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Fig13: SDD-EDS spectrum of the MoS2 with E0 = 10 keV (red); residual spectrum after MLLSQ peak fitting (blue) (Color figure online)

Mentions: The SDD-EDS spectrum of MoS2 is shown in Fig. 13 along with the residual spectrum after fitting. The principal interferences are between the SKα (2.307 keV) and MoLα ((2.293 keV) with a separation of 14 eV; SKβ (2.468 keV) and MoLβ1 (2.395) with a separation of 73 eV; and SKβ (2.468 keV) and MoLβ2 (2.518 keV) with a separation of 50 eV.Fig. 13


Performing elemental microanalysis with high accuracy and high precision by scanning electron microscopy/silicon drift detector energy-dispersive X-ray spectrometry (SEM/SDD-EDS).

Newbury DE, Ritchie NW - J Mater Sci (2014)

SDD-EDS spectrum of the MoS2 with E0 = 10 keV (red); residual spectrum after MLLSQ peak fitting (blue) (Color figure online)
© Copyright Policy
Related In: Results  -  Collection

Show All Figures
getmorefigures.php?uid=PMC4555346&req=5

Fig13: SDD-EDS spectrum of the MoS2 with E0 = 10 keV (red); residual spectrum after MLLSQ peak fitting (blue) (Color figure online)
Mentions: The SDD-EDS spectrum of MoS2 is shown in Fig. 13 along with the residual spectrum after fitting. The principal interferences are between the SKα (2.307 keV) and MoLα ((2.293 keV) with a separation of 14 eV; SKβ (2.468 keV) and MoLβ1 (2.395) with a separation of 73 eV; and SKβ (2.468 keV) and MoLβ2 (2.518 keV) with a separation of 50 eV.Fig. 13

Bottom Line: SDD-EDS throughput, resolution, and stability provide practical operating conditions for measurement of high-count spectra that form the basis for peak fitting procedures that recover the characteristic peak intensities even for elemental combination where severe peak overlaps occur, such PbS, MoS2, BaTiO3, SrWO4, and WSi2.Accurate analyses are also demonstrated for interferences involving large concentration ratios: a major constituent on a minor constituent (Ba at 0.4299 mass fraction on Ti at 0.0180) and a major constituent on a trace constituent (Ba at 0.2194 on Ce at 0.00407; Si at 0.1145 on Ta at 0.0041).Measurement of trace constituents with limits of detection below 0.001 mass fraction (1000 ppm) is possible within a practical measurement time of 500 s.

View Article: PubMed Central - PubMed

Affiliation: Materials Measurement Science Division, National Institute of Standards and Technology, Gaithersburg, MD 20899 USA.

ABSTRACT

Electron-excited X-ray microanalysis performed in the scanning electron microscope with energy-dispersive X-ray spectrometry (EDS) is a core technique for characterization of the microstructure of materials. The recent advances in EDS performance with the silicon drift detector (SDD) enable accuracy and precision equivalent to that of the high spectral resolution wavelength-dispersive spectrometer employed on the electron probe microanalyzer platform. SDD-EDS throughput, resolution, and stability provide practical operating conditions for measurement of high-count spectra that form the basis for peak fitting procedures that recover the characteristic peak intensities even for elemental combination where severe peak overlaps occur, such PbS, MoS2, BaTiO3, SrWO4, and WSi2. Accurate analyses are also demonstrated for interferences involving large concentration ratios: a major constituent on a minor constituent (Ba at 0.4299 mass fraction on Ti at 0.0180) and a major constituent on a trace constituent (Ba at 0.2194 on Ce at 0.00407; Si at 0.1145 on Ta at 0.0041). Accurate analyses of low atomic number elements, C, N, O, and F, are demonstrated. Measurement of trace constituents with limits of detection below 0.001 mass fraction (1000 ppm) is possible within a practical measurement time of 500 s.

No MeSH data available.


Related in: MedlinePlus