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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.


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SDD-EDS spectrum of BaTiO3 at a beam energy of E0 = 10 keV (red); residual spectrum (blue) after peak fitting with Ti and BaSi2O5 (sanbornite) (Color figure online)
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Fig14: SDD-EDS spectrum of BaTiO3 at a beam energy of E0 = 10 keV (red); residual spectrum (blue) after peak fitting with Ti and BaSi2O5 (sanbornite) (Color figure online)

Mentions: The spectrum of BaTiO3 at E0 = 10 keV is shown in Fig. 14 along with the residual spectrum after peak fitting with BaSi2O5 (the mineral sanbornite) and Ti. The principal peak interferences are BaLα (4.467 keV) and TiKα (4.508 keV): 41 eV separation, and BaLβ3 (4.927 keV) and TiKβ (4.931 keV): 4 eV separation. The analytical results (atomic concentrations) for 15 locations are presented in Table 8, along with a single analyzed location (mass concentration) and the components of the error budget.Fig. 14


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 BaTiO3 at a beam energy of E0 = 10 keV (red); residual spectrum (blue) after peak fitting with Ti and BaSi2O5 (sanbornite) (Color figure online)
© Copyright Policy
Related In: Results  -  Collection

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

Fig14: SDD-EDS spectrum of BaTiO3 at a beam energy of E0 = 10 keV (red); residual spectrum (blue) after peak fitting with Ti and BaSi2O5 (sanbornite) (Color figure online)
Mentions: The spectrum of BaTiO3 at E0 = 10 keV is shown in Fig. 14 along with the residual spectrum after peak fitting with BaSi2O5 (the mineral sanbornite) and Ti. The principal peak interferences are BaLα (4.467 keV) and TiKα (4.508 keV): 41 eV separation, and BaLβ3 (4.927 keV) and TiKβ (4.931 keV): 4 eV separation. The analytical results (atomic concentrations) for 15 locations are presented in Table 8, along with a single analyzed location (mass concentration) and the components of the error budget.Fig. 14

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