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

• Published in: Journal of materials science 2015-01, Vol.50 (2), p.493-518
• Main Authors: Newbury, Dale E., Ritchie, Nicholas W. M.
• Format: Article
• Language: English
• Subjects: Atomic properties; barium; Barium titanates; Characterization and Evaluation of Materials; Chemistry and Materials Science; Classical Mechanics; Constituents; Crystallography and Scattering Methods; detection limit; Detectors; Drift; Electron microscopes; Electron microscopy; Electron probes; Energy dispersive X ray spectroscopy; energy-dispersive X-ray analysis; Materials Science; microstructure; Molybdenum disulfide; Polymer Sciences; Review; scanning electron microscopes; Scanning electron microscopy; Scientific imaging; Silicon; Solid Mechanics; Spectral resolution; Spectrometry; Spectroscopy; X-radiation; X-ray spectroscopy; X-rays
• ISSN: 0022-2461; 1573-4803
• DOI: 10.1007/s10853-014-8685-2

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, MoS 2 , BaTiO 3 , SrWO 4 , and WSi 2 . 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.