Journal
MICROSCOPY AND MICROANALYSIS
Volume 21, Issue 5, Pages 1327-1340Publisher
CAMBRIDGE UNIV PRESS
DOI: 10.1017/S1431927615014993
Keywords
energy-dispersive X-ray spectrometry; scanning electron microscopy; quantitative X-ray microanalysis; low atomic number elements
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A scanning electron microscope with a silicon drift detector energy-dispersive X-ray spectrometer (SEM/SDD-EDS) was used to analyze materials containing the low atomic number elements B, C, N, O, and F achieving a high degree of accuracy. Nearly all results fell well within an uncertainty envelope of +/- 5% relative (where relative uncertainty (%)=[(measured-ideal)/ideal]x100%). Quantification was performed with the standards-based k-ratio method with matrix corrections calculated based on the Pouchou and Pichoir expression for the ionization depth distribution function, as implemented in the NIST DTSA-II EDS software platform. The analytical strategy that was followed involved collection of high count (>2.5 million counts from 100 eV to the incident beam energy) spectra measured with a conservative input count rate that restricted the deadtime to similar to 10% to minimize coincidence effects. Standards employed included pure elements and simple compounds. A 10 keV beam was employed to excite the K- and L-shell X-rays of intermediate and high atomic number elements with excitation energies above 3 keV, e.g., the Fe K-family, while a 5 keV beam was used for analyses of elements with excitation energies below 3 keV, e.g., the Mo L-family.
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