Atomic-resolution chemical mapping of ordered precipitates in Al alloys using energy-dispersive X-ray spectroscopy

•Beam-sensitive Al-alloy precipitates were chemically mapped with EDS.•Non-rigid registration was applied to correct for drift and scan distortions.•Chemical maps were achieved with atomic resolution and high signal-to-noise ratio.•Local elemental substitution was observed in single atomic columns....

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Veröffentlicht in:Micron (Oxford, England : 1993) England : 1993), 2017-05, Vol.96, p.103-111
Hauptverfasser: Wenner, Sigurd, Jones, Lewys, Marioara, Calin D., Holmestad, Randi
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Sprache:eng
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Zusammenfassung:•Beam-sensitive Al-alloy precipitates were chemically mapped with EDS.•Non-rigid registration was applied to correct for drift and scan distortions.•Chemical maps were achieved with atomic resolution and high signal-to-noise ratio.•Local elemental substitution was observed in single atomic columns. Scanning transmission electron microscopy (STEM) coupled with energy-dispersive X-ray spectroscopy (EDS) is a common technique for chemical mapping in thin samples. Obtaining high-resolution elemental maps in the STEM is jointly dependent on stepping the sharply focused electron probe in a precise raster, on collecting a significant number of characteristic X-rays over time, and on avoiding damage to the sample. In this work, 80kV aberration-corrected STEM-EDS mapping was performed on ordered precipitates in aluminium alloys. Probe and sample instability problems are handled by acquiring series of annular dark-field (ADF) images and simultaneous EDS volumes, which are aligned and non-rigidly registered after acquisition. The summed EDS volumes yield elemental maps of Al, Mg, Si, and Cu, with sufficient resolution and signal-to-noise ratio to determine the elemental species of each atomic column in a periodic structure, and in some cases the species of single atomic columns. Within the uncertainty of the technique, S and β” phases were found to have pure elemental atomic columns with compositions Al2CuMg and Al2Mg5Si4, respectively. The Q’ phase showed some variation in chemistry across a single precipitate, although the majority of unit cells had a composition Al6Mg6Si7.2Cu2.
ISSN:0968-4328
1878-4291
DOI:10.1016/j.micron.2017.02.007