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 |
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description | •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. |
doi_str_mv | 10.1016/j.micron.2017.02.007 |
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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.</description><identifier>ISSN: 0968-4328</identifier><identifier>EISSN: 1878-4291</identifier><identifier>DOI: 10.1016/j.micron.2017.02.007</identifier><identifier>PMID: 28282549</identifier><language>eng</language><publisher>England: Elsevier Ltd</publisher><subject>Aluminium alloys ; Energy-dispersive X-ray spectroscopy ; Precipitation ; Scanning transmission electron microscopy</subject><ispartof>Micron (Oxford, England : 1993), 2017-05, Vol.96, p.103-111</ispartof><rights>2017 Elsevier Ltd</rights><rights>Copyright © 2017 Elsevier Ltd. All rights reserved.</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c474t-e9a85c4c725d861895e5383d9245f03d57fc4c0efdc779cfb5aa1971fff0a84a3</citedby><cites>FETCH-LOGICAL-c474t-e9a85c4c725d861895e5383d9245f03d57fc4c0efdc779cfb5aa1971fff0a84a3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://dx.doi.org/10.1016/j.micron.2017.02.007$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,780,784,3550,27924,27925,45995</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/28282549$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Wenner, Sigurd</creatorcontrib><creatorcontrib>Jones, Lewys</creatorcontrib><creatorcontrib>Marioara, Calin D.</creatorcontrib><creatorcontrib>Holmestad, Randi</creatorcontrib><title>Atomic-resolution chemical mapping of ordered precipitates in Al alloys using energy-dispersive X-ray spectroscopy</title><title>Micron (Oxford, England : 1993)</title><addtitle>Micron</addtitle><description>•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.</description><subject>Aluminium alloys</subject><subject>Energy-dispersive X-ray spectroscopy</subject><subject>Precipitation</subject><subject>Scanning transmission electron microscopy</subject><issn>0968-4328</issn><issn>1878-4291</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2017</creationdate><recordtype>article</recordtype><recordid>eNp9kEFv2yAUgNHUaUmz_YOq4tiLXbCxgUulqOq2SpF62aTdEIFHRmQbD-xI_vcjSrZjxQEe73vv6X0I3VFSUkLbx2PZexPDUFaE8pJUJSH8A1pTwUXBKklv0JrINr_rSqzQbUpHQghlLfmEVpXIp2FyjeJ2CrlPESGFbp58GLD5DflHd7jX4-iHAw4Oh2ghgsVjBONHP-kJEvYD3nZYd11YEp7TGYUB4mEprE8jxORPgH8VUS84h2aKIZkwLp_RR6e7BF-u9wb9_Pry4_l7sXv79vq83RWGcTYVILVoDDO8aqxoqZANNLWoraxY40htG-5yloCzhnNp3L7RmkpOnXNEC6brDXq49B1j-DNDmlTvk4Gu0wOEOalsqmWSckkzyi5oFppSBKfG6HsdF0WJOttWR3Wxrc62FalUtp3L7q8T5n0P9n_RP70ZeLoAkPc8eYgqGQ-DAeuzyEnZ4N-f8Bfm9pWO</recordid><startdate>201705</startdate><enddate>201705</enddate><creator>Wenner, Sigurd</creator><creator>Jones, Lewys</creator><creator>Marioara, Calin D.</creator><creator>Holmestad, Randi</creator><general>Elsevier Ltd</general><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7X8</scope></search><sort><creationdate>201705</creationdate><title>Atomic-resolution chemical mapping of ordered precipitates in Al alloys using energy-dispersive X-ray spectroscopy</title><author>Wenner, Sigurd ; Jones, Lewys ; Marioara, Calin D. ; Holmestad, Randi</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c474t-e9a85c4c725d861895e5383d9245f03d57fc4c0efdc779cfb5aa1971fff0a84a3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2017</creationdate><topic>Aluminium alloys</topic><topic>Energy-dispersive X-ray spectroscopy</topic><topic>Precipitation</topic><topic>Scanning transmission electron microscopy</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Wenner, Sigurd</creatorcontrib><creatorcontrib>Jones, Lewys</creatorcontrib><creatorcontrib>Marioara, Calin D.</creatorcontrib><creatorcontrib>Holmestad, Randi</creatorcontrib><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><jtitle>Micron (Oxford, England : 1993)</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Wenner, Sigurd</au><au>Jones, Lewys</au><au>Marioara, Calin D.</au><au>Holmestad, Randi</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Atomic-resolution chemical mapping of ordered precipitates in Al alloys using energy-dispersive X-ray spectroscopy</atitle><jtitle>Micron (Oxford, England : 1993)</jtitle><addtitle>Micron</addtitle><date>2017-05</date><risdate>2017</risdate><volume>96</volume><spage>103</spage><epage>111</epage><pages>103-111</pages><issn>0968-4328</issn><eissn>1878-4291</eissn><abstract>•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.</abstract><cop>England</cop><pub>Elsevier Ltd</pub><pmid>28282549</pmid><doi>10.1016/j.micron.2017.02.007</doi><tpages>9</tpages><oa>free_for_read</oa></addata></record> |
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subjects | Aluminium alloys Energy-dispersive X-ray spectroscopy Precipitation Scanning transmission electron microscopy |
title | Atomic-resolution chemical mapping of ordered precipitates in Al alloys using energy-dispersive X-ray spectroscopy |
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