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Correlative analysis with electron microscopy applied in different operating modes (SEM, STEM-in-SEM and TEM) for the accurate morphological characterisation of non-spherical fine nanoparticles

  • Electron microscopy applied in different operating modes, e.g., SEM, TEM or STEM-in-SEM, is the gold standard method to investigate the exact size and shape of individual nanoparticles. However, when fine nanoparticles with a non-monodisperse size distribution and non-spherical shapes are analysed, achieving an accurate result is challenging. Deviations in size measurements of more than 10% may occur. Understanding of the contrasts and sensitivities characteristic to the individual operating modes of an electron microscope is key in interpreting and evaluating quantitatively the measurement uncertainties needed for an eventual certification of specific nanoparticles via traceable results. Further, beyond the pure measurement, the other components in the analysis workflow with significant impact on the overall measurement uncertainties are the sample preparation and the image segmentation. In the present study the same areas of selected iron oxide fine nanoparticles (<25 nm) asElectron microscopy applied in different operating modes, e.g., SEM, TEM or STEM-in-SEM, is the gold standard method to investigate the exact size and shape of individual nanoparticles. However, when fine nanoparticles with a non-monodisperse size distribution and non-spherical shapes are analysed, achieving an accurate result is challenging. Deviations in size measurements of more than 10% may occur. Understanding of the contrasts and sensitivities characteristic to the individual operating modes of an electron microscope is key in interpreting and evaluating quantitatively the measurement uncertainties needed for an eventual certification of specific nanoparticles via traceable results. Further, beyond the pure measurement, the other components in the analysis workflow with significant impact on the overall measurement uncertainties are the sample preparation and the image segmentation. In the present study the same areas of selected iron oxide fine nanoparticles (<25 nm) as reference nanomaterial (candidate) prepared on substrate for electron microscopy imaging are analysed correlatively with SEM, STEM-in-SEM and TEM with respect to their size and shape distribution. Individual significant measurement uncertainties are discussed, e.g., the sensitivity of secondary electron detectors of InLens-type to the surface morphology, particularly to the presence of an ultrathin organic coating or signal saturation effects on the particle edges, to electron beam exposure, to surface contamination, or the selection of the threshold for image segmentation. Another goal of this study is to establish a basis of analysis conditions which shall guarantee accurate results when both manual and particularly (semi-)automated segmentation approaches are applied. Advantages as well as limitations of the use of different electron microscopy operating modes, applied individually and correlatively, are highlighted.zeige mehrzeige weniger

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Metadaten
Autor*innen:Paul MrkwitschkaORCiD
Koautor*innen:Sarah-Luise Abram, Bastian Rühle, Vasile-Dan Hodoroaba
Dokumenttyp:Vortrag
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2024
Organisationseinheit der BAM:1 Analytische Chemie; Referenzmaterialien
1 Analytische Chemie; Referenzmaterialien / 1.0 Abteilungsleitung und andere
1 Analytische Chemie; Referenzmaterialien / 1.2 Biophotonik
6 Materialchemie
6 Materialchemie / 6.1 Oberflächen- und Dünnschichtanalyse
DDC-Klassifikation:Technik, Medizin, angewandte Wissenschaften / Ingenieurwissenschaften / Angewandte Physik
Freie Schlagwörter:Electron Microscopy; Imaging; Metrology; Nanoparticles; Reference materials
Themenfelder/Aktivitätsfelder der BAM:Material
Material / Nano
Veranstaltung:E-MRS 2024 Spring Meeting
Veranstaltungsort:Strasbourg, France
Beginndatum der Veranstaltung:27.05.2024
Enddatum der Veranstaltung:31.05.2024
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:01.07.2024
Referierte Publikation:Nein
Eingeladener Vortrag:Nein
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