Improved Sample Preparation for the Analysis of Nanoparticles by Electron Microscopy

  • Various promising sample preparation procedures aiming to avoid drying artifacts and guarantee homogeneously distributed NP samples for imaging techniques like TEM, SEM or AFM are presented. This involves retarded drying in an environment of high relative humidity as well as spin coating or freeze drying of the sample on the substrate. Depending on the type of the NPs, different techniques are successful in obtaining homogenous sample deposition. Simple drying at ambient conditions often results in heavily agglomerated NPs densely packed in coffee ring traces. Retardation of the drying speed in an environment of high relative humidity, however, yields homogeneous NP deposition in the case of bimodal SiO2 and bimodal gold NP’s. In contrast, a sample of bipyramidal TiO2, heavily agglomerated when commonly dried, is successfully dispersed by spin coating the suspension on the substrate. The analysis of the particle size distribution of the bimodal silica and gold samples yielded numberVarious promising sample preparation procedures aiming to avoid drying artifacts and guarantee homogeneously distributed NP samples for imaging techniques like TEM, SEM or AFM are presented. This involves retarded drying in an environment of high relative humidity as well as spin coating or freeze drying of the sample on the substrate. Depending on the type of the NPs, different techniques are successful in obtaining homogenous sample deposition. Simple drying at ambient conditions often results in heavily agglomerated NPs densely packed in coffee ring traces. Retardation of the drying speed in an environment of high relative humidity, however, yields homogeneous NP deposition in the case of bimodal SiO2 and bimodal gold NP’s. In contrast, a sample of bipyramidal TiO2, heavily agglomerated when commonly dried, is successfully dispersed by spin coating the suspension on the substrate. The analysis of the particle size distribution of the bimodal silica and gold samples yielded number ratios resembling the nominal number ratios. The reliable measurement of the NP concentration of polydisperse samples by electron microscopy, even if relative, is new and of special relevance because up to now only the size of the particles, i.e. the abscissa of the PSD, can be measured reliably.zeige mehrzeige weniger

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Metadaten
Autor*innen:Christoph Hörenz
Dokumenttyp:Vortrag
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2020
Organisationseinheit der BAM:6 Materialchemie
6 Materialchemie / 6.1 Oberflächen- und Dünnschichtanalyse
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Technik, Medizin, angewandte Wissenschaften / Ingenieurwissenschaften / Ingenieurwissenschaften und zugeordnete Tätigkeiten
Freie Schlagwörter:Electron microscopy; Nanoparticles; Particle size distribution; Sample peparation
Themenfelder/Aktivitätsfelder der BAM:Chemie und Prozesstechnik
Material
Material / Nano
Veranstaltung:EMPIR nPSize Training Course "Metrology for Measurement of Nanoparticle Size by Electron Microscopy and Atomic Force Microscopy"
Veranstaltungsort:Online meeting
Beginndatum der Veranstaltung:27.10.2020
Enddatum der Veranstaltung:27.10.2020
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:02.12.2020
Referierte Publikation:Nein
Eingeladener Vortrag:Nein
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