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Comprehensive characterization of Al-coated titania nanoparticles with electron microscopy and surface chemical analytics

  • The wide use of nanoforms with at least one dimension below 100 nm in our daily life requires a detailed knowledge of their physicochemical properties which are needed for risk assessment or quality control. Therefore, a comprehensive characterization of these properties was considered as relevant including: chemical composition, crystallinity, particle size, particle shape, surface chemistry, and specific surface area (SSA). We want to discuss, how Scanning Electron Microscopy (SEM), Electron Probe Microanalysis (EPMA) in the version with energy dispersive X-ray spectroscopy (EDS), Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and X-ray Photoelectron Spectroscopy (XPS) can contribute to gain comprehensive insights into the nature of the nanoparticles. SEM results provide the particle size and shape (distribution). A quick identification of the main chemical elements present in the sample can be obtained with EDS, whereas XPS allows a more detailed chemical identificationThe wide use of nanoforms with at least one dimension below 100 nm in our daily life requires a detailed knowledge of their physicochemical properties which are needed for risk assessment or quality control. Therefore, a comprehensive characterization of these properties was considered as relevant including: chemical composition, crystallinity, particle size, particle shape, surface chemistry, and specific surface area (SSA). We want to discuss, how Scanning Electron Microscopy (SEM), Electron Probe Microanalysis (EPMA) in the version with energy dispersive X-ray spectroscopy (EDS), Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and X-ray Photoelectron Spectroscopy (XPS) can contribute to gain comprehensive insights into the nature of the nanoparticles. SEM results provide the particle size and shape (distribution). A quick identification of the main chemical elements present in the sample can be obtained with EDS, whereas XPS allows a more detailed chemical identification of the small nanoparticles below 20 nm or of the near-surface region of larger particles. ToF-SIMS is even much more surface-sensitive and leads to a deeper understanding of the surface chemistry of the nanoparticles. As exemplary samples, two Al-coated TiO2 samples in nanopowder form were chosen from the JRC repository, capped either with a hydrophilic or a hydrophobic organic shell. A focus of our case study was to show, how reliable, reproducible and traceable data can be obtained. Therefore, each step in the workflow of sample investigation must be described in detail. For the most of these steps, well-established standards are available. Usually, the conditions of the particular measurements with each analysis method are saved as meta-data in the common file formats. But other factors like sample preparation and data reduction approaches may influence the result of the investigations in a significant manner and must be described often in a separate file (as a protocol) together with the data file. For sensitive materials like nanoobjects, the preparation of the sample influences the results crucially, e.g. measured as suspension or as powders. Furthermore, data reduction like selection of relevant peaks in spectra or particles in images, background subtraction, peak deconvolution, models for the quantification of the spectra must be considered in the interpretation of the results ideally with associated individual measurement uncertainties. Only a detailed description of all these factors allows to obtain a comprehensive characterization with reliable, reproduceable and traceable data. Examples of standardized procedures of measurement or on data reduction will be highlighted. We thank for the funding from the European Unions’s Horizon 2020 for the project NanoSolveIt (grant agreement No. 814572) and for the project NANORIGO (grant agreement No. 814530).zeige mehrzeige weniger

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Metadaten
Autor*innen:Jörg RadnikORCiD
Koautor*innen:R. Kersting, B. Hagenhoff, Francesca Bennett, Dmitri Ciornii, Vasile-Dan Hodoroaba
Dokumenttyp:Vortrag
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2021
Organisationseinheit der BAM:6 Materialchemie
6 Materialchemie / 6.1 Oberflächen- und Dünnschichtanalyse
Veröffentlichende Institution:Bundesanstalt für Materialforschung und -prüfung (BAM)
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Technik, Medizin, angewandte Wissenschaften / Ingenieurwissenschaften / Ingenieurwissenschaften und zugeordnete Tätigkeiten
Freie Schlagwörter:Energy dispersive X-ray spectroscopy; Scanning Electron Microscopy; Time-of-Flight Secondary Ion Mass Spectrometry; Titania nanoparticles; X-ray Photoelectron Spectroscopy
Themenfelder/Aktivitätsfelder der BAM:Chemie und Prozesstechnik
Material
Material / Nano
Veranstaltung:E-MRS Spring Meeting
Veranstaltungsort:Online meeting
Beginndatum der Veranstaltung:31.05.2021
Enddatum der Veranstaltung:03.06.2021
URN:urn:nbn:de:kobv:b43-527486
Verfügbarkeit des Dokuments:Datei für die Öffentlichkeit verfügbar ("Open Access")
Lizenz (Deutsch):License LogoCreative Commons - CC BY-NC-SA - Namensnennung - Nicht kommerziell - Weitergabe unter gleichen Bedingungen 4.0 International
Datum der Freischaltung:03.06.2021
Referierte Publikation:Nein
Eingeladener Vortrag:Nein
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