Zitieren Sie bitte immer diesen URN: urn:nbn:de:kobv:b43-522284
Chemical in-depth analysis of (Ca/Sr)F2 core–shell like nanoparticles by X-ray photoelectron spectroscopy with tunable excitation energy
- The fluorolytic sol–gel synthesis is applied with the intention to obtain two different types of core–shell nanoparticles, namely, SrF2–CaF2 and CaF2–SrF2. In two separate fluorination steps for core and shell formation, the corresponding metal lactates are reacted with anhydrous HF in ethylene glycol. Scanning transmission electron microscopy (STEM) and dynamic light scattering (DLS) confirm the formation of particles with mean dimensions between 6.4 and 11.5 nm. The overall chemical composition of the particles during the different reaction steps is monitored by quantitative Al Kα excitation X-ray photoelectron spectroscopy (XPS). Here, the formation of stoichiometric metal fluorides (MF2) is confirmed, both for the core and the final core–shell particles. Furthermore, an in-depth analysis by synchrotron radiation XPS (SR-XPS) with tunable excitation energy is performed to confirm the core–Shell character of the nanoparticles. Additionally, Ca2p/Sr3d XPS intensity ratio in-DepthThe fluorolytic sol–gel synthesis is applied with the intention to obtain two different types of core–shell nanoparticles, namely, SrF2–CaF2 and CaF2–SrF2. In two separate fluorination steps for core and shell formation, the corresponding metal lactates are reacted with anhydrous HF in ethylene glycol. Scanning transmission electron microscopy (STEM) and dynamic light scattering (DLS) confirm the formation of particles with mean dimensions between 6.4 and 11.5 nm. The overall chemical composition of the particles during the different reaction steps is monitored by quantitative Al Kα excitation X-ray photoelectron spectroscopy (XPS). Here, the formation of stoichiometric metal fluorides (MF2) is confirmed, both for the core and the final core–shell particles. Furthermore, an in-depth analysis by synchrotron radiation XPS (SR-XPS) with tunable excitation energy is performed to confirm the core–Shell character of the nanoparticles. Additionally, Ca2p/Sr3d XPS intensity ratio in-Depth profiles are simulated using the software Simulation of Electron Spectra for Surface Analysis (SESSA). In principle, core–shell like particle morphologies are formed but without a sharp interface between calcium and strontium containing phases. Surprisingly, the in-depth chemical distribution of the two types of nanoparticles is equal within the error of the experiment. Both comprise a SrF2-rich core domain and CaF2-rich shell domain with an intermixing zone between them. Consequently, the internal morphology of the final nanoparticles seems to be independent from the synthesis chronology.…
Autor*innen: | Anja MüllerORCiD, T. Krahl, Jörg RadnikORCiD, Andreas Wagner, W. S. M. Werner, B. Ritter, E. Kemnitz, Wolfgang UngerORCiD |
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Dokumenttyp: | Zeitschriftenartikel |
Veröffentlichungsform: | Verlagsliteratur |
Sprache: | Englisch |
Titel des übergeordneten Werkes (Englisch): | Surface and Interface Analysis |
Jahr der Erstveröffentlichung: | 2021 |
Organisationseinheit der BAM: | 6 Materialchemie |
6 Materialchemie / 6.1 Oberflächen- und Dünnschichtanalyse | |
Veröffentlichende Institution: | Bundesanstalt für Materialforschung und -prüfung (BAM) |
Verlag: | Wiley VCH |
Jahrgang/Band: | 53 |
Ausgabe/Heft: | 5 |
Erste Seite: | 494 |
Letzte Seite: | 508 |
DDC-Klassifikation: | Naturwissenschaften und Mathematik / Chemie / Analytische Chemie |
Technik, Medizin, angewandte Wissenschaften / Ingenieurwissenschaften / Ingenieurwissenschaften und zugeordnete Tätigkeiten | |
Freie Schlagwörter: | Metal fluorides; Sol-gel synthesis; Synchrotron radiation; X-ray photoelectron spectroscopy |
Themenfelder/Aktivitätsfelder der BAM: | Chemie und Prozesstechnik |
Material | |
Material / Nano | |
DOI: | 10.1002/sia.6937 |
URN: | urn:nbn:de:kobv:b43-522284 |
ISSN: | 0142-2421 |
Verfügbarkeit des Dokuments: | Datei für die Öffentlichkeit verfügbar ("Open Access") |
Lizenz (Deutsch): | Creative Commons - CC BY-NC-ND - Namensnennung - Nicht kommerziell - Keine Bearbeitungen 4.0 International |
Datum der Freischaltung: | 10.03.2021 |
Referierte Publikation: | Ja |
Datum der Eintragung als referierte Publikation: | 10.03.2021 |
Schriftenreihen ohne Nummerierung: | Wissenschaftliche Artikel der BAM |