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Analysis of Fluorine Traces in TiO2 Nanoplatelets by SEM/EDX, AES and TOF-SIMS

  • The synthesis of TiO2 nanoplatelets with fluorine-containing reactants is carried out using Ti (IV) butoxide as precursor and concentrated HF as shape controller, the final product requires a working up in order to eliminate or at least to reduce the amount of residual fluorides, which is realized here by well-defined thermal treatment. Qualitative investigation of the bulk elemental composition by means of EDX of TiO2 nanoparticles (NPs) has identified fluorine in case of the as-synthesized samples. EDX spectra of thermally treated products exhibit either a fluorine content close to the limit of detection. The latter holds also true for the reference sample, TiO2 NPs of bipyramidal shape and prepared by a different synthesis route. For differentiation whether fluorine is present in the bulk or at the surface of the TiO2 nanoplatelets, top-surface sensitive AES and ToF-SIMS has been applied. Secondary ions of fluorine are detected in ToF-SIMS spectra of all samples, but could beThe synthesis of TiO2 nanoplatelets with fluorine-containing reactants is carried out using Ti (IV) butoxide as precursor and concentrated HF as shape controller, the final product requires a working up in order to eliminate or at least to reduce the amount of residual fluorides, which is realized here by well-defined thermal treatment. Qualitative investigation of the bulk elemental composition by means of EDX of TiO2 nanoparticles (NPs) has identified fluorine in case of the as-synthesized samples. EDX spectra of thermally treated products exhibit either a fluorine content close to the limit of detection. The latter holds also true for the reference sample, TiO2 NPs of bipyramidal shape and prepared by a different synthesis route. For differentiation whether fluorine is present in the bulk or at the surface of the TiO2 nanoplatelets, top-surface sensitive AES and ToF-SIMS has been applied. Secondary ions of fluorine are detected in ToF-SIMS spectra of all samples, but could be roughly quantified by measurement of same reference sample as for EDX, namely TiO2 nano-bipyramids. This revealed that the amount of fluorine within1 nm depth beneath the surface is reduced in the thermally treated specimen compared to the raw product down to a content about as low as in the reference sample. AES allows analyzing analysis of the first few nanometers from the top-surface of individual NPs by point analysis. An F KLL peak has been detected at the surface of samples of as-prepared TiO2 nanoplatelets under optimized measurement conditions, but was not detectable after their calcination, which is in agreement with ToF-SIMS results. Moreover, high resolution AES on single TiO2 nanoplatelets elucidated that the surface atomic layers surrounding the TiO2 nanopaltelet contain fluorides before thermal treatment of the NPs.zeige mehrzeige weniger

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  • Analysis of Fluorine Traces in TiO2 Nanoplatelets by SEM/EDX, AES and TOF-SIMS
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Metadaten
Autor*innen:Vasile-Dan HodoroabaORCiD
Koautor*innen:Steffi Rades, Thomas Wirth, Markus Holzweber, F. Pellegrino, G. Martra
Dokumenttyp:Posterpräsentation
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2017
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Freie Schlagwörter:Auger Electron Spectroscopy; Fluorine; Nanoparticles; Nanoplatelets; SEM/EDX; Titania
Veranstaltung:17th European Conference on Applications of Surface and Interface Analysis ECASIA 2017
Veranstaltungsort:Montpellier, France
Beginndatum der Veranstaltung:24.09.2017
Enddatum der Veranstaltung:29.09.2017
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:06.11.2017
Referierte Publikation:Nein
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