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New approach on quantification of porosity of thin films via electron-excited X‑ray spectra

  • One of the crucial characteristics of functionalized thin films is their porosity (i.e., the ratio between the pore volume and the volume of the whole film). Due to the very low amount of material per coated area corresponding to thin films, it is a challenge for analytics to measure the film porosity. In this work, we present an Approach to determine the porosity of thin films by means of electron probe microanalysis (EPMA) either by wavelength-dispersive X-ray spectrometry (WDX) or by energy-dispersive X-ray spectrometry (EDX) with a scanning electron microscope (SEM). The procedure is based on the calculation of the film mass deposition from electron-excited X-ray spectra. The mass deposition is converted into film density by division of measured film thickness. Finally, the film porosity is calculated from the measured film density and the density of bulk, nonporous film material. The general applicability of the procedure to determine the porosity is demonstrated on thinOne of the crucial characteristics of functionalized thin films is their porosity (i.e., the ratio between the pore volume and the volume of the whole film). Due to the very low amount of material per coated area corresponding to thin films, it is a challenge for analytics to measure the film porosity. In this work, we present an Approach to determine the porosity of thin films by means of electron probe microanalysis (EPMA) either by wavelength-dispersive X-ray spectrometry (WDX) or by energy-dispersive X-ray spectrometry (EDX) with a scanning electron microscope (SEM). The procedure is based on the calculation of the film mass deposition from electron-excited X-ray spectra. The mass deposition is converted into film density by division of measured film thickness. Finally, the film porosity is calculated from the measured film density and the density of bulk, nonporous film material. The general applicability of the procedure to determine the porosity is demonstrated on thin templated mesoporous TiO₂ films, dip-coated on silicon wafer, with controlled porosity in the range of 15 to 50%. The high accuracy of the mass deposition as determined from X-ray spectra was validated with independent methods (ICP-OES and weighing). Furthermore, for the validation of the porosity results, ellipsometry, interference fringes method (IFM), and focused ion beam (FIB) cross sectioning were employed as independent techniques. Hence, the approach proposed in the present study is proven to be suited as a new analytical tool for accurate and relatively fast determination of the porosity of thin films.zeige mehrzeige weniger

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  • Ortel_et_al - AC_2016_PoroByEPMA.pdf
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  • SI_Ortel_et_al - AC2016.pdf
    eng

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Metadaten
Autor*innen:Erik Ortel, Andreas HertwigORCiD, D. Berger, P. Esposito, A. M. Rossi, R. Kraehnert, Vasile-Dan HodoroabaORCiD
Dokumenttyp:Zeitschriftenartikel
Veröffentlichungsform:Verlagsliteratur
Sprache:Englisch
Titel des übergeordneten Werkes (Englisch):Analytical Chemistry
Jahr der Erstveröffentlichung:2016
Herausgeber (Institution):American Chemical Society
Verlag:ACS Publications
Verlagsort:1155 Sixteenth Street N.W., Washington, DC 20036
Jahrgang/Band:88
Ausgabe/Heft:14
Erste Seite:7083
Letzte Seite:7090
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Freie Schlagwörter:Density; EDX; Mass deposition; Porosity; STRATAGem; Thin film; TiO2; X-rays
DOI:10.1021/acs.analchem.6b00847
URL:http://pubs.acs.org/doi/abs/10.1021/acs.analchem.6b00847
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:20.07.2016
Referierte Publikation:Ja
Datum der Eintragung als referierte Publikation:01.09.2016
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