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Methodology for the identification of carbonyl absorption maxima of carbon surface oxides in DRIFT spectra

Herold, Felix ; Leubner, Oliver ; Jeschonek, Katharina ; Hess, Christian ; Drochner, Alfons ; Qi, Wei ; Etzold, Bastian J.M. (2024)
Methodology for the identification of carbonyl absorption maxima of carbon surface oxides in DRIFT spectra.
In: Carbon Trends, 2021, 3
doi: 10.26083/tuprints-00026760
Artikel, Zweitveröffentlichung, Verlagsversion

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Kurzbeschreibung (Abstract)

Carbon surface oxides have been demonstrated to be crucial for high performing carbon materials in various applications. Diffuse reflectance infrared Fourier transform spectroscopy represents a powerful time-resolved method to study the surfaces of functional materials under process conditions. Due to the severe overlap of the contributions of individual surface groups in combination with compared to organic molecules shifted absorption maxima meaningful analysis remains challenging. Especially due to the unknown maxima, deconvolution of the superimposed bands is strongly hindered. In this study, we developed a procedure based on hydrolysis, thermal annealing or a combination thereof, which allows to disentangle carbonyl absorption maxima of carboxylic acids, anhydrides and lactones on carbon surfaces. In order to verify the proposed transformations, thorough characterization by temperature programmed desorption, X-ray photoelectron spectroscopy, potentiometric titration and Boehm titration was carried out. Applying this procedure for a polymer derived reference material, the carbonyl absorption maximum could be deduced, which are positioned for lactones at 1771 cm⁻¹, for carboxylic acids between 1753 cm⁻¹ and 1760 cm⁻¹, and for carboxylic anhydrides at 1792 cm⁻¹ and 1852 cm⁻¹. This allowed deconvolution of the carbonyl band, paving the way for in situ time-resolved analyses.

Typ des Eintrags: Artikel
Erschienen: 2024
Autor(en): Herold, Felix ; Leubner, Oliver ; Jeschonek, Katharina ; Hess, Christian ; Drochner, Alfons ; Qi, Wei ; Etzold, Bastian J.M.
Art des Eintrags: Zweitveröffentlichung
Titel: Methodology for the identification of carbonyl absorption maxima of carbon surface oxides in DRIFT spectra
Sprache: Englisch
Publikationsjahr: 24 April 2024
Ort: Darmstadt
Publikationsdatum der Erstveröffentlichung: 2021
Ort der Erstveröffentlichung: Amsterdam
Verlag: Elsevier
Titel der Zeitschrift, Zeitung oder Schriftenreihe: Carbon Trends
Jahrgang/Volume einer Zeitschrift: 3
Kollation: 13 Seiten
DOI: 10.26083/tuprints-00026760
URL / URN: https://tuprints.ulb.tu-darmstadt.de/26760
Zugehörige Links:
Herkunft: Zweitveröffentlichungsservice
Kurzbeschreibung (Abstract):

Carbon surface oxides have been demonstrated to be crucial for high performing carbon materials in various applications. Diffuse reflectance infrared Fourier transform spectroscopy represents a powerful time-resolved method to study the surfaces of functional materials under process conditions. Due to the severe overlap of the contributions of individual surface groups in combination with compared to organic molecules shifted absorption maxima meaningful analysis remains challenging. Especially due to the unknown maxima, deconvolution of the superimposed bands is strongly hindered. In this study, we developed a procedure based on hydrolysis, thermal annealing or a combination thereof, which allows to disentangle carbonyl absorption maxima of carboxylic acids, anhydrides and lactones on carbon surfaces. In order to verify the proposed transformations, thorough characterization by temperature programmed desorption, X-ray photoelectron spectroscopy, potentiometric titration and Boehm titration was carried out. Applying this procedure for a polymer derived reference material, the carbonyl absorption maximum could be deduced, which are positioned for lactones at 1771 cm⁻¹, for carboxylic acids between 1753 cm⁻¹ and 1760 cm⁻¹, and for carboxylic anhydrides at 1792 cm⁻¹ and 1852 cm⁻¹. This allowed deconvolution of the carbonyl band, paving the way for in situ time-resolved analyses.

Freie Schlagworte: Oxygen surface groups on carbon, Selective surface functionalization, DRIFTS, TPD
ID-Nummer: Artikel-ID: 100020
Status: Verlagsversion
URN: urn:nbn:de:tuda-tuprints-267603
Sachgruppe der Dewey Dezimalklassifikatin (DDC): 500 Naturwissenschaften und Mathematik > 540 Chemie
Fachbereich(e)/-gebiet(e): 07 Fachbereich Chemie
07 Fachbereich Chemie > Ernst-Berl-Institut
07 Fachbereich Chemie > Eduard Zintl-Institut
07 Fachbereich Chemie > Eduard Zintl-Institut > Fachgebiet Physikalische Chemie
07 Fachbereich Chemie > Ernst-Berl-Institut > Fachgebiet Technische Chemie
07 Fachbereich Chemie > Ernst-Berl-Institut > Fachgebiet Technische Chemie > Technische Chemie I
Hinterlegungsdatum: 24 Apr 2024 12:30
Letzte Änderung: 25 Apr 2024 07:50
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