Standardized Chemical Composition Analysis of Graphene Oxide Flakes with SEM/EDS and XPS Works Reliably

  • Reliable quantification of the chemical composition of graphene-related 2D materials (GR2M) as powders and liquid suspensions is a challenging task. Analytical methods such as XPS, ICP-MS, TGA and FTIR are recommended in projects at standardization bodies. The parameters to be measured are also defined, e.g. the oxygen-to-carbon (O/C) concentration ratio, the trace metal impurities, or the functional groups present. In this contribution, for the first time, the capability of SEM/EDS to reliably quantify the O/C ratio in a well-characterized graphene oxide (GO) material is evaluated. The robustness of the SEM/EDS results under various measurement conditions is tested by comparison to the established XPS analysis. A crucial step is the sample preparation from liquid suspension with GO flakes onto a substrate for analysis with both EDS and XPS. It is demonstrated that if a closed and enough thick drop-cast spot is deposited on a substrate, both surface-sensitive XPS analysis andReliable quantification of the chemical composition of graphene-related 2D materials (GR2M) as powders and liquid suspensions is a challenging task. Analytical methods such as XPS, ICP-MS, TGA and FTIR are recommended in projects at standardization bodies. The parameters to be measured are also defined, e.g. the oxygen-to-carbon (O/C) concentration ratio, the trace metal impurities, or the functional groups present. In this contribution, for the first time, the capability of SEM/EDS to reliably quantify the O/C ratio in a well-characterized graphene oxide (GO) material is evaluated. The robustness of the SEM/EDS results under various measurement conditions is tested by comparison to the established XPS analysis. A crucial step is the sample preparation from liquid suspension with GO flakes onto a substrate for analysis with both EDS and XPS. It is demonstrated that if a closed and enough thick drop-cast spot is deposited on a substrate, both surface-sensitive XPS analysis and bulk-characterizing EDS result in very similar elemental composition of oxygen and carbon. Hence, the theoretical, expected O/C atomic ratio values for pure GO of ~0.5 are achieved with both methods. Further, the effect of untight deposited material causing co-analysis of the silicon substrate, is evaluated for both methods, XPS and EDS. Note that all the EDS results in this study have been quantified standardless. The standard measurement procedure including the GO material considered here as a candidate reference material will make a significant contribution to analyse reliably the chemical composition of GR2M with SEM/EDS as one of the most widely used methods in analytical laboratories.zeige mehrzeige weniger

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Autor*innen:Vasile-Dan HodoroabaORCiD
Koautor*innen:Paul Mrkwitschka, Mario SahreORCiD, A. Zurutuza, Jörg RadnikORCiD
Dokumenttyp:Vortrag
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2025
Organisationseinheit der BAM:6 Materialchemie
6 Materialchemie / 6.1 Oberflächen- und Dünnschichtanalyse
DDC-Klassifikation:Technik, Medizin, angewandte Wissenschaften / Ingenieurwissenschaften / Ingenieurwissenschaften und zugeordnete Tätigkeiten
Freie Schlagwörter:EDX; Graphene-related 2D materials; O/C ratio; Samle preparation; Standardisation; XPS
Themenfelder/Aktivitätsfelder der BAM:Material
Material / Advanced Materials
Veranstaltung:Graphene Week 2025
Veranstaltungsort:Vicenza, Italy
Beginndatum der Veranstaltung:22.09.2025
Enddatum der Veranstaltung:26.09.2024
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:06.10.2025
Referierte Publikation:Nein
Eingeladener Vortrag (wissenschaftliche Konferenzen):Nein
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