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. 2019 Aug 18;9(8):1180.
doi: 10.3390/nano9081180.

Structural Characterization of Graphene Oxide: Surface Functional Groups and Fractionated Oxidative Debris

Elvin Aliyev  1 , Volkan Filiz  2 , Muntazim M Khan  1 , Young Joo Lee  3 , Clarissa Abetz  1 , Volker Abetz  1   4
Affiliations

Structural Characterization of Graphene Oxide: Surface Functional Groups and Fractionated Oxidative Debris

Elvin Aliyev et al. Nanomaterials (Basel). .

Abstract

The purpose of this work is the structural analysis of graphene oxide (GO) and by means of a new structural model to answer the questions arising from the Lerf-Klinowski and the Lee structural models. Surface functional groups of GO layers and the oxidative debris (OD) stacked on them were investigated after OD was extracted. Analysis was performed successfully using Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy (UV-Vis), X-ray photoemission spectroscopy (XPS), energy-dispersive X-ray spectroscopy (EDX), Raman spectroscopy, solid-state nuclear magnetic resonance spectroscopy (SSNMR), standardized Boehm potentiometric titration analysis, elemental analysis, X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The analysis showed that graphene oxide layers, as well as oxidative debris contain different functional groups such as phenolic -OH, ketone, lactone, carboxyl, quinone and epoxy. Based on these results, a new structural model for GO layers is proposed, which covers all spectroscopic data and explains the presence of the other oxygen functionalities besides carboxyl, phenolic -OH and epoxy groups.

Keywords: base-washed graphene oxide; graphene oxide; oxidative debris; standardized Boehm titration method; surface functional group analysis.

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Conflict of interest statement

The authors declare no conflicts of interest.

Figures

Figure 1
Figure 1
C1s XPS spectra of graphene oxide samples: (a) GO, (b) bwGO, (c) rGO and rbwGO.
Figure 2
Figure 2
O1s XPS spectra of graphene oxide samples: (a) GO; (b) bwGO; (c) rGO and (d) rbwGO.
Figure 3
Figure 3
FTIR (a) and UV-Vis (b) spectra of GO, base-washed GO and their reduced forms.
Figure 4
Figure 4
Direct excitation 13C MAS NMR spectra of graphene oxide samples.
Figure 5
Figure 5
Raman spectra of graphene oxide samples.
Figure 6
Figure 6
XRD patterns of graphene oxide samples.
Figure 7
Figure 7
Thermogravimetric results of graphene oxide samples.
Figure 8
Figure 8
SEM (a–e) and TEM (f–i) images of graphene oxide and oxidative debris samples: (a)—graphite, (b)—GO, (c)—bwGO, (d)—rGO, (e)—rbwGO, (f)—bulk GO, (g)—single layer GO, (h)—oxidative debris, (i)—stacked and wrinkled GO layers.
Figure 9
Figure 9
Proposed structure of graphene oxide layer.
See this image and copyright information in PMC

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