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Title: In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

Abstract

Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted -more » Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.« less

Authors:
; ;
Publication Date:
OSTI Identifier:
22584177
Resource Type:
Journal Article
Resource Relation:
Journal Name: Journal of Solid State Chemistry; Journal Volume: 240; Other Information: Copyright (c) 2016 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; 77 NANOSCIENCE AND NANOTECHNOLOGY; CLATHRATES; CRYSTALLIZATION; CRYSTALS; DISSOLUTION; GRAPHENE; HEATING; OXIDES; PEAKS; POWDERS; SYNTHESIS; X RADIATION; X-RAY DIFFRACTION

Citation Formats

Storm, Mie Møller, E-mail: mmst@dtu.dk, Johnsen, Rune E., and Norby, Poul. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide. United States: N. p., 2016. Web. doi:10.1016/J.JSSC.2016.05.019.
Storm, Mie Møller, E-mail: mmst@dtu.dk, Johnsen, Rune E., & Norby, Poul. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide. United States. doi:10.1016/J.JSSC.2016.05.019.
Storm, Mie Møller, E-mail: mmst@dtu.dk, Johnsen, Rune E., and Norby, Poul. Mon . "In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide". United States. doi:10.1016/J.JSSC.2016.05.019.
@article{osti_22584177,
title = {In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide},
author = {Storm, Mie Møller, E-mail: mmst@dtu.dk and Johnsen, Rune E. and Norby, Poul},
abstractNote = {Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.},
doi = {10.1016/J.JSSC.2016.05.019},
journal = {Journal of Solid State Chemistry},
number = ,
volume = 240,
place = {United States},
year = {Mon Aug 15 00:00:00 EDT 2016},
month = {Mon Aug 15 00:00:00 EDT 2016}
}