Controlled reduction of graphene oxide using sulfuric acid

Ana Cecilia Reynosa-Martínez; Erika Gómez-Chayres; Rafael Villaurrutia; Eddie López-Honorato

doi:10.3390/ma14010059

Controlled reduction of graphene oxide using sulfuric acid

Ana Cecilia Reynosa-Martínez, Erika Gómez-Chayres, Rafael Villaurrutia, Eddie López-Honorato

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Abstract

Sulfuric acid under different concentrations and with the addition of SO₃ (fuming sulfuric acid) was studied as a reducing agent for the production of reduced graphene oxide (RGO). Three concentrations of sulfuric acid (1.5, 5, and 12 M), as well as 12 M with 30% SO₃, were used. The reduction of graphene oxide increased with H₂SO₄ concentration as observed by Fourier-transformed infrared spectroscopy and X-ray photoelectron spectroscopy. It was observed that GO lost primarily epoxide functional groups from 40.4 to 9.7% and obtaining 69.8% carbon when using 12 M H₂SO₄, without leaving sulfur doping. Additionally, the appearance of hexagonal domain structures observed in transmission electron microscopy and analyzed by selected area electron diffraction patterns con-firmed the improvement in graphitization. Although the addition of SO₃ in H₂SO₄ improved the GO reduction with 74% carbon, as measured by XPS, the use of SO₃ introduced sulfur doping of 1.3%. RGO produced with sulfuric acid was compared with a sample obtained via ultraviolet (UV) irradiation, a very common reduction route, by observing that the RGO produced with sulfuric acid had a higher C/O ratio than the material reduced by UV irradiation. This work showed that sulfuric acid can be used as a single-step reducing agent for RGO without sulfur contamination.

Original language	English
Article number	59
Pages (from-to)	1-10
Number of pages	10
Journal	Materials
Volume	14
Issue number	1
DOIs	https://doi.org/10.3390/ma14010059
State	Published - Jan 1 2021

Funding

Funding: Work sponsored by a grant from Secretaría de Energía and Consejo Nacional de Ciencia y Tecnología (SENER-CONACYT) as part of the Centro Mexicano de Innovación en Energía del Océano (CEMIE-Océano) (project number 249795). Work sponsored by a grant from Secretar?a de Energ?a and Consejo Nacional de Ciencia y Tecnolog?a (SENER-CONACYT) as part of the Centro Mexicano de Innovaci?n en Energ?a del Oc?ano (CEMIE-Oc?ano) (project number 249795). The authors acknowledge CONACYT for the Ph.D. scholarship awarded to A. C. Reynosa-Mart?nez and E. Gomez-Chaires. This manuscript has been authored by UT-Battelle, LLC, under contract DE-AC05-00OR22725 with the US Department of Energy (DOE). The US government retains and the publisher, by accepting the article for publication, acknowledges that the US government retains a nonexclusive, paid-up, irrevocable, worldwide license to publish or reproduce the published form of this manuscript, or allow others to do so, for US government purposes. DOE will provide public access to these results of federally sponsored research in accordance with the DOE Public Access Plan (http://energy.gov/downloads/doe-public-access-plan). Acknowledgments: The authors acknowledge CONACYT for the Ph.D. scholarship awarded to A. C. Reynosa-Martínez and E. Gomez-Chaires. This manuscript has been authored by UT-Battelle, LLC, under contract DE-AC05-00OR22725 with the US Department of Energy (DOE). The US government retains and the publisher, by accepting the article for publication, acknowledges that the US government retains a nonexclusive, paid-up, irrevocable, worldwide license to publish or reproduce the published form of this manuscript, or allow others to do so, for US government purposes. DOE will provide public access to these results of federally sponsored research in accordance with the DOE Public Access Plan (http://energy.gov/downloads/doe-public-access-plan).

Funders	Funder number
CEMIE-Océano	249795
Centro Mexicano de Innovaci?n en Energ?a del Oc?ano
Consejo Nacional de Ciencia y Tecnolog?a
DOE Public Access Plan
SENER-CONACYT
Secretar?a de Energ?a
US Department of Energy
U.S. Department of Energy
Centro Mexicano de Innovación en Energía Geotérmica
Consejo Nacional de Ciencia y Tecnología	DE-AC05-00OR22725
Secretaría de Energía de México

Keywords

Fuming sulfuric acid
Reduce graphene oxide
Sulfuric acid
UV-radiation

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10.3390/ma14010059

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title = "Controlled reduction of graphene oxide using sulfuric acid",

abstract = "Sulfuric acid under different concentrations and with the addition of SO3 (fuming sulfuric acid) was studied as a reducing agent for the production of reduced graphene oxide (RGO). Three concentrations of sulfuric acid (1.5, 5, and 12 M), as well as 12 M with 30% SO3, were used. The reduction of graphene oxide increased with H2SO4 concentration as observed by Fourier-transformed infrared spectroscopy and X-ray photoelectron spectroscopy. It was observed that GO lost primarily epoxide functional groups from 40.4 to 9.7% and obtaining 69.8% carbon when using 12 M H2SO4, without leaving sulfur doping. Additionally, the appearance of hexagonal domain structures observed in transmission electron microscopy and analyzed by selected area electron diffraction patterns con-firmed the improvement in graphitization. Although the addition of SO3 in H2SO4 improved the GO reduction with 74% carbon, as measured by XPS, the use of SO3 introduced sulfur doping of 1.3%. RGO produced with sulfuric acid was compared with a sample obtained via ultraviolet (UV) irradiation, a very common reduction route, by observing that the RGO produced with sulfuric acid had a higher C/O ratio than the material reduced by UV irradiation. This work showed that sulfuric acid can be used as a single-step reducing agent for RGO without sulfur contamination.",

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Controlled reduction of graphene oxide using sulfuric acid

Abstract

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Keywords

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