Controlled Reduction of Graphene Oxide Using Sulfuric Acid
Sulfuric acid under different concentrations and with the addition of SO<sub>3</sub> (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% SO<sub>...
| Main Authors: | , , , |
|---|---|
| Format: | Article |
| Language: | English |
| Published: |
MDPI AG
2020-12-01
|
| Series: | Materials |
| Subjects: | |
| Online Access: | https://www.mdpi.com/1996-1944/14/1/59 |
| _version_ | 1797543600878256128 |
|---|---|
| author | Ana Cecilia Reynosa-Martínez Erika Gómez-Chayres Rafael Villaurrutia Eddie López-Honorato |
| author_facet | Ana Cecilia Reynosa-Martínez Erika Gómez-Chayres Rafael Villaurrutia Eddie López-Honorato |
| author_sort | Ana Cecilia Reynosa-Martínez |
| collection | DOAJ |
| description | Sulfuric acid under different concentrations and with the addition of SO<sub>3</sub> (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% SO<sub>3</sub>, were used. The reduction of graphene oxide increased with H<sub>2</sub>SO<sub>4</sub> 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 H<sub>2</sub>SO<sub>4</sub>, without leaving sulfur doping. Additionally, the appearance of hexagonal domain structures observed in transmission electron microscopy and analyzed by selected area electron diffraction patterns confirmed the improvement in graphitization. Although the addition of SO<sub>3</sub> in H<sub>2</sub>SO<sub>4</sub> improved the GO reduction with 74% carbon, as measured by XPS, the use of SO<sub>3</sub> 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. |
| first_indexed | 2024-03-10T13:46:58Z |
| format | Article |
| id | doaj.art-ee689643748149838e7aa0dbb0f23b21 |
| institution | Directory Open Access Journal |
| issn | 1996-1944 |
| language | English |
| last_indexed | 2024-03-10T13:46:58Z |
| publishDate | 2020-12-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Materials |
| spelling | doaj.art-ee689643748149838e7aa0dbb0f23b212023-11-21T02:32:04ZengMDPI AGMaterials1996-19442020-12-011415910.3390/ma14010059Controlled Reduction of Graphene Oxide Using Sulfuric AcidAna Cecilia Reynosa-Martínez0Erika Gómez-Chayres1Rafael Villaurrutia2Eddie López-Honorato3Centro de Investigación y de Estudios Avanzados del IPN, Unidad Saltillo, Av. Industria Metalúrgica 1062, Parque Industrial, Ramos Arizpe 25900, Coahuila, MexicoCentro de Investigación y de Estudios Avanzados del IPN, Unidad Saltillo, Av. Industria Metalúrgica 1062, Parque Industrial, Ramos Arizpe 25900, Coahuila, MexicoThermo Fisher Scientific de México, Avenida Morones Prieto 2805 Pte., Monterrey 64710, Nuevo León, MexicoCentro de Investigación y de Estudios Avanzados del IPN, Unidad Saltillo, Av. Industria Metalúrgica 1062, Parque Industrial, Ramos Arizpe 25900, Coahuila, MexicoSulfuric acid under different concentrations and with the addition of SO<sub>3</sub> (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% SO<sub>3</sub>, were used. The reduction of graphene oxide increased with H<sub>2</sub>SO<sub>4</sub> 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 H<sub>2</sub>SO<sub>4</sub>, without leaving sulfur doping. Additionally, the appearance of hexagonal domain structures observed in transmission electron microscopy and analyzed by selected area electron diffraction patterns confirmed the improvement in graphitization. Although the addition of SO<sub>3</sub> in H<sub>2</sub>SO<sub>4</sub> improved the GO reduction with 74% carbon, as measured by XPS, the use of SO<sub>3</sub> 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.https://www.mdpi.com/1996-1944/14/1/59reduce graphene oxidesulfuric acidfuming sulfuric acidUV-radiation |
| spellingShingle | Ana Cecilia Reynosa-Martínez Erika Gómez-Chayres Rafael Villaurrutia Eddie López-Honorato Controlled Reduction of Graphene Oxide Using Sulfuric Acid Materials reduce graphene oxide sulfuric acid fuming sulfuric acid UV-radiation |
| title | Controlled Reduction of Graphene Oxide Using Sulfuric Acid |
| title_full | Controlled Reduction of Graphene Oxide Using Sulfuric Acid |
| title_fullStr | Controlled Reduction of Graphene Oxide Using Sulfuric Acid |
| title_full_unstemmed | Controlled Reduction of Graphene Oxide Using Sulfuric Acid |
| title_short | Controlled Reduction of Graphene Oxide Using Sulfuric Acid |
| title_sort | controlled reduction of graphene oxide using sulfuric acid |
| topic | reduce graphene oxide sulfuric acid fuming sulfuric acid UV-radiation |
| url | https://www.mdpi.com/1996-1944/14/1/59 |
| work_keys_str_mv | AT anaceciliareynosamartinez controlledreductionofgrapheneoxideusingsulfuricacid AT erikagomezchayres controlledreductionofgrapheneoxideusingsulfuricacid AT rafaelvillaurrutia controlledreductionofgrapheneoxideusingsulfuricacid AT eddielopezhonorato controlledreductionofgrapheneoxideusingsulfuricacid |