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Large-scale Production of Few-Layer Reduced Graphene Oxide by the Rapid Thermal Reduction of Graphene Oxide and Its Structural Characterization

Year 2024, Volume: 11 Issue: 2, 665 - 672
https://doi.org/10.18596/jotcsa.1327988

Abstract

Graphene, a carbon allotrope, is a two-dimensional honeycomb of carbon atoms. Although graphene is a thin material, it is the strongest material known on Earth thanks to the strong carbon bonds in its structure. It is stated that the strength of these carbon bonds in graphene is about 100 times stronger than steel. In this study, graphite was first converted into graphene oxide (GO) by the Improved Hummers method, which is one of the methods suitable for large-scale production. Reduced graphene oxide (RGO) was obtained from the synthesized GOs by thermal reduction. TGA, FTIR, XRD, XPS, Raman, BET, and SEM analyses were used to characterize GO produced using the improved Hummers method and RGO reduced by thermal methods. TGA measurements show that RGO produced using the thermal approach had a lower mass loss than graphite oxidized using the improved Hummers process. This shows that the GO sample prepared using the improved Hummers approach contains a considerable number of distinct oxygen-containing groups. The novelty of the modified Hummers' method lies in its enhanced efficiency in producing graphene oxide through reduced thermal reaction times and improved scalability compared to the original approach in the literature. The C:O ratio of the GO and RGO samples was determined by XPS to be 1.88 and 11.17, respectively. The ID/IG ratio obtained by Raman analysis was 0.973. In addition, RGO's BET surface area was discovered to be 543.6 m2 g-1. These findings demonstrated that graphite was successfully oxidized by an improved Hummers method, and the resulting GO was thermally converted to few-layer RGO.

Supporting Institution

Gebze Technical University BAP Unit

Project Number

2022-A-113-04.

References

  • 1. Geim AK, Novoselov KS. The rise of graphene. Nat Mater [Internet]. 2007 [cited 2023 Jul 14];6(3):183–91. Available from: URL
  • 2. Chen W, Lv G, Hu W, Li D, Chen S, Dai Z. Synthesis and applications of graphene quantum dots: a review. Nanotechnol Rev [Internet]. 2018;7(2):157–85. Available from: URL
  • 3. Coroş M, Pogăcean F, Măgeruşan L, Socaci C, Pruneanu S. A brief overview on synthesis and applications of graphene and graphene-based nanomaterials. Front Mater Sci [Internet]. 2019;13(1):23–32. Available from: URL
  • 4. Afroj S, Tan S, Abdelkader AM, Novoselov KS, Karim N. Highly conductive, scalable, and machine washable graphene‐based E‐textiles for multifunctional wearable electronic applications. Adv Funct Mater [Internet]. 2020;30(23):2000293. Available from: URL
  • 5. Razaq A, Bibi F, Zheng X, Papadakis R, Jafri SHM, Li H. Review on graphene-, graphene oxide-, reduced graphene oxide-based flexible composites: From fabrication to applications. Materials (Basel) [Internet]. 2022 [cited 2023 Jul 14];15(3):1012. Available from: URL
  • 6. Smaisim GF, Abed AM, Al-Madhhachi H, Hadrawi SK, Al-Khateeb HMM, Kianfar E. Graphene-based important carbon structures and nanomaterials for energy storage applications as chemical capacitors and supercapacitor electrodes: A review. Bionanoscience [Internet]. 2023;13(1):219–48. Available from: URL
  • 7. Vivaldi FM, Dallinger A, Bonini A, Poma N, Sembranti L, Biagini D, et al. Three-dimensional (3D) laser-induced graphene: Structure, properties, and application to chemical sensing. ACS Appl Mater Interfaces [Internet]. 2021;13(26):30245–60. Available from: URL
  • 8. Guo H, Zhao H, Niu H, Ren Y, Fang H, Fang X, et al. Highly thermally conductive 3D printed graphene filled polymer composites for scalable thermal management applications. ACS Nano [Internet]. 2021;15(4):6917–28. Available from: URL
  • 9. Dreyer DR, Todd AD, Bielawski CW. Harnessing the chemistry of graphene oxide. Chem Soc Rev [Internet]. 2014 [cited 2023 Jul 14];43(15):5288–301. Available from: URL
  • 10. Poh HL, Šaněk F, Ambrosi A, Zhao G, Sofer Z, Pumera M. Graphenes prepared by Staudenmaier, Hofmann and Hummers methods with consequent thermal exfoliation exhibit very different electrochemical properties. Nanoscale [Internet]. 2012 [cited 2023 Jul 14];4(11):3515–22. Available from: URL
  • 11. Shahriary L, Athawale AA. Graphene Oxide Synthesized by using Modified Hummers Approach. Int. J. Energy Environ. Eng. 2012;2(1):58-63. Available from: URL
  • 12. Gilje S, Han S, Wang M, Wang KL, Kaner RB. A chemical route to graphene for device applications. Nano Lett [Internet]. 2007;7(11):3394–8. Available from: URL
  • 13. Acik M, Lee G, Mattevi C, Chhowalla M, Cho K, Chabal YJ. Unusual infrared-absorption mechanism in thermally reduced graphene oxide. Nat Mater [Internet]. 2010 [cited 2023 Jul 14];9(10):840–5. Available from: URL
  • 14. Sharma S, Ganguly A, Papakonstantinou P, Miao X, Li M, Hutchison JL, et al. Rapid microwave synthesis of CO tolerant reduced graphene oxide-supported platinum electrocatalysts for oxidation of methanol. J Phys Chem C Nanomater Interfaces [Internet]. 2010;114(45):19459–66. Available from: URL
  • 15. Akhavan O. Photocatalytic reduction of graphene oxides hybridized by ZnO nanoparticles in ethanol. Carbon N Y [Internet]. 2011;49(1):11–8. Available from: URL
  • 16. Wang Z, Zhou X, Zhang J, Boey F, Zhang H. Direct electrochemical reduction of single-layer graphene oxide and subsequent functionalization with glucose oxidase. J Phys Chem C Nanomater Interfaces [Internet]. 2009;113(32):14071–5. Available from: URL
  • 17. Alam SN, Sharma N, Kumar L. Synthesis of graphene oxide (GO) by improved hummers method and its thermal reduction to obtain reduced graphene oxide (rGO). Graphene [Internet]. 2017 [cited 2023 Jul 14];06(01):1–18. Available from: URL
  • 18. Losic D, Farivar F, Yap PL, Karami A. Accounting carbonaceous counterfeits in graphene materials using the thermogravimetric analysis (TGA) approach. Anal Chem [Internet]. 2021;93(34):11859–67. Available from: URL
  • 19. Muzyka R, Kwoka M, Smędowski Ł, Díez N, Gryglewicz G. Oxidation of graphite by different improved Hummers methods. New Carbon Mater [Internet]. 2017;32(1):15–20. Available from: URL
  • 20. Manoratne CH, Rosa SRD, Kottegoda IRM. XRD-HTA, UV Visible, FTIR and SEM interpretation of reduced graphene oxide synthesized from high purity vein graphite. Mater. Sci. Res. India. 2017;14(1):19:30. Available from: URL
  • 21. Oliveira AEF, Braga GB, Tarley CRT, Pereira AC. Thermally reduced graphene oxide: synthesis, studies and characterization. J Mater Sci [Internet]. 2018;53(17):12005–15. Available from: URL
  • 22. Al-Gaashani R, Najjar A, Zakaria Y, Mansour S, Atieh MA. XPS and structural studies of high quality graphene oxide and reduced graphene oxide prepared by different chemical oxidation methods. Ceram Int [Internet]. 2019;45(11):14439–48. Available from: URL
  • 23. Farah S, Farkas A, Madarász J, László K. Comparison of thermally and chemically reduced graphene oxides by thermal analysis and Raman spectroscopy. J Therm Anal Calorim [Internet]. 2020;142(1):331–7. Available from: URL
  • 24. Lee AY, Yang K, Anh ND, Park C, Lee SM, Lee TG, et al. Raman study of D* band in graphene oxide and its correlation with reduction. Appl Surf Sci [Internet]. 2021;536(147990):147990. Available from: URL
  • 25. Saleem H, Haneef M, Abbasi HY. Synthesis route of reduced graphene oxide via thermal reduction of chemically exfoliated graphene oxide. Mater Chem Phys [Internet]. 2018;204:1–7. Available from: URL
Year 2024, Volume: 11 Issue: 2, 665 - 672
https://doi.org/10.18596/jotcsa.1327988

Abstract

Project Number

2022-A-113-04.

References

  • 1. Geim AK, Novoselov KS. The rise of graphene. Nat Mater [Internet]. 2007 [cited 2023 Jul 14];6(3):183–91. Available from: URL
  • 2. Chen W, Lv G, Hu W, Li D, Chen S, Dai Z. Synthesis and applications of graphene quantum dots: a review. Nanotechnol Rev [Internet]. 2018;7(2):157–85. Available from: URL
  • 3. Coroş M, Pogăcean F, Măgeruşan L, Socaci C, Pruneanu S. A brief overview on synthesis and applications of graphene and graphene-based nanomaterials. Front Mater Sci [Internet]. 2019;13(1):23–32. Available from: URL
  • 4. Afroj S, Tan S, Abdelkader AM, Novoselov KS, Karim N. Highly conductive, scalable, and machine washable graphene‐based E‐textiles for multifunctional wearable electronic applications. Adv Funct Mater [Internet]. 2020;30(23):2000293. Available from: URL
  • 5. Razaq A, Bibi F, Zheng X, Papadakis R, Jafri SHM, Li H. Review on graphene-, graphene oxide-, reduced graphene oxide-based flexible composites: From fabrication to applications. Materials (Basel) [Internet]. 2022 [cited 2023 Jul 14];15(3):1012. Available from: URL
  • 6. Smaisim GF, Abed AM, Al-Madhhachi H, Hadrawi SK, Al-Khateeb HMM, Kianfar E. Graphene-based important carbon structures and nanomaterials for energy storage applications as chemical capacitors and supercapacitor electrodes: A review. Bionanoscience [Internet]. 2023;13(1):219–48. Available from: URL
  • 7. Vivaldi FM, Dallinger A, Bonini A, Poma N, Sembranti L, Biagini D, et al. Three-dimensional (3D) laser-induced graphene: Structure, properties, and application to chemical sensing. ACS Appl Mater Interfaces [Internet]. 2021;13(26):30245–60. Available from: URL
  • 8. Guo H, Zhao H, Niu H, Ren Y, Fang H, Fang X, et al. Highly thermally conductive 3D printed graphene filled polymer composites for scalable thermal management applications. ACS Nano [Internet]. 2021;15(4):6917–28. Available from: URL
  • 9. Dreyer DR, Todd AD, Bielawski CW. Harnessing the chemistry of graphene oxide. Chem Soc Rev [Internet]. 2014 [cited 2023 Jul 14];43(15):5288–301. Available from: URL
  • 10. Poh HL, Šaněk F, Ambrosi A, Zhao G, Sofer Z, Pumera M. Graphenes prepared by Staudenmaier, Hofmann and Hummers methods with consequent thermal exfoliation exhibit very different electrochemical properties. Nanoscale [Internet]. 2012 [cited 2023 Jul 14];4(11):3515–22. Available from: URL
  • 11. Shahriary L, Athawale AA. Graphene Oxide Synthesized by using Modified Hummers Approach. Int. J. Energy Environ. Eng. 2012;2(1):58-63. Available from: URL
  • 12. Gilje S, Han S, Wang M, Wang KL, Kaner RB. A chemical route to graphene for device applications. Nano Lett [Internet]. 2007;7(11):3394–8. Available from: URL
  • 13. Acik M, Lee G, Mattevi C, Chhowalla M, Cho K, Chabal YJ. Unusual infrared-absorption mechanism in thermally reduced graphene oxide. Nat Mater [Internet]. 2010 [cited 2023 Jul 14];9(10):840–5. Available from: URL
  • 14. Sharma S, Ganguly A, Papakonstantinou P, Miao X, Li M, Hutchison JL, et al. Rapid microwave synthesis of CO tolerant reduced graphene oxide-supported platinum electrocatalysts for oxidation of methanol. J Phys Chem C Nanomater Interfaces [Internet]. 2010;114(45):19459–66. Available from: URL
  • 15. Akhavan O. Photocatalytic reduction of graphene oxides hybridized by ZnO nanoparticles in ethanol. Carbon N Y [Internet]. 2011;49(1):11–8. Available from: URL
  • 16. Wang Z, Zhou X, Zhang J, Boey F, Zhang H. Direct electrochemical reduction of single-layer graphene oxide and subsequent functionalization with glucose oxidase. J Phys Chem C Nanomater Interfaces [Internet]. 2009;113(32):14071–5. Available from: URL
  • 17. Alam SN, Sharma N, Kumar L. Synthesis of graphene oxide (GO) by improved hummers method and its thermal reduction to obtain reduced graphene oxide (rGO). Graphene [Internet]. 2017 [cited 2023 Jul 14];06(01):1–18. Available from: URL
  • 18. Losic D, Farivar F, Yap PL, Karami A. Accounting carbonaceous counterfeits in graphene materials using the thermogravimetric analysis (TGA) approach. Anal Chem [Internet]. 2021;93(34):11859–67. Available from: URL
  • 19. Muzyka R, Kwoka M, Smędowski Ł, Díez N, Gryglewicz G. Oxidation of graphite by different improved Hummers methods. New Carbon Mater [Internet]. 2017;32(1):15–20. Available from: URL
  • 20. Manoratne CH, Rosa SRD, Kottegoda IRM. XRD-HTA, UV Visible, FTIR and SEM interpretation of reduced graphene oxide synthesized from high purity vein graphite. Mater. Sci. Res. India. 2017;14(1):19:30. Available from: URL
  • 21. Oliveira AEF, Braga GB, Tarley CRT, Pereira AC. Thermally reduced graphene oxide: synthesis, studies and characterization. J Mater Sci [Internet]. 2018;53(17):12005–15. Available from: URL
  • 22. Al-Gaashani R, Najjar A, Zakaria Y, Mansour S, Atieh MA. XPS and structural studies of high quality graphene oxide and reduced graphene oxide prepared by different chemical oxidation methods. Ceram Int [Internet]. 2019;45(11):14439–48. Available from: URL
  • 23. Farah S, Farkas A, Madarász J, László K. Comparison of thermally and chemically reduced graphene oxides by thermal analysis and Raman spectroscopy. J Therm Anal Calorim [Internet]. 2020;142(1):331–7. Available from: URL
  • 24. Lee AY, Yang K, Anh ND, Park C, Lee SM, Lee TG, et al. Raman study of D* band in graphene oxide and its correlation with reduction. Appl Surf Sci [Internet]. 2021;536(147990):147990. Available from: URL
  • 25. Saleem H, Haneef M, Abbasi HY. Synthesis route of reduced graphene oxide via thermal reduction of chemically exfoliated graphene oxide. Mater Chem Phys [Internet]. 2018;204:1–7. Available from: URL
There are 25 citations in total.

Details

Primary Language English
Subjects Chemical Engineering (Other)
Journal Section RESEARCH ARTICLES
Authors

Osman Eksik 0000-0002-4061-9858

Project Number 2022-A-113-04.
Publication Date
Submission Date July 15, 2023
Acceptance Date January 3, 2024
Published in Issue Year 2024 Volume: 11 Issue: 2

Cite

Vancouver Eksik O. Large-scale Production of Few-Layer Reduced Graphene Oxide by the Rapid Thermal Reduction of Graphene Oxide and Its Structural Characterization. JOTCSA. 11(2):665-72.