Synthesis and characterization of graphene oxide using modified hummers method

Abstract

Since graphene is expensive and relatively difficult to produce, significant efforts have been made to develop effective and inexpensive methods for creating and utilizing graphene [1], derivatives, or related materials. Graphene oxide (GO) is one such material. It consists of a single layer of atoms produced through the strong oxidation of cheap and abundant graphite. GO is an oxidized form of graphene containing oxygen-functional groups. Due to its ability to disperse in water and other solvents, GO is easy to process and can even serve as a precursor for graphene production. Although GO is not a good conductor, various processes can enhance its properties. GO is typically synthesized as a powder, in dispersion, or substrate coating. There are four primary methods for synthesizing GO: Staudenmaier, Hofmann, Brodie, and Hummers, with many variations available and ongoing improvements aimed at achieving better results and more cost-effective processes. The efficiency of the oxidation process is typically evaluated by the carbon-to-oxygen ratio of GO. In this study, graphene oxide was synthesized from graphite using a modified Hummers method. In this modification, an ice bath and sodium nitrate (NaNO3) were omitted, and the synthesis was conducted at room temperature. FT-IR, RAMAN, XRD, SEM, and EDS analyses were performed for characterization, yielding results consistent with findings reported in the literature.

Keywords

• Graphene oxide
• graphite powder
• modified hummer’s method
• XRD
• characterization

References

1. Tiwari, S. K., Mishra, R. K., Ha, S. K., Huczko, A., Evolution of graphene oxide and graphene: from imagination to industrialization, ChemNanoMat 4 (2018), 598-620.
2. Brisebois, P., Siaj, M., Harvesting graphene oxide–years 1859 to 2019: a review of its structure, synthesis, properties and exfoliation, Journal of Materials Chemistry C 8 (2020), 1517-1547.
3. Shahriary, L., Athawale, A. A., Graphene oxide synthesized by using modified hummers approach, International Journal of Renewable Energy and Environmental Engineering 2 (2014), 58-63.
4. Kumar, P., Penta, S., Mahapatra, S. P., Mahapatra, Dielectric properties of graphene oxide synthesized by modified hummers’ method from graphite powder, Integrated Ferroelectrics 202 (2019), 41-51.
5. Song, J., Wang, X., Chang, C.-T., Chang, Preparation and characterization of graphene oxide, Journal of Nanomaterials (2014), 276143.
6. Zaaba, N., Foo, K., Hashim, U., Tan, S., Liu, W.-W., Voon, C., Synthesis of graphene oxide using modified hummers method: solvent influence, Procedia Engineering 184 (2017), 469-477.
7. Madurani, K. A., Suprapto, S., Machrita, N. I., Bahar, S. L., Illiya, W., Kurniawan, F., Progress in graphene synthesis and its application: history, challenge and the future outlook for research and industry, ECS Journal of Solid State Science and Technology 9 (2020), 093013.
8. Farjadian, F., Abbaspour, S., Sadatlu, M. A. A., Mirkiani, S., Ghasemi, A., Hoseini‐Ghahfarokhi, M., Mozaffari, N., Karimi, M., Hamblin, M. R., Recent developments in graphene and graphene oxide: Properties, synthesis, and modifications: A review, ChemistrySelect 5 (2020), 10200-10219.

9. Gutiérrez-Cruz, A., Ruiz-Hernández, A. R., Vega-Clemente, J. F., Luna-Gazcón, D. G., Campos-Delgado, J., A review of top-down and bottom-up synthesis methods for the production of graphene, graphene oxide and reduced graphene oxide, Journal of Materials Science 57 (2022), 14543-14578.
10. Gomez, C. V., Robalino, E., Haro, D., Tene, T., Escudero, P., Haro, A., Orbe, J., Structural and electronic properties of graphene oxide for different degree of oxidation, Materials Today: Proceedings 3 (2016), 796-802.
11. Schöche, S., Hong, N., Khorasaninejad, M., Ambrosio, A., Orabona, E., Maddalena, P., Capasso, F., Optical properties of graphene oxide and reduced graphene oxide determined by spectroscopic ellipsometry, Applied Surface Science 421 (2017), 778-782.
12. Aradhana, R., Mohanty, S., Nayak, S. K., Comparison of mechanical, electrical and thermal properties in graphene oxide and reduced graphene oxide filled epoxy nanocomposite adhesives, Polymer 141 (2018), 109-123.
13. Mu, X., Wu, X., Zhang, T., Go, D. B., Luo, T., Thermal transport in graphene oxide–from ballistic extreme to amorphous limit, Scientific Reports 4 (2014), 3909.
14. Mahanta, N. K., Abramson, A. R., Thermal conductivity of graphene and graphene oxide nanoplatelets, 13th intersociety conference on thermal and thermomechanical phenomena in electronic systems (2012), 1-6.
15. Abdullah, S. I., Ansari, M., Mechanical properties of graphene oxide (GO)/epoxy composites, Hbrc Journal 11 (2015), 151-156.
16. Suk, J. W., Piner, R. D., An, J., Ruoff, R. S., Mechanical properties of monolayer graphene oxide, ACS Nano 4 (2010), 6557-6564.
17. Jiříčková, A., Jankovský, O., Sofer, Z., Sedmidubský, D., Synthesis and applications of graphene oxide, Materials 15 (2022), 920.
18. Konios, D., Stylianakis, M. M., Stratakis, E., Kymakis, E., Dispersion behaviour of graphene oxide and reduced graphene oxide, Journal of Colloid and Interface Science 430 (2014), 108-112.
19. Chung, C., Kim, Y.-K., Shin, D., Ryoo, S.-R., Hong, B. H., Min, D.-H., Biomedical applications of graphene and graphene oxide, Accounts of Chemical Research 46 (2013), 2211-2224.
20. Wan, X., Huang, Y., Chen, Y., Focusing on energy and optoelectronic applications: a journey for graphene and graphene oxide at large scale, Accounts of Chemical Research 45 (2012), 598-607.
21. Kiew, S. F., Kiew, L. V., Lee, H. B., Imae, T., Chung, L. Y., Assessing biocompatibility of graphene oxide-based nanocarriers: A review, Journal of Controlled Release 226 (2016), 217-228.
22. Liu, J., Cui, L., Losic, D., Graphene and graphene oxide as new nanocarriers for drug delivery applications, Acta Biomaterialia 9 (2013), 9243-9257.
23. Botas, C., Álvarez, P., Blanco, P., Granda, M., Blanco, C., Santamaría, R., Romasanta, L. J., Verdejo, R., López-Manchado, M. A., Menéndez, R., Graphene materials with different structures prepared from the same graphite by the Hummers and Brodie methods, Carbon 65 (2013), 156-164.
24. Chen, J., Yao, B., Li, C., Shi, G., An improved Hummers method for eco-friendly synthesis of graphene oxide, Carbon 64 (2013), 225-229.
25. Minitha, C. R., Rajendrakumar, R. T., Synthesis and characterization of reduced graphene oxide, Advanced Materials Research 678 (2013), 56-60.
26. Chaiyakun, S., Witit-Anun, N., Nuntawong, N., Chindaudom, P., Oaew, S., Kedkeaw, C., Limsuwan, P., Preparation and characterization of graphene oxide nanosheets, Procedia Engineering 32 (2012), 759-764.
27. Surekha, G., Krishnaiah, K. V., Ravi, N., Suvarna, R. P., FTIR, Raman and XRD analysis of graphene oxide films prepared by modified Hummers method, Journal of Physics: Conference Series, IOP Publishing 1495 (2020), 012012.
28. Emiru, T. F., Ayele, D. W., Controlled synthesis, characterization and reduction of graphene oxide: A convenient method for large scale production, Egyptian Journal of Basic and Applied Sciences 4 (2017), 74-79.
29. Loryuenyong, V., Totepvimarn, K., Eimburanapravat, P., Boonchompoo, W., Buasri, A., Preparation and characterization of reduced graphene oxide sheets via water‐based exfoliation and reduction methods, Advances in Materials Science and Engineering 2013 (2013), 923403.
30. Bera, M., Gupta, P., Maji, P. K., Facile one-pot synthesis of graphene oxide by sonication assisted mechanochemical approach and its surface chemistry, Journal of Nanoscience and Nanotechnology (2018), 902-912.
31. Zólyomi, V., Koltai, J., Kürti, J., Resonance Raman spectroscopy of graphite and graphene, Physica Status Solidi (b) 248 (2011), 2435-2444.
32. Kudin, K. N., Ozbas, B., Schniepp, H. C., Prud'Homme, R. K., Aksay, I. A., Car, R., Raman spectra of graphite oxide and functionalized graphene sheets, Nano letters 8 (2008), 36-41.
33. Lyon, L. A., Keating, C. D., Fox, A. P., Baker, B. E., He, L., Nicewarner, S. R., Mulvaney, S. P., Natan, M. J., Raman spectroscopy, Analytical Chemistry 70 (1998), 341-362.
34. Mokhtar, M., El Enein, S. A., Hassaan, M., Morsy, M., Khalil, M., Thermally reduced graphene oxide: synthesis, structural and electrical properties, International Journal of Nanoparticles and Nanotechnology 3 (2017), 8.
35. Kim, S.-G., Park, O.-K., Lee, J. H., Ku, B.-C., Layer-by-layer assembled graphene oxide films and barrier properties of thermally reduced graphene oxide membranes, Carbon letters (2013), 247-250.
36. Faiz, M. A., Azurahanim, C. C., Raba'ah, S. A., Ruzniza, M. Z., Low cost and green approach in the reduction of graphene oxide (GO) using palm oil leaves extract for potential in industrial applications, Results in Physics 16 (2020), 102954.
37. Siddarth, R. K., Manopriya, M., Swathi, G., Vijayvenkataraman, G., Aranganayagam, K., One step synthesis of reduced and moringa oleifera treated graphene oxide: characterization and antibacterial studies, Proceedings of the International Conference on Nanomedicine, Springer, (2019), 54-62.
38. Wilson, N. R., Pandey, P. A., Beanland, R., Rourke, J., Lupo, U., Rowlands, G., Römer, R. A., On the structure and topography of free-standing chemically modified graphene, New Journal of Physics 12 (2010), 125010.
39. Wilson, N. R., Pandey, P. A., Beanland, R., Young, R. J., Kinloch, I. A., Gong, L., Liu, Z., Suenaga, K., Rourke, J. P., York, S. J., Graphene oxide: structural analysis and application as a highly transparent support for electron microscopy, ACS Nano 3 (2009), 2547-2556.