Skip to main content
SpringerLink
Log in

Thermally reduced graphene oxide: synthesis, studies and characterization

  • Chemical routes to materials
  • Published:
Journal of Materials Science Aims and scope Submit manuscript

Abstract

The main purpose of this study is to synthesize reduced graphene oxide (rGO) using graphite (GR) as a starting material. This paper explains didactic step-by-step of the synthesis, the role of each reagent, showing pictures of the entire process and including a well-explained characterization study. The rGO was prepared using modified Hummer’s method, followed by thermal reduction. The materials were characterized from the starting material (GR), through the intermediate material (GO) and finally the material of interest (rGO). Various techniques and procedures were used to characterize the materials such as X-ray diffraction, infrared and Raman spectroscopy, scanning electron microscopy, electrochemical characterization and dispersion analysis. Morphological and structural characterization of the obtained materials suggests that the synthesis and reduction to obtain rGO were effective. The obtained materials were electrochemically evaluated using ferri/ferrocyanide redox probe. The association of chemical oxidation of GR with KMnO4 in the presence of H2SO4 with further thermal reduction makes possible to produce rGO in large scale and with quality as noticed by outstanding electrochemical behavior toward the redox couple [Fe(CN)6]3−/[Fe(CN)6]4− probe.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Figure 1
Figure 2
Figure 3
Figure 4
Figure 5
Figure 6
Figure 7
Figure 8
Figure 9

Similar content being viewed by others

References

  1. Singh V, Joung D, Zhai L, Das S, Khondaker SI, Seal S (2011) Progress in materials science graphene based materials: past, present and future. Prog Mater Sci 56(8):1178–1271

    Article  Google Scholar 

  2. Lavender L (2014) Graphene: applications and future uses. The Institute of Physics, London

    Google Scholar 

  3. Geim AK, Novoselov KS (2007) The rise of graphene. Nat Mater 6(3):183–191

    Article  Google Scholar 

  4. Bianco A et al (2013) All in the graphene family—a recommended nomenclature for two dimensional carbon materials. Carbon 65:1–6

    Article  Google Scholar 

  5. Allen MJ, Tung VC, Kaner RB (2010) Honeycomb carbon: a review of graphene. Chem Rev 110:132–145

    Article  Google Scholar 

  6. Zarbin AJG, Oliveira MM (2013) Carbon nanostructures (nanotubes and graphene): Quo Vadis? Quim Nova 36(10):1533–1539

    Article  Google Scholar 

  7. Sengupta R et al (2011) A review on the mechanical and electrical properties of graphite and modified graphite reinforced polymer composites. Prog Polym Sci 36(5):638–670

    Article  Google Scholar 

  8. Novoselov KS, Geim AK, Morozov SV, Jiang D, Zhang Y, Dubonos SV, Grigorieva AA (2004) Electric field effect in atomically thin carbon films. Science 306(1):666–669

    Article  Google Scholar 

  9. Pei S, Cheng HM (2012) The reduction of graphene oxide. Carbon 50(9):3210–3228

    Article  Google Scholar 

  10. Gao W (2015) Graphene oxide: reduction recipes, spectroscopy and applications. Springer, Cham

    Book  Google Scholar 

  11. Wang Y, Li Y, Tang L, Lu J, Li J (2009) Application of graphene-modified electrode for selective detection of dopamine. Electrochem Commun 11:889

    Article  Google Scholar 

  12. Sun JY, Huang KJ, Wei SY, Wu ZW, Ren F (2011) A graphene-based electrochemical sensor for sensitive determination of caffeine. Colloids Surf B 84:421

    Article  Google Scholar 

  13. Hummers J, Offeman RE (1958) Preparation of graphitic oxide. J Am Chem Soc 80:1339–1340

    Article  Google Scholar 

  14. Bagri A et al (2010) Structural evolution during the reduction of chemically derived graphene oxide. Nat Chem 2(7):581–587

    Article  Google Scholar 

  15. Abdolhosseinzadeh S, Asgharzadeh H, Kim HS (2015) Fast and fully-scalable synthesis of reduced graphene oxide. Sci Rep 5:1–15

    Article  Google Scholar 

  16. Kong L, Jiang X, Zeng Y, Zhou T, Shi G (2013) Molecularly imprinted sensor based on electropolmerized poly(o-phenylenediamine). membranes at reduced graphene oxide modified electrode for imidacloprid determination. Sens Actuat B Chem 185:424–431

    Article  Google Scholar 

  17. Pumera M, Ambrosi A, Bonanni A, Khim EL, Poh HL (2010) Graphene for electrochemical sensing and biosensing. Trends Anal Chem 29(9):954–965

    Article  Google Scholar 

  18. Dreyer DR, Park S, Bielawski CW, Ruoff RS (2010) The chemistry of graphene oxide. Chem Soc Rev 39:228–240

    Article  Google Scholar 

  19. Dimiev AM, Tour J (2014) Mechanism of graphene oxide formation. ACS Nano 8:3060–3068

    Article  Google Scholar 

  20. Stankovich S, Dikin DA, Piner RD, Kohlhaas KA, Kleinhammes A, Jia Y (2007) Synthesis of graphene-based nanosheets via chemical reduction of exfoliated graphite oxide. Carbon 45(7):1558–1565

    Article  Google Scholar 

  21. Wu ZS, Ren W, Gao L, Liu B, Jiang C, Cheng HM (2008) Synthesis of high-quality graphene with a pre-determined number of layers. Carbon 47:493–499

    Article  Google Scholar 

  22. Mcallister MJ, Li JL, Adamson DH, Schniepp HC, Abdala AA, Liu J (2007) Expansion of graphite. Chem Mater 19(4):4396–4404

    Article  Google Scholar 

  23. Russel JB (1994) Química Geral, 2nd edn. Pearson, São Paulo

    Google Scholar 

  24. Clayden J, Greeves N, Warren S (2012) Organic chemistry, 2nd edn. Oxford University Press, Oxford

    Google Scholar 

  25. Nonomura Y, Morita Y, Deguchi S, Mukai S (2010) Anomalously stable dispersions of graphite in water/acetone mixtures. J Colloid Interface Sci 346:96–99

    Article  Google Scholar 

  26. Khan M, Al-Marri AH, Khan M, Mohri N, Adil SF, Al-Warthan A, Siddiqui RMH, Alkhathlan HZ, Berger R, Tremelb W, Tahir MN (2014) Pulicaria glutinosa plant extract: a green and ecofriendly reducing agent for the preparation of highly reduced graphene oxide. RSC Adv 4:24119–24125

    Article  Google Scholar 

  27. Shahriary L, Athawale AA (2014) Graphene oxide synthesized by using modified hummers approach. Int J Renew Energy Environ Eng 2:58–63

    Google Scholar 

  28. Bai YL et al (2015) Effects of graphene reduction degree on thermal oxidative stability of reduced graphene oxide/silicone rubber nanocomposites. High Perform Polym 27(8):997–1006

    Article  Google Scholar 

  29. Ball DW (2006) Físico-Química, vol 2. Thomson, São Paulo

    Google Scholar 

  30. Ewing GW (2009) Métodos instrumentais de análise química, vol 2. Blücher, São Paulo

    Google Scholar 

  31. Nekahi PH, Haghshenas MD (2014) Transparent conductive thin film of ultra large reduced graphene oxide monolayers. Appl Surf Sci 295:59–65

    Article  Google Scholar 

  32. Krishnamurthy G, Namitha RB (2013) Synthesis of structurally novel carbon micro/nanospheres by low temperature-hydrothermal process. J Chil Chem Soc 58(3):1930–1933

    Article  Google Scholar 

  33. Stuart B (2004) Infrared spectroscopy: fundamentals and applications. Wiley, New York

    Book  Google Scholar 

  34. Lerf A, He H, Forster M, Klinowski J (1998) Structure of graphite oxide revisited. J Phys Chem B 5647(97):4477–4482

    Article  Google Scholar 

  35. Klinowski J, He H, Forster M, Lerf A (1998) A new structural model for graphite oxide. Chem Phys Lett 287:53–56

    Article  Google Scholar 

  36. Yaragalla S, Meera AP, Kalarikkal N, Thomas S (2015) Chemistry associated with natural rubber—graphene nanocomposites and its effect on physical and structural properties. Ind Crops Prod 74:792–802

    Article  Google Scholar 

  37. Han JH, Cho KW, Lee K-H, Kim H (1998) Porous graphite matrix for chemical heat pumps. Carbon 36(12):1801–1810

    Article  Google Scholar 

  38. Bissessur R, Scully SF (2007) Intercalation of solid polymer electrolytes into graphite oxide. Solid States Ionics 178:877–882

    Article  Google Scholar 

  39. Vinayan BP, Nagar R, Raman BN, Rajalakshmi KS, Dhathathreyan BS, Ramaprabhu A (2012) Synthesis of graphene-multiwalled carbon nanotubes hybrid nanostructure by strengthened electrostatic interaction and its lithium ion battery application. J Mater Chem 22:9949–9956

    Article  Google Scholar 

  40. Zhang H, Zheng W, Yan Q, Yang Y, Wang J, Lu Z, Ji G, Yu Z (2010) Electrically conductive polyethylene terephthalate/graphene nanocomposites prepared by melt compounding. Polymer 51:1191–1196

    Article  Google Scholar 

  41. Tang Z, Zhang L, Zeng C, Lin T, Guo B (2012) General route to graphene with liquidlike behavior by non-covalent modification. Soft Matter 8(35):9214–9220

    Article  Google Scholar 

  42. Soldano C, Mahmood A, Dujardin E (2010) Production, properties and potential of graphene. Carbon 48(8):2127–2150

    Article  Google Scholar 

  43. Feng H, Wang X, Wu D (2013) Fabrication of spirocyclic phosphazene epoxy-based nanocomposites with graphene via exfoliation of graphite platelets and thermal curing for enhancement of mechanical and conductive properties. Ind Eng Chem Res 52:10160–10171

    Article  Google Scholar 

  44. Sharon M, Sharon M (2015) Graphene: An Introduction to the fundamentals and industrial applications. Scrivener Publishing, Beverly

    Book  Google Scholar 

  45. Sreeprasad TS, Berry V (2013) How do the electrical properties of graphene change with its functionalization. Small 9(3):341–350

    Article  Google Scholar 

Download references

Acknowledgements

We thank FAPEMIG, CAPES, CNPQ and Rede Mineira de Química for the continuous support of our research that has led to this synthesis. We also thank Prof. Dr. Emerson S. Ribeiro for the partnership.

Author information

Authors and Affiliations

  1. Departamento de Ciências Naturais, Universidade Federal de São João del-Rei, UFSJ, São João del-Rei, MG, CEP 36307-352, Brazil

    Ana Elisa Ferreira Oliveira, Guilherme Bettio Braga & Arnaldo César Pereira

  2. Departamento de Química, Universidade Estadual de Londrina, UEL, Londrina, PR, CEP 86057-970, Brazil

    César Ricardo Teixeira Tarley

Authors
  1. Ana Elisa Ferreira Oliveira
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Guilherme Bettio Braga
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. César Ricardo Teixeira Tarley
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Arnaldo César Pereira
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Arnaldo César Pereira.

Ethics declarations

Conflict of interest

No potential conflict of interest was reported by the authors.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Oliveira, A.E.F., Braga, G.B., Tarley, C.R.T. et al. Thermally reduced graphene oxide: synthesis, studies and characterization. J Mater Sci 53, 12005–12015 (2018). https://doi.org/10.1007/s10853-018-2473-3

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10853-018-2473-3

Keywords

Search

Navigation