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Exfoliation and reduction of graphene oxide at low temperature and its resulting electrocapacitive properties

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Abstract

Low-temperature reduced graphene oxide (LT-RGO) powder with full exfoliated morphology was achieved directly from freeze-dried graphite oxide (GO) aqueous solution in air atmosphere, which is simple and energy-saving. For explaining this phenomenon, the microstructure and thermal behavior of freeze-dried GO and vacuum filtered GO film was compared. Moreover, the thermal-induced reduction process of freeze-dried GO has been in situ monitored by temperature-dependent infrared spectroscopy. The results show that freeze-dried GO demonstrates the floc morphology with larger interlayer distance than that of vacuum filtered GO film, which should be the essential reason for its low-temperature reduction and exfoliation behavior. The dispersibility and capacitance property of as-prepared LT-RGO has also been investigated. At current density of 6 A g−1, the specific capacitance of 460 F g−1 was achieved, shows that the prepared LT-RGO holds great application potential in electric energy storage.

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References

  1. Boehm HP, Clauss A, Fischer GO, Hofmann U (1962) Thin carbon leaves. Z Naturforsch 17b:150–153

    Google Scholar 

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

    Article  Google Scholar 

  3. Stoller MD, Park S, Zhu Y, An J, Ruoff RS (2008) Graphene-based ultracapacitors. Nano Lett 8:3498–3502

    Article  Google Scholar 

  4. Park S, Ruoff RS (2009) Chemical methods for the production of graphenes. Nat Nanotechnol 4:217–224

    Article  Google Scholar 

  5. Bunch JS, Verbridge SS, Alden JS, van der Zande AM, Parpia JM, Craighead HG, McEuen PL (2008) Impermeable atomic membranes from graphene sheets. Nano Lett 8:2458–2462

    Article  Google Scholar 

  6. Lee C, Wei X, Kysar JW, Hone J (2008) Measurement of the elastic properties and intrinsic strength of monolayer graphene. Science 321(5887):385–388

    Article  Google Scholar 

  7. Balandin AA, Ghosh S, Bao W, Calizo I, Teweldebrhan D, Miao F, Lau CN (2008) Superior thermal conductivity of single-layer graphene. Nano Lett 8:902–907

    Article  Google Scholar 

  8. Bolotin KI, Sikes KJ, Jiang Z, Klima M, Fudenberg G, Hone J, Stormer HL (2008) Ultrahigh electron mobility in suspended graphene. Solid State Commun 146:351–355

    Article  Google Scholar 

  9. Lotya M, King PJ, Khan U, De S, Coleman JN (2010) High-concentration, surfactant-stabilized graphene dispersions. ACS Nano 4:3155–3162

    Article  Google Scholar 

  10. Coleman JN (2009) Liquid-phase exfoliation of nanotubes and graphene. Adv Funct Mater 19:3680–3695

    Article  Google Scholar 

  11. Hernandez Y, Nicolosi V, Lotya M, Blighe FM, Sun Z, De S, Coleman JN (2008) High-yield production of graphene by liquid-phase exfoliation of graphite. Nat Nanotechnol 3:563–568

    Article  Google Scholar 

  12. Robinson J, Weng X, Trumbull K, Cavalero R, Wetherington M, Frantz E, Snyder D (2009) Nucleation of epitaxial graphene on SiC. ACS Nano 4:153–158

    Article  Google Scholar 

  13. Berger C, Song Z, Li X, Wu X, Brown N, Naud C, de Heer WA (2006) Electronic confinement and coherence in patterned epitaxial graphene. Science 312:1191–1196

    Article  Google Scholar 

  14. Wang X, You H, Liu F, Li M, Wan L, Li S, Cheng J (2009) Large-scale synthesis of few-layered graphene using CVD. Chem Vap Depos 15:53–56

    Article  Google Scholar 

  15. Li X, Cai W, An J, Kim S, Nah J, Yang D, Ruoff RS (2009) Large-area synthesis of high-quality and uniform graphene films on copper foils. Science 324:1312–1314

    Article  Google Scholar 

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

    Article  Google Scholar 

  17. Park S, An J, Piner RD, Jung I, Yang D, Velamakanni A, Ruoff RS (2008) Aqueous suspension and characterization of chemically modified graphene sheets. Chem Mater 20:6592–6594

    Article  Google Scholar 

  18. Li D, Kaner RB (2008) Graphene-based materials. Nat Nanotechnol 3:101

    Article  Google Scholar 

  19. Stankovich S, Piner RD, Chen X, Wu N, Nguyen ST, Ruoff RS (2006) Stable aqueous dispersions of graphitic nanoplatelets via the reduction of exfoliated graphite oxide in the presence of poly (sodium 4-styrenesulfonate). J Mater Chem 16:155–158

    Article  Google Scholar 

  20. Gao W, Alemany LB, Ci L, Ajayan PM (2009) New insights into the structure and reduction of graphite oxide. Nat chem 1:403–408

    Article  Google Scholar 

  21. Che J, Shen L, Xiao Y (2010) A new approach to fabricate graphene nanosheets in organic medium: combination of reduction and dispersion. J Mater Chem 20:1722–1727

    Article  Google Scholar 

  22. Wang G, Yang J, Park J, Gou X, Wang B, Liu H, Yao J (2008) Facile synthesis and characterization of graphene nanosheets. J Phys Chem C 112:8192–8195

    Article  Google Scholar 

  23. Fan X, Peng W, Li Y, Li X, Wang S, Zhang G, Zhang F (2008) Deoxygenation of exfoliated graphite oxide under alkaline conditions: a green route to graphene preparation. Adv Mater 20:4490–4493

    Article  Google Scholar 

  24. McAllister MJ, Li JL, Adamson DH, Schniepp HC, Abdala AA, Liu J, Aksay IA (2007) Single sheet functionalized graphene by oxidation and thermal expansion of graphite. Chem Mater 19:4396–4404

    Article  Google Scholar 

  25. Schniepp HC, Li JL, McAllister MJ, Sai H, Herrera-Alonso M, Adamson DH, Aksay IA (2006) Functionalized single graphene sheets derived from splitting graphite oxide. J Phys Chem B 110:8535–8539

    Article  Google Scholar 

  26. Becerril HA, Mao J, Liu Z, Stoltenberg RM, Bao Z, Chen Y (2008) Evaluation of solution-processed reduced graphene oxide films as transparent conductors. ACS Nano 2:463–470

    Article  Google Scholar 

  27. Wu ZS, Ren W, Gao L, Liu B, Jiang C, Cheng HM (2009) Synthesis of high-quality graphene with a pre-determined number of layers. Carbon 47:493–499

    Article  Google Scholar 

  28. Lv W, Tang DM, He YB, You CH, Shi ZQ, Chen XC, Yang QH (2009) Low-temperature exfoliated graphenes: vacuum-promoted exfoliation and electrochemical energy storage. ACS Nano 3:3730–3736

    Article  Google Scholar 

  29. Zhang HB, Wang JW, Yan Q, Zheng WG, Chen C, Yu ZZ (2011) Vacuum-assisted synthesis of graphene from thermal exfoliation and reduction of graphite oxide. J Mater Chem 21:5392–5397

    Article  Google Scholar 

  30. Liu F, Song S, Xue D, Zhang H (2012) Folded structured graphene paper for high performance electrode materials. Adv Mater 24:1089–1094

    Article  Google Scholar 

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

    Article  Google Scholar 

  32. Compton OC, Jain B, Dikin DA, Abouimrane A, Amine K, Nguyen ST (2011) Chemically active reduced graphene oxide with tunable C/O ratios. ACS Nano 5:4380–4391

    Article  Google Scholar 

  33. Acik M, Lee G, Mattevi C, Pirkle A, Wallace RM, Chhowalla M, Chabal Y (2011) The role of oxygen during thermal reduction of graphene oxide studied by infrared absorption spectroscopy. J Phys Chem C 115:19761–19781

    Article  Google Scholar 

  34. Ferrari AC, Meyer JC, Scardaci V, Casiraghi C, Lazzeri M, Mauri F, Geim AK (2006) Raman spectrum of graphene and graphene layers. Phys Rev Lett 97:187401

    Article  Google Scholar 

  35. Kudin KN, Ozbas B, Schniepp HC, Prud’Homme RK, Aksay IA, Car R (2008) Raman spectra of graphite oxide and functionalized graphene sheets. Nano Lett 8:36–41

    Article  Google Scholar 

  36. Kaniyoor A, Baby TT, Ramaprabhu S (2010) Graphene synthesis via hydrogen induced low temperature exfoliation of graphite oxide. J Mater Chem 20:8467–8469

    Article  Google Scholar 

  37. Beamson G, Briggs D (1992) High-resolution XPS of organic polymers, the scienta ESCA 300 database. John Wiley & Sons, Chichester

    Google Scholar 

  38. Ganguly A, Sharma S, Papakonstantinou P, Hamilton J (2011) Probing the thermal deoxygenation of graphene oxide using high-resolution in situ X-ray-based spectroscopies. J Phys Chem C 115:17009–17019

    Article  Google Scholar 

  39. Niyogi S, Bekyarova E, Itkis ME, McWilliams JL, Hamon MA, Haddon RC (2006) Solution properties of graphite and graphene. J Am Chem Soc 128:7720–7721

    Article  Google Scholar 

  40. Stankovich S, Dikin DA, Dommett GH, Kohlhaas KM, Zimney EJ, Stach EA, Ruoff RS (2006) Graphene-based composite materials. Nature 442:282–286

    Article  Google Scholar 

  41. Villar-Rodil S, Paredes JI, Martínez-Alonso A, Tascón JM (2009) Preparation of graphene dispersions and graphene-polymer composites in organic media. J Mater Chem 19:3591–3593

    Article  Google Scholar 

  42. Cao Y, Feng J, Wu P (2010) Preparation of organically dispersible graphene nanosheet powders through a lyophilization method and their poly (lactic acid) composites. Carbon 48:3834–3839

    Article  Google Scholar 

  43. El-Kady MF, Strong V, Dubin S, Kaner RB (2012) Laser scribing of high-performance and flexible graphene-based electrochemical capacitors. Science 335:1326–1330

    Article  Google Scholar 

Download references

Acknowledgements

The financial supports from Natural Science Foundation of China (20804004 and 21274071), Taishan Mountain Scholar Constructive Engineering Foundation (TS20081120), and Natural Science Fund for Distinguished Young Scholars of Shandong Province (JQ200905) are greatly appreciated.

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Correspondence to Jianming Zhang.

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Wan, L., Liu, P., Zhang, T. et al. Exfoliation and reduction of graphene oxide at low temperature and its resulting electrocapacitive properties. J Mater Sci 49, 4989–4997 (2014). https://doi.org/10.1007/s10853-014-8201-8

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  • DOI: https://doi.org/10.1007/s10853-014-8201-8

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