Journal of Materials Science

, Volume 51, Issue 24, pp 10782–10792 | Cite as

Ultrasonic cavitation effects on the structure of graphene oxide in aqueous suspension

  • P. Pérez-Martínez
  • J. M. Galvan-Miyoshi
  • J. Ortiz-López
Original Paper


Ultrasonic treatments are a common procedure to exfoliate graphite oxide for the preparation of graphene oxide flakes in aqueous suspension. High-power ultrasonic instrumentation is capable to produce cavitation on the solution that may cause undesirable side effects on the structure and properties of graphene oxide flakes. In this work, we investigate the effects of cavitation on graphite oxide pH neutral aqueous suspensions by monitoring its structural and optical properties as a function of exposure time to ultrasonic cavitation (UC). From analysis of the evolution of these properties, we identify three stages in which both flake exfoliation and fragmentation evolve, including partial reduction caused by removal of oxygen moieties due to the harsh mechanical vibrations and thermal effects produced by UC. Photoluminescence emission red-shifts due to the appearance of low lying excited defect energy levels caused by long exposure to UC.


Graphene Oxide Cavitation Graphite Oxide Cavitation Bubble Sonication Time 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.



This research was funded by Instituto Politecnico Nacional (IPN) Secretaria de Investigacion y Posgrado through Projects Numbers 20130427, 20140184, and 20150364. We acknowledge partial financial support from FESE-COMEX Project “Investigacion para la Vinculacion 2014.″ We are grateful to Centro Nanociencias y MicroNanotecnologias-IPN for TEM and XRD analyses. PPM thanks Consejo Nacional de Ciencia y Tecnologia for support through a scholarship and PPG-COMEX, CIP for support through project I + D+I FESE-COMEX. JOL thanks EDI-IPN and COFAA-IPN for support through academic fellowships.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.


  1. 1.
    Wu J, Agrawal M, Becerril HA, Bao Z, Liu Z, Chen Y, Peumans P (2010) Organic light-emitting diodes on solution-processed graphene transparent electrodes. ACS Nano 4:43–48CrossRefGoogle Scholar
  2. 2.
    Hummers WS, Offeman RE (1958) Preparation of graphitic oxide. J Am Chem Soc 80:1339–1370CrossRefGoogle Scholar
  3. 3.
    Szabó T, Berkesi O, Forgó P, Josepovits K, Sanakis Y, Petridis D, Dékány I (2006) Evolution of surface functional groups in a series of progressively oxidized graphite oxides. Chem Mater 18:2740–2749CrossRefGoogle Scholar
  4. 4.
    Bagri A, Mattevi C, Acik M, Chabal YJ, Chhowalla M, Shenoy VB (2010) Structural evolution during the reduction of chemically derived graphene oxide. Nat Chem 2:581–587CrossRefGoogle Scholar
  5. 5.
    Mathkar A, Tozier D, Cox P, Ong P, Galande C, Balakrishnan K, Reddy ALM, Ajayan PM (2012) Controlled, stepwise reduction and band gap manipulation of graphene oxide. J Phys Chem Lett 3:986–991CrossRefGoogle Scholar
  6. 6.
    Velasco-Soto MA, Perez-Garcıa SA, Alvarez-Quintana J, Cao Y, Nyborg L, Licea-Jimenez L (2015) Selective band gap manipulation of graphene oxide by its reduction with mild reagents. Carbon 93:967–973CrossRefGoogle Scholar
  7. 7.
    Stankovich S, Dikin DA, Piner RD, Kohlhaas KA, Kleinhammes A, Jia Y, Wu Y, Nguyen ST, Ruoff RS (2007) Synthesis of graphene-based nanosheets via chemical reduction of exfoliated graphite oxide. Carbon 45:1558–1565CrossRefGoogle Scholar
  8. 8.
    Thompson LH, Doraiswamy LK (1999) Sonochemistry: science and engineering. Ind Eng Chem Res 38:1215–1249CrossRefGoogle Scholar
  9. 9.
    ASTM D2369-10 (Reapproved 2015) Standard test method for volatile content of coatings, ASTM International Accessed 7 Jan 2015
  10. 10.
    Suslick KS (1990) Sonochemistry. Science 247:1438–1445CrossRefGoogle Scholar
  11. 11.
    Wu TY, Guo N, Teh CY, Hay JXW (2013) Advances in ultrasound technology for environmental remediation. Theory and fundamentals of ultrasound. Springer, Netherlands, pp 5–12Google Scholar
  12. 12.
    Adewuyi YG (2001) Sonochemistry: environmental science and engineering, applications. Ind Eng Chem Res 40:4681–4715CrossRefGoogle Scholar
  13. 13.
    Sun H, Yang Y, Huang Q (2011) Preparation and structural variation of graphite oxide and graphene oxide. Integr Ferroelectr 128:163–170CrossRefGoogle Scholar
  14. 14.
    Botas C, Álvarez P, Blanco P, Granda M, Blanco C, Santamaría R, Romasanta LJ et al (2013) Graphene materials with different structures prepared from the same graphite by the Hummers and Brodie methods. Carbon 65:156–164CrossRefGoogle Scholar
  15. 15.
    Zhou T, Chen F, Liu K, Deng H, Zhang Q, Feng J, Fu Q (2011) A simple and efficient method to prepare graphene by reduction of graphite oxide with sodium hydrosulfite. Nanotechnology 22:045704–045707CrossRefGoogle Scholar
  16. 16.
    Marcano DC, Kosynkin DV, Berlin JM, Sinitskii A, Sun Z, Slesarev A, Alemany LB et al (2010) Improved synthesis of graphene oxide. ACS Nano 4:4806–4814CrossRefGoogle Scholar
  17. 17.
    Huh SH (2011) Physics and applications of graphene—experiments. In: Mikhailov S (ed) Thermal reduction of graphene oxide InTech. Accessed 18 Apr 2016
  18. 18.
    Paredes JI, Villar-Rodil S, Martínez-Alonso A, Tascón JMD (2008) Graphene oxide dispersions in organic solvents. Langmuir 24:10560–10564CrossRefGoogle Scholar
  19. 19.
    Tan PH, Dimovski S, Gogotsi Y (2004) Raman scattering of non-planar graphite: arched edges, polyhedral crystals, whiskers and cones. Phil Trans R Soc Lond A 362:2289–2310CrossRefGoogle Scholar
  20. 20.
    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 8:36–41CrossRefGoogle Scholar
  21. 21.
    Shang J, Ma L, Li J, Ai W, Yu T, Gurzadyan GG (2012) The origin of fluorescence from graphene oxide. Sci Rep 2:792. doi: 10.1038/srep00792 CrossRefGoogle Scholar
  22. 22.
    Galande C, Mohite AD, Naumov AV, Gao W, Ci L, Ajayan A, Gao H, Srivastava A, Weisman RB, Ajayan PM (2011) Quasi-molecular fluorescence from graphene oxide. Sci Rep 1:85. doi: 10.1038/srep00085 CrossRefGoogle Scholar
  23. 23.
    Eda G, Lin YY, Mattevi C, Yamaguchi H, Chen HA, Chen IS, Chen CW, Chhowalla M (2010) Blue photoluminescence from chemically derived graphene oxide. Adv Mater 22:505–509CrossRefGoogle Scholar
  24. 24.
    Luo Z, Vora PM, Mele EJ, Johnson ATC, Kikkawaa JM (2009) Photoluminescence and band gap modulation in graphene oxide. Appl Phys Lett 94:111909CrossRefGoogle Scholar
  25. 25.
    Chien CT, Li SS, Lai WJ, Yeh YC, Chen HA, Chen IS, Chen LC, Chen KH, Nemoto T, Isoda S, Chen M, Fujita T, Eda G, Yamaguchi H, Chhowalla M, Chen CW (2012) Tunable photoluminescence from graphene oxide. Angew Chem Int Ed 51:6662–6666. doi: 10.1002/anie.201200474 CrossRefGoogle Scholar
  26. 26.
    Maiti R, Midya A, Narayana C, Ray SK (2014) Tunable optical properties of graphene oxide by tailoring the oxygen functionalities using infrared irradiation. Nanotechnology 25:495704CrossRefGoogle Scholar
  27. 27.
    Subrahmanyam KS, Kumar P, Nag A, Rao CNR (2010) Blue light emitting graphene-based materials and their use in generating white light. Solid State Commun 150:1774–1777CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media New York 2016

Authors and Affiliations

  1. 1.Departamento de FísicaInstituto Politécnico Nacional, ESFMMexico CityMexico
  2. 2.Centro de Investigación en Polímeros, PPG-COMEXTepexpanMexico

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