Skip to main content
Log in

High-yield production of graphene flakes using a novel electrochemical/mechanical hybrid exfoliation

  • ORIGINAL ARTICLE
  • Published:
The International Journal of Advanced Manufacturing Technology Aims and scope Submit manuscript

Abstract

This research aims to develop a novel hybrid process of an electrochemical intercalation and mechanical exfoliation for fabricating graphene flakes. Using a rotational tool as electrode, the graphite powders were electrochemically intercalated using ions in electrolyte, and then the expanded graphite powders were mechanically exfoliated for few-layer graphene flakes. To obtain the high-quality graphene flakes, the graphite powders were intercalated in the mixed electrolyte of myristyl alcohol surfactant added in H2SO4 solution at the speed of the rotational tool of 2000 rpm and the applied voltage of ± 4 V for 1 h, and then the expanded graphite powders were mechanically exfoliated at the speed of the rotational tool of 10000 rpm for 1 h. The average thickness and lateral size of the graphene flakes was 1.42 nm and 0.5 μm measured by an atomic force microscope, respectively. The maximum C/O and I2D/IG ratios of graphene flakes were 22.29 and 1.22 analyzed by an X-ray photoelectron spectroscope and a Raman spectrometer, respectively. Besides, the production yield of the exfoliated few-layer graphene flakes was evaluated that could achieve to 20%, which was approximately 2 times more than the pure electrochemical or pure mechanical exfoliation methods.

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

Access this article

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

Instant access to the full article PDF.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9
Fig. 10
Fig. 11

Similar content being viewed by others

References

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

    Article  Google Scholar 

  2. Bonaccorso F, Lombardo A, Hasan T, Sun Z, Colombo L, Ferrari AC (2012) Production and processing of graphene and 2d crystals. Mater Today 15:564–589

    Article  Google Scholar 

  3. Karamat S, Çelik K, Shah Zaman S, Oral A (2018) Multilayer graphene growth on polar dielectric substrates using chemical vapour deposition. Appl Surf Sci 442:720–725

    Article  Google Scholar 

  4. Mendoza CD, Caldas PG, Freire FL, Maia da Costa MEH (2018) Growth of single-layer graphene on Ge (1 0 0) by chemical vapor deposition. Appl Surf Sci 447:816–821

    Article  Google Scholar 

  5. Qiao D, Song J, Zhang H, Liu Q, Zhang Y, Jing L, He P (2018) The adsorption geometry and molecular self-assembly of graphene for 1,3,5-triphenylbenzene on Cu(111). Surf Sci 675:42–46

    Article  Google Scholar 

  6. Song J, Zhang H, Zhang Y, Cai Y, Bao S, He P (2016) Scanning tunneling microscopy and density functional theory investigations on molecular self-assembly of graphene on Ru(0001). Appl Surf Sci 367:424–431

    Article  Google Scholar 

  7. Kruskopf M, Pierz K, Pakdehi DM, Wundrack S, Stosch R, Bakin A, Schumacher HW (2018) A morphology study on the epitaxial growth of graphene and its buffer layer. Thin Solid Films 659:7–15

    Article  Google Scholar 

  8. Lundin WV, Zavarin EE, Sakharov AV, Zakheim DA, Davydov VY, Smirnov AN, Eliseyev IA, Yagovkina MA, Brunkov PN, Lundina EY, Markov LK, Tsatsulnikov AF (2018) Growth of III-N/graphene heterostructures in single vapor phase epitaxial process. J Cryst Growth 504:1–6

    Article  Google Scholar 

  9. Zhang Y, Liu F (2016) Laser induced domino exfoliation of graphite to graphene in spheroidal graphite cast iron. Surf Coat Technol 285:235–241

    Article  Google Scholar 

  10. Qian M, Zhou YS, Gao Y, Feng T, Sun Z, Jiang L, Lu YF (2012) Production of few-layer graphene through liquid-phase pulsed laser exfoliation of highly ordered pyrolytic graphite. Appl Surf Sci 258:9092–9095

    Article  Google Scholar 

  11. Lapshin RV (2016) STM observation of a box-shaped graphene nanostructure appeared after mechanical cleavage of pyrolytic graphite. Appl Surf Sci 360:451–460

    Article  Google Scholar 

  12. Gu S, Hsieh CT, Chiang YM, Tzou DY, Chen YF, Gandomi YA (2018) Optimization of graphene quantum dots by chemical exfoliation from graphite powders and carbon nanotubes. Mater Chem Phys 215:104–111

    Article  Google Scholar 

  13. Yang CR, Tseng SF, Chen YT (2018) Characteristics of graphene oxide films reduced by using an atmospheric plasma system. Nanomaterials 8:802

    Article  Google Scholar 

  14. Liu M, Zhang X, Wu W, Liu T, Liu Y, Guo B, Zhang R (2019) One-step chemical exfoliation of graphite to ∼100% few-layer graphene with high quality and large size at ambient temperature. Chem Eng J 355:181–185

    Article  Google Scholar 

  15. Yang CR, Tseng SF, Chen YT (2018) Laser-induced reduction of graphene oxide powders by high pulsed ultraviolet laser irradiations. Appl Surf Sci 444:578–583

    Article  Google Scholar 

  16. Mir A, Shukla A (2018) Bilayer-rich graphene suspension from electrochemical exfoliation of graphite. Mater Des 156:62–70

    Article  Google Scholar 

  17. Bakhshandeh R, Shafiekhani A (2018) Ultrasonic waves and temperature effects on graphene structure fabricated by electrochemical exfoliation method. Mater Chem Phys 212:95–102

    Article  Google Scholar 

  18. He M, Guo X, Huang J, Shen H, Zeng Q, Wang L (2018) Mass production of tunable multicolor graphene quantum dots from an energy resource of coke by a one-step electrochemical exfoliation. Carbon 140:508–520

    Article  Google Scholar 

  19. Paton KR, Varrla E, Backes C, Smith RJ, Khan U, O’Neill A, Boland C, Lotya M, Istrate OM, King P, Higgins T, Barwich S, May P, Puczkarski P, Ahmed I, Moebius M, Pettersson H, Long E, Coelho J, O’Brien SE, McGuire EK, Sanchez BM, Duesberg GS, McEvoy N, Pennycook TJ (2014) Scalable production of large quantities of defect-free few-layer graphene by shear exfoliation in liquids. Nat Mater 13:624–630

    Article  Google Scholar 

  20. Liu L, Shen Z, Yi M, Zhang X, Ma S (2014) A green, rapid and size-controlled production of high-quality graphene sheets by hydrodynamic forces. RSC Adv 4:36464–36470

    Article  Google Scholar 

  21. Yi M, Shen Z (2014) Kitchen blender for producing high-quality few-layer graphene. Carbon 78:622–626

    Article  Google Scholar 

  22. Varrla E, Paton KR, Backes C, Harvey A, Smith RJ, McCauley J, Coleman JN (2014) Turbulence-assisted shear exfoliation of graphene using household detergent and a kitchen blender. Nanoscale 6:11810–11819

    Article  Google Scholar 

  23. Gong Y, Ping Y, Li D, Luo C, Ruan X, Fu Q, Pan C (2017) Preparation of high-quality graphene via electrochemical exfoliation & spark plasma sintering and its applications. Appl Surf Sci 397:213–219

    Article  Google Scholar 

  24. Chen K, Xue D (2014) Preparation of colloidal graphene in quantity by electrochemical exfoliation. J Colloid Interface Sci 436:41–46

    Article  Google Scholar 

  25. Tian J, Guo L, Yin X, Wu W (2019) The liquid-phase preparation of graphene by shear exfoliation with graphite oxide as a dispersant. Mater Chem Phys 223:1–8

    Article  Google Scholar 

  26. Li L, Xu J, Li G, Jia X, Li Y, Yang F, Zhang L, Xu C, Gao J, Liu Y, Fang Z (2016) Preparation of graphene nanosheets by shear-assisted supercritical CO2 exfoliation. Chem Eng J 284:78–84

    Article  Google Scholar 

  27. Guo L, Yin X, Wu W, Meng H (2017) Preparation of graphene via liquid-phase exfoliation with high gravity technology from edge-oxidized graphite. Colloids Surf A Physicochem Eng Asp 531:25–31

    Article  Google Scholar 

  28. Ferrari AC, Basko DM (2013) Raman spectroscopy as a versatile tool for studying the properties of graphene. Nat Nanotechnol 8:235–246

    Article  Google Scholar 

  29. Tseng SF, Hsiao WT, Cheng PY, Lin YS, Chang TL, Chung CK (2017) Laser structuring of parallel electrode array on graphene/glass substrates for rapid inspections of moisturizing efficacy. Int J Adv Manuf Technol 91:3663–3671

    Article  Google Scholar 

  30. Nguyen VT, Le HD, Nguyen VC, Ngo TTT, Le DQ, Nguyen XN, Phan NM (2013) Synthesis of multi-layer graphene films on copper tape by atmospheric pressure chemical vapor deposition method. Adv Nat Sci Nanosci Nanotechnol 4:035012

    Article  Google Scholar 

Download references

Funding

We thank the Ministry of Science and Technology of Taiwan for financially supporting this research under projects MOST 107-2221-E-027-129-MY2 and MOST 107-2622-E-027-019-CC3.

Author information

Authors and Affiliations

Authors

Corresponding authors

Correspondence to Shih-Feng Tseng or Chii-Rong Yang.

Additional information

Publisher’s note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Teng, TP., Chang, SC., Chen, ZY. et al. High-yield production of graphene flakes using a novel electrochemical/mechanical hybrid exfoliation. Int J Adv Manuf Technol 104, 2751–2760 (2019). https://doi.org/10.1007/s00170-019-04158-3

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00170-019-04158-3

Keywords

Navigation