Power Parameter Analysis in the Electrochemical Graphite Exfoliation for Graphene Fabrication
Received: 29 January 2025 | Revised: 26 April 2025 | Accepted: 8 May 2025 | Online: 2 August 2025
Corresponding author: Anif Jamaluddin
Abstract
Electrochemical exfoliation is considered an essential method for the rapid production of graphene in both high quality and quantity. This study investigates the electrochemical exfoliation of graphite rods, specifically the impact of the power variations in a Direct Current (DC) source on the quality of graphene. Furthermore, Scanning Electron Microscope-Energy Dispersive X-Ray (SEM-EDX) is employed to analyze the morphology and elemental composition. In addition, Fourier Transform Infrared (FTIR) spectroscopy is utilized to determine the functional groups of graphene. The defect of graphite is observed with Raman spectroscopy. The SEM results suggest that graphene layers are formed in all the power variations. Graphene at 98 W (G98) exhibits a wrinkle and cluttered surface compared to graphene at 70 W (G70) and graphene at 84 W (G84). Based on the FTIR results, the highest peak of C=O bond appeared in G70, while sharp peaks indicating O-H bonds are observed in G84 and G98. Furthermore, the power analysis is a critical factor affecting graphene mass production, with higher power levels resulting in higher graphene yield, but lower graphene quality by reducing the carbon (C) content and increasing Oxygen (O) content. This exploration contributes to advancing the understanding of the electrochemical exfoliation process, offering insights into optimizing the power parameters for enhanced graphene synthesis.
Keywords:
graphene, electrochemical exfoliation, functional group, surface morphology, powerDownloads
References
A. A. Moosa, Z. H. Mahdi, and M. A. Mutar, "Preparation of Graphene Oxide from Expanded Graphite at Different Microwave Heating Times," Journal of Engineering and Technological Sciences, vol. 53, no. 3, pp. 210305–210305, Jun. 2021. DOI: https://doi.org/10.5614/j.eng.technol.sci.2021.53.3.5
A. Ambrosi, C. K. Chua, A. Bonanni, and M. Pumera, "Electrochemistry of Graphene and Related Materials," Chemical Reviews, vol. 114, no. 14, pp. 7150–7188, Jun. 2014. DOI: https://doi.org/10.1021/cr500023c
F. Jeschull et al., "Graphite Particle-Size Induced Morphological and Performance Changes of Graphite–Silicon Electrodes," Journal of The Electrochemical Society, vol. 167, no. 10, Mar. 2020, Art. no. 100535. DOI: https://doi.org/10.1149/1945-7111/ab9b9a
R. Mirea, "Advanced Graphite/Metal Composite Materials for High Voltage Automotive Applications," Engineering, Technology & Applied Science Research, vol. 14, no. 5, pp. 17302–17307, Oct. 2024. DOI: https://doi.org/10.48084/etasr.7988
D. A. C. Brownson, G. C. Smith, and C. E. Banks, "Graphene oxide electrochemistry: the electrochemistry of graphene oxide modified electrodes reveals coverage dependent beneficial electrocatalysis," Royal Society Open Science, vol. 4, no. 11, Nov. 2017, Art. no. 171128. DOI: https://doi.org/10.1098/rsos.171128
K. Kakaei, "One-pot electrochemical synthesis of graphene by the exfoliation of graphite powder in sodium dodecyl sulfate and its decoration with platinum nanoparticles for methanol oxidation," Carbon, vol. 51, pp. 195–201, Jan. 2013. DOI: https://doi.org/10.1016/j.carbon.2012.08.028
R. B. Kohakade, E. S. Kumar, R. W. Gaikwad, S. Raghu, and R. A. Kalaivani, "Electrochemical Surface Oxidation of Graphite Electrode and Its Superior Sensitive Platform For Electrochemical Sensors," Rasayan Journal of Chemistry, vol. 10, no. 4, pp. 1151–1158.
J. Mei et al., "Process regulation of the electrochemical exfoliation for graphene production with graphite powder as starting materials," Journal of Materials Science, vol. 58, no. 22, pp. 9116–9129, May 2023. DOI: https://doi.org/10.1007/s10853-023-08601-5
E. Yoo, J. Kim, E. Hosono, H. Zhou, T. Kudo, and I. Honma, "Large Reversible Li Storage of Graphene Nanosheet Families for Use in Rechargeable Lithium Ion Batteries," Nano Letters, vol. 8, no. 8, pp. 2277–2282, Jun. 2008. DOI: https://doi.org/10.1021/nl800957b
D. Lee and J. Seo, "Layer-by-layer-stacked graphene/graphene-island supercapacitor," AIP Advances, vol. 10, no. 5, May 2020, Art. no. 055202. DOI: https://doi.org/10.1063/5.0007887
N. P. Sari, D. Dutta, A. Jamaluddin, J.-K. Chang, and C.-Y. Su, "Controlled multimodal hierarchically porous electrode self-assembly of electrochemically exfoliated graphene for fully solid-state flexible supercapacitor," Physical Chemistry Chemical Physics, vol. 19, no. 45, pp. 30381–30392, Nov. 2017. DOI: https://doi.org/10.1039/C7CP05799G
A. Jamaluddin, B. Umesh, F. Chen, J.-K. Chang, and C.-Y. Su, "Facile synthesis of core–shell structured Si@graphene balls as a high-performance anode for lithium-ion batteries," Nanoscale, vol. 12, no. 17, pp. 9616–9627, May 2020. DOI: https://doi.org/10.1039/D0NR01346C
M. U. Arshad et al., "Multi-functionalized fluorinated graphene composite coating for achieving durable electronics: Ultralow corrosion rate and high electrical insulating passivation," Carbon, vol. 195, pp. 141–153, Apr. 2022. DOI: https://doi.org/10.1016/j.carbon.2022.04.004
A. Peyravi, F. Ahmadijokani, M. Arjmand, and Z. Hashisho, "Graphene oxide enhances thermal stability and microwave absorption/regeneration of a porous polymer," Journal of Hazardous Materials, vol. 433, p. 128792, Jul. 2022. DOI: https://doi.org/10.1016/j.jhazmat.2022.128792
M. Cai, D. Thorpe, D. H. Adamson, and H. C. Schniepp, "Methods of graphite exfoliation," Journal of Materials Chemistry, vol. 22, no. 48, pp. 24992–25002, Nov. 2012. DOI: https://doi.org/10.1039/c2jm34517j
Y. Yang, F. Lu, Z. Zhou, W. Song, Q. Chen, and X. Ji, "Electrochemically cathodic exfoliation of graphene sheets in room temperature ionic liquids N-butyl, methylpyrrolidinium bis(trifluoromethylsulfonyl)imide and their electrochemical properties," Electrochimica Acta, vol. 113, pp. 9–16, Sep. 2013, https://doi.org/10.1016/j.electacta.2013.09.031.
M. Yusuf, M. Kumar, M. A. Khan, M. Sillanpää, and H. Arafat, "A review on exfoliation, characterization, environmental and energy applications of graphene and graphene-based composites," Advances in Colloid and Interface Science, vol. 273, Oct. 2019, Art. no. 102036. DOI: https://doi.org/10.1016/j.cis.2019.102036
L. Saikam, P. Arthi, B. Senthil, and M. Shanmugam, "A review on exfoliated graphite: Synthesis and applications," Inorganic Chemistry Communications, vol. 152, Apr. 2023, Art. no. 110685. DOI: https://doi.org/10.1016/j.inoche.2023.110685
A. Agrawal, "Top-down strategies for achieving high-quality graphene: Recent advancements," Journal of Industrial and Engineering Chemistry, vol. 142, pp. 103–126, Dec. 2024. DOI: https://doi.org/10.1016/j.jiec.2024.07.053
Y. Yang, F. Lu, Z. Zhou, W. Song, Q. Chen, and X. Ji, "Electrochemically cathodic exfoliation of graphene sheets in room temperature ionic liquids N-butyl, methylpyrrolidinium bis(trifluoromethylsulfonyl)imide and their electrochemical properties," Electrochimica Acta, vol. 113, pp. 9–16, Nov. 2013. DOI: https://doi.org/10.1016/j.electacta.2013.09.031
A. Gutiérrez-Cruz, A. R. Ruiz-Hernández, J. F. Vega-Clemente, D. G. Luna-Gazcón, and J. Campos-Delgado, "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, vol. 57, no. 31, pp. 14543–14578, Aug. 2022. DOI: https://doi.org/10.1007/s10853-022-07514-z
K. Parvez et al., "Exfoliation of Graphite into Graphene in Aqueous Solutions of Inorganic Salts," Journal of the American Chemical Society, vol. 136, no. 16, pp. 6083–6091, Mar. 2014. DOI: https://doi.org/10.1021/ja5017156
Y. Zhang, Y. Xu, Y. Niu, W. Hou, and R. Liu, "Highly efficient dual-electrode exfoliation of graphite into high-quality graphene via square-wave alternating currents," Chemical Engineering Journal, vol. 456, Dec. 2022, Art. no. 140977. DOI: https://doi.org/10.1016/j.cej.2022.140977
D. Ehjeij et al., "Electrochemical Exfoliation of Graphene and Formation of its Copolyamide 6/66 Nanocomposites by Wet Phase Inversion and Injection Molding," Macromolecular Chemistry and Physics, vol. 226, no. 1, Oct. 2025, Art. no. 2400320. DOI: https://doi.org/10.1002/macp.202400320
X. Zhao et al., "Electrochemical exfoliation of graphene as an anode material for ultra-long cycle lithium ion batteries," Journal of Physics and Chemistry of Solids, vol. 139, Dec. 2019, Art. no. 109301. DOI: https://doi.org/10.1016/j.jpcs.2019.109301
T. N. J. I. Edison et al., "Electrochemically exfoliated graphene sheets as electrode material for aqueous symmetric supercapacitors," Surface and Coatings Technology, vol. 416, Apr. 2021, Art. no. 127150. DOI: https://doi.org/10.1016/j.surfcoat.2021.127150
W.-W. Liu and A. Aziz, "Review on the Effects of Electrochemical Exfoliation Parameters on the Yield of Graphene Oxide," ACS Omega, vol. 7, no. 38, pp. 33719–33731, Sep. 2022. DOI: https://doi.org/10.1021/acsomega.2c04099
P. K. M. K, S. Shanthini, and C. Srivastava, "Electrochemical exfoliation of graphite for producing graphene using saccharin," RSC Advances, vol. 5, no. 66, pp. 53865–53869, Jun. 2015. DOI: https://doi.org/10.1039/C5RA07846F
S. Tian et al., "One-step fast electrochemical fabrication of water-dispersible graphene," Carbon, vol. 111, pp. 617–621, Oct. 2016. DOI: https://doi.org/10.1016/j.carbon.2016.10.044
M. Coroş et al., "Simple and cost-effective synthesis of graphene by electrochemical exfoliation of graphite rods," RSC Advances, vol. 6, no. 4, pp. 2651–2661, Jan. 2016. DOI: https://doi.org/10.1039/C5RA19277C
A. Taheri Najafabadi and E. Gyenge, "Synergistic production of graphene microsheets by simultaneous anodic and cathodic electro-exfoliation of graphitic electrodes in aprotic ionic liquids," Carbon, vol. 84, pp. 449–459, Dec. 2014. DOI: https://doi.org/10.1016/j.carbon.2014.12.041
F. Alabdo, W. Alahmad, U. Pengsomjit, M. Halabi, P. Varanusupakul, and C. Kraiya, "An environmentally friendly and simple method for producing multi-layer exfoliated graphene in mass production from pencil graphite and its utilization for removing cadmium from an aqueous medium," Carbon Letters, vol. 33, no. 2, pp. 455–465, Nov. 2022. DOI: https://doi.org/10.1007/s42823-022-00435-6
N. N. Aida, M. Ikhsanudin, A. Jamaludin, A. Nur’aini, E. L. Septiani, and H. Widiyandari, "Synthesis of Graphene from Pencils Graphite Via Electrochemical Exfoliation Method as a Cu-Foil Coating on the Anode-Free Lithium-Ion Battery," ALCHEMY Jurnal Penelitian Kimia, vol. 20, no. 1, pp. 31–37, Mar. 2024. DOI: https://doi.org/10.20961/alchemy.20.1.74620.31-37
T. C. Achee et al., "High-yield scalable graphene nanosheet production from compressed graphite using electrochemical exfoliation," Scientific Reports, vol. 8, no. 1, Sep. 2018, Art. no. 14525. DOI: https://doi.org/10.1038/s41598-018-32741-3
A. A. Muhsan and K. Lafdi, "Numerical study of the electrochemical exfoliation of graphite," SN Applied Sciences, vol. 1, no. 3, Feb. 2019, Art. no. 276. DOI: https://doi.org/10.1007/s42452-019-0296-8
S. Vadivel, W. Tejangkura, and M. Sawangphruk, "Graphite/Graphene Composites from the Recovered Spent Zn/Carbon Primary Cell for the High-Performance Anode of Lithium-Ion Batteries," ACS Omega, vol. 5, no. 25, pp. 15240–15246, Jun. 2020. DOI: https://doi.org/10.1021/acsomega.0c01270
S. H. Ilias, J. A. Murshidi, and K. K. Ying, "Effect of electrolyte concentration on the synthesis of graphene by electrochemical exfoliation process," IOP Conference Series: Materials Science and Engineering, vol. 1106, no. 1, Nov. 2021, Art. no. 012013. DOI: https://doi.org/10.1088/1757-899X/1106/1/012013
R. Patil, H. Patel, S. B. Pillai, P. K. Jha, P. Bahadur, and S. Tiwari, "Influence of surface oxygen clusters upon molecular stacking of paclitaxel over graphene oxide sheets," Materials Science & Engineering. C, Materials for Biological Applications, vol. 116, Jun. 2020, Art. no. 111232. DOI: https://doi.org/10.1016/j.msec.2020.111232
V. Ţucureanu, Matei ,Alina, and A. M. and Avram, "FTIR Spectroscopy for Carbon Family Study," Critical Reviews in Analytical Chemistry, vol. 46, no. 6, pp. 502–520, Jun. 2016. DOI: https://doi.org/10.1080/10408347.2016.1157013
S. Sedaghat, M. M. Ahadian, M. Jafarian, and S. Hatamie, "Model Fuel Deep Desulfurization Using Modified 3D Graphenic Adsorbents: Isotherm, Kinetic, and Thermodynamic Study," Industrial & Engineering Chemistry Research, vol. 58, no. 24, pp. 10341–10351, May 2019. DOI: https://doi.org/10.1021/acs.iecr.9b00250
Y. Chen et al., "Updated understandings on coke formation during the inferior heavy oil in-situ combustion process: A combined FTIR, XPS, TG/DTG, and DSC study," Sustainable Energy Technologies and Assessments, vol. 65, Apr. 2024, Art. no. 103772. DOI: https://doi.org/10.1016/j.seta.2024.103772
M. Ostermann, L. Kalchgruber, J. Schodl, P. Lieberzeit, P. Bilotto, and M. Valtiner, "Tailoring the properties of graphene nanosheets during electrochemical exfoliation," Carbon Trends, vol. 18, Dec. 2024, Art. no. 100449. DOI: https://doi.org/10.1016/j.cartre.2024.100449
E. A. Ganash, G. A. Al-Jabarti, and R. M. Altuwirqi, "The synthesis of carbon-based nanomaterials by pulsed laser ablation in water," Materials Research Express, vol. 7, no. 1, Nov. 2019, Art. no. 015002. DOI: https://doi.org/10.1088/2053-1591/ab572b
S. Li, J. Zhang, M. Liu, R. Wang, and L. Wu, "Influence of polyethyleneimine functionalized graphene on tribological behavior of epoxy composite," Polymer Bulletin, vol. 78, no. 11, pp. 6493–6515, Oct. 2020. DOI: https://doi.org/10.1007/s00289-020-03439-2
M. Eredia et al., "Morphology and Electronic Properties of Electrochemically Exfoliated Graphene," The Journal of Physical Chemistry Letters, vol. 8, no. 14, pp. 3347–3355, Jul. 2017. DOI: https://doi.org/10.1021/acs.jpclett.7b01301
A. C. Ferrari et al., "Raman Spectrum of Graphene and Graphene Layers," Physical Review Letters, vol. 97, no. 18, Oct. 2006, Art. no. 187401. DOI: https://doi.org/10.1103/PhysRevLett.97.187401
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Copyright (c) 2025 Nur Afifah Muthmainnah, Hendri Widiyandari, Lita Rahmasari, Yulianto Agung Rezeki, Andita Nataria Fitri Ganda, Suriani Abu Bakar, Sri Budiawanti, Anif Jamaluddin
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