Synthesis and Characterization of Electrochemically Reduced Graphene Oxide for Applications in Supercapacitors
DOI:
https://doi.org/10.18321/cpc24(3)269-286Keywords:
graphene oxide, reduced graphene oxide, electrochemical reduction, cyclic voltammetry, supercapacitor, energy storageAbstract
Graphene oxide (GO) was prepared from graphite by the modified Hummers’ method using strong oxidizing agents which was reduced removing its oxygen-containing functional groups. sp2 carbon domains in GO material do not allow for electron transferring due to tight geometry and higher electronegativity of sp2 orbitals than sp3 carbon centers. Successful synthesis of GO from graphite powder was confirmed by X-ray diffraction (XRD) technique showing a diffraction peak 2θ = ~9.8°. Further, GO reduction procedures were performed through electrochemical (three-electrode cell, 1 M KOH, potential range from 0 to -1.2 V) and chemical (1 M ascorbic asid, 60 °C, stirring) methods. Morphological (scanning electron microscopy (SEM) and transmission electron microscopy (TEM)), structural (X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy) and thermal (thermogravimetric analysis (TGA)) analyses confirmed the removal of oxygen-containing groups, indicating conversion from GO to reduced GO (rGO). The electrochemical characteristics (CV, GCD, EIS) were investigated in a symmetric two-electrode Swagelok-type cell using 1 M NaNO3. Based on the obtained results, the most promising material was electrochemically reduced graphene oxide (E-RGO), where the capacitance increased from ~54 F·g-1 at 0.7 V to ~67 F·g-1 at 1.5 V at a specific current density of 200 mA·g-1 in a 1 M NaNO3 electrolyte. The specific capacitance of the E-RGO electrodes is 13.7% higher than that of chemically reduced graphene oxide (C-RGO), and these results demonstrate the effectiveness of electrochemically reduced graphene oxide, further demonstrating its potential applications in supercapacitors.
References
(1) S. Shivakumara, B. Kishore, T. Rao Penki, N. Munichandraiah. Symmetric Supercapacitor Based on Reduced Graphene Oxide in Non-Aqueous Electrolyte. ECS Electrochemistry Letters 4 (2015) A87-A90. Crossref
(2) E. Alqrafy, M.M. Ghobashy, M. Baqta, M.S. Almoiqi, A. Siddiq, et al. Two-dimensional material electrodes for next-generation energy storage synthesis, characterization, and applications. Journal of Alloys and Compounds 1072 (2026) 188840. Crossref
(3) A.Z. Abdullahi, A.A. Buba, M.A. Umar-Osuma, A. Ramalan. Chemical Passivation of Graphene: Emerging Trends and Applications in Supercapacitor Technologies. Bayero Journal of Pure and Applied Sciences 18 (2025) 1-11. Crossref
(4) S. Lin, J. Tang, K. Zhang, Y. Chen, R. Gao, et al. Tuning oxygen-containing functional groups of graphene for supercapacitors with high stability. Nanoscale Advances 5 (2023) 1163-1171. Crossref
(5) K. Rhili, S. Chergui, J.C. Abergo-Martinez, A.S. El Douhaibi, M. Siaj. Phosphorus and nitrogen co-doped reduced graphene oxide as superior electrode nanomaterials for supercapacitors. Materials Advances 4 (2023) 5263-5272. Crossref
(6) S. Mitra, C.K. Kamaja, M. Katiyar. Facile formation of porous, multilayer reduced graphene oxide electrodes using electrophoretic deposition and flash sintering. Carbon 203 (2023) 186-195. Crossref
(7) Q. Yu, L. Wei, X. Yang, C. Wang, J. Chen, et al. Electrochemical synthesis of graphene oxide from graphite flakes exfoliated at room temperature. Applied Surface Science 598 (2022) 153788. Crossref
(8) D.C. Marcano, D.V. Kosynkin, J.M. Berlin, A. Sinitskii, Z. Sun, et al. Improved synthesis of graphene oxide. ACS Nano 4 (2010) 4806-4814. Crossref
(9) L.G. Guex, B. Sacchi, K.F. Peuvot, R.L. Andersson, A.M. Pourrahimi, et al. Experimental review: Chemical reduction of graphene oxide (GO) to reduced graphene oxide (rGO) by aqueous chemistry. Nanoscale 9 (2017) 9562-9571. Crossref
(10) J.T. Robinson, F.K. Perkins, E.S. Snow, Z. Wei, P.E. Sheehan. Reduced graphene oxide molecular sensors. Nano Letters 8 (2008) 3137-3140. Crossref
(11) D.R. Dreyer, S. Park, C.W. Bielawski, R.S. Ruoff. The chemistry of graphene oxide. Chemical Society Reviews 39 (2010) 228-240. Crossref
(12) S.Y. Toh, K.S. Loh, S.K. Kamarudin, W.R.W. Daud. Graphene production via electrochemical reduction of graphene oxide: Synthesis and characterization. Chemical Engineering Journal 251 (2014) 422-434. Crossref
(13) R. Tarcan, O. Todor-Boer, I. Petrovai, C. Leordean, S. Astilean, et al. Reduced graphene oxide today. Journal of Materials Chemistry C 8 (2020) 1198-1224. Crossref
(14) X. Feng, W. Chen, L. Yan. Electrochemical reduction of bulk graphene oxide materials. RSC Advances 6 (2016) 80106-80113. Crossref
(15) J.A. Quezada-Renteria, C.O. Ania, L.F. Chazaro-Ruiz, J.R. Rangel-Mendez. Influence of protons on reduction degree and defect formation in electrochemically reduced graphene oxide. Carbon 149 (2019) 722-732. Crossref
(16) J.A. Quezada Renteria, C. Ruiz-Garcia, T. Sauvage, L.F. Chazaro-Ruiz, J.R. Rangel-Mendez, et al. Photochemical and electrochemical reduction of graphene oxide thin films: Tuning the nature of surface defects. Physical Chemistry Chemical Physics 22 (2020) 20732-20743. Crossref
(17) D. Karačić, S. Korać, A.S. Dobrota, I.A. Pašti, N.V. Skorodumova, et al. When supporting electrolyte matters – Tuning capacitive response of graphene oxide via electrochemical reduction in alkali and alkaline earth metal chlorides. Electrochimica Acta 297 (2019) 112-117. Crossref
(18) J. Yang, S. Gunasekaran. Electrochemically reduced graphene oxide sheets for use in high performance supercapacitors. Carbon 51 (2013) 36-44. Crossref
(19) S.K. Bikkarolla, P. Cumpson, P. Joseph, P. Papakonstantinou. Oxygen reduction reaction by electrochemically reduced graphene oxide. Faraday Discussions 173 (2014) 415-428. Crossref
(20) S. Choi, C. Kim, J.M. Suh, H.W. Jang. Reduced graphene oxide-based materials for electrochemical energy conversion reactions. Carbon Energy 1 (2019) 85-108. Crossref
(21) Y. Shao, J. Wang, M. Engelhard, C. Wang, Y. Lin. Facile and controllable electrochemical reduction of graphene oxide and its applications. Journal of Materials Chemistry 20 (2010) 743-748. Crossref
(22) C.K. Chua, M. Pumera. Chemical reduction of graphene oxide: A synthetic chemistry viewpoint. Chemical Society Reviews 43 (2014) 291-312. Crossref
(23) S. Zafar, S.K. Mani, M. Monisha, B. Lochab. Concentration-dependent kinetic study of graphene oxide (GO) reduction using biophenol and electrochemical analysis. RSC Sustainability 3 (2025) 365-375. Crossref
(24) M.K. Fathy, A.H. Zaki, H.A. Shawkey, H.R. Tantawy. Preparation and Qualification of Reduced Graphene Oxide by Different Reduction Methods. Transactions on Electrical and Electronic Materials 25 (2024) 732-744. Crossref
(25) T. Chudziak, V. Montes-García, W. Czepa, D. Pakulski, A. Musiat, et al. A comparative investigation of the chemical reduction of graphene oxide for electrical engineering applications. Nanoscale 15 (2023) 17765-17775. Crossref
(26) C. Valentini, V. Montes-García, P.A. Livio, T. Chudziak, J. Raya, et al. Tuning the electrical properties of graphene oxide through low-temperature thermal annealing. Nanoscale 15 (2023) 5743-5755. Crossref
(27) I. Imae. Reduction of Graphene Oxide Using an Environmentally Friendly Method and Its Application to Energy-Related Materials. Coatings 11 (2021) 297. Crossref
(28) L. Chen, Y. Tang, K. Wang, C. Liu, S. Luo. Direct electrodeposition of reduced graphene oxide on glassy carbon electrode and its electrochemical application. Electrochemistry Communications 13 (2011) 133-137. Crossref
(29) C. Liu, K. Wang, S. Luo, Y. Tang, L. Chen. Direct Electrodeposition of Graphene Enabling the One-Step Synthesis of Graphene-Metal Nanocomposite Films. Small 7 (2011) 1203-1206. Crossref
(30) H. Öztürk Doğan, D. Ekinci, Ü. Demir. Atomic scale imaging and spectroscopic characterization of electrochemically reduced graphene oxide. Surface Science 611 (2013) 54-59. Crossref
(31) H.L. Guo, X.F. Wang, Q.Y. Qian, F.B. Wang, X.H. Xia. A Green Approach to the Synthesis of Graphene Nanosheets. ACS Nano 3 (2009) 2653-2659. Crossref
(32) J. Yang, S. Deng, J. Lei, H. Ju, S. Gunasekaran. Electrochemical synthesis of reduced graphene sheet-AuPd alloy nanoparticle composites for enzymatic biosensing. Biosensors and Bioelectronics 29 (2011) 159-166. Crossref
(33) M. Handayani, E. Sulistiyono, F. Rokhmanto, N. Darsono, P.L. Fransisca. Fabrication of Graphene Oxide/Calcium Carbonate/Chitosan Nanocomposite Film with Enhanced Mechanical Properties. IOP Conference Series: Materials Science and Engineering 578 (2019) 012073. Crossref
(34) W. Gul, H. Alrobei. Effect of Graphene Oxide Nanoparticles on the Physical and Mechanical Properties of Medium Density Fiberboard. Polymers 13 (2021) 1818. Crossref
(35) S. Rao, J. Upadhyay, K. Polychronopoulou, R. Umer, R. Das. Reduced Graphene Oxide: Effect of Reduction on Electrical Conductivity. Journal of Composites Science 2 (2018) 25. Crossref
(36) S.B. Singh, S.A. Dastgheib. Physicochemical transformation of graphene oxide during heat treatment at 110-200 °C. Carbon Trends 10 (2023) 100251. Crossref
(37) L. Pustahija, W. Kern. Surface Functionalization of (Pyrolytic) Carbon-An Overview. C 9 (2023) 38. Crossref
(38) R. Al-Gaashani, A. Najjar, Y. Zakaria, S. Mansour, M.A. Atieh. XPS and structural studies of high quality graphene oxide and reduced graphene oxide prepared by different chemical oxidation methods. Ceramics International 45 (2019) 14439-14448. Crossref
(39) X. Zhang, D.C. Zhang, Y. Chen, X.Z. Sun, Y.W. Ma. Electrochemical reduction of graphene oxide films: Preparation, characterization and their electrochemical properties. Chinese Science Bulletin 57 (2012) 3045-3050. Crossref
(40) Z. Mansurov, Z. Supiyeva, Kh. Avchukir, A. Taurbekov, M. Yeleuov, et al. Investigation of Gold Electrosorption onto Gold and Carbon Electrodes using an Electrochemical Quartz Crystal Microbalance Institute of Combustion Problems. Eurasian Chemico-Technological Journal 21 (2019) 283-289. Crossref
(41) Z. Supiyeva, Z. Mansurov, S. Azat, Q. Abbas. A unique choline nitrate-based organo-aqueous electrolyte enables carbon/carbon supercapacitor operation in a wide temperature window (−40°C to 60°C). Frontiers in Chemistry 12 (2024) 1377144. Crossref
(42) K. Zhang, L. Mao, L.L. Zhang, H.S.O. Chan, X.S. Zhao, et al. Surfactant-intercalated, chemically reduced graphene oxide for high performance supercapacitor electrodes. Journal of Materials Chemistry 21 (2011) 7302-7307. Crossref
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Copyright (c) 2026 Ж.А. Супиева, Б.K. Балгабаева, Н. Мухаметгазы, Ф. Султанов, A.Б. Тугелбаева, X. Pan

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