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Author: Grafiati
Published: 6 September 2023

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1

Grushevski, E., D. Savelev, L. Mazaletski, N. Savinski, and D. Puhov. "The scalable production of high-quality nanographite by organic radical-assisted electrochemical exfoliation." Journal of Physics: Conference Series 2086, no. 1 (December 1, 2021): 012014. http://dx.doi.org/10.1088/1742-6596/2086/1/012014.

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Abstract One of the promising ways to produce graphene is the technology of graphite splitting or exfoliation, both by physical or mechanical and chemical, including electrochemical methods. The product of electro exfoliation is nanographite, which is transformed into multigraphene at the subsequent stage of liquid-phase mechanical and ultrasonic disintegration. This approach demonstrates a successful method of obtaining multigraphene from available graphite raw materials. Since, already at a potential of 1.23V, during the electrolysis of water on a graphite anode, the hydroxyl anion is discharged with the formation of a very active hydroxyl radical oxidizer, it is not surprising that when the graphite electro exfoliation process is overvolted at 10V, graphite oxidation products are formed. In order to control the defectiveness of the graphene lattice by oxidation products, we carried out processes of graphite exfoliation in the presence of both a number of reducing agents ascorbic acid, sodium borohydride, hydrazine hydrate, and in the presence of industrial antioxidants radical traps (2,2,6,6-tetramethylpiperidine-1-il)oxyl (TEMPO), (2,2,6,6-tetramethyl-4 oxo-piperidine-1-yl)oxyl (IPON), a mixture of 5,8,9-bis isomers[(2,2,6,6-tetramethyl - 4 oxo-piperidine-1-yl)]-{5,8,9-[1,1’- bi(cyclopentylidene)]-2,2’,4,4’- tetraene}(YARSIM-0215). It should be noted, that the best result of preventing the oxidation of nanographite in electro exfoliation technology in our studies is the ratio of carbon to oxygen (C/O) about 69.
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2

Shah, Syed Sajid Ali, and Habib Nasir. "Exfoliation of Graphene and its Application as Filler in Reinforced Polymer Nanocomposites." Nano Hybrids and Composites 11 (October 2016): 7–21. http://dx.doi.org/10.4028/www.scientific.net/nhc.11.7.

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Recently, graphene has played a promising role due to its exceptional mechanical and thermal properties and the broad range of applications. This paper reviews the synthesis of graphene and its use as fillers in polymer nanocomposites. The nanocomposites prepared by different methods have the wide range of applications, such as in energy storage devices, biosensor applications, automotive industries and electronic industries. Graphene can be prepared by different methods, for example, mechanical exfoliation, chemical exfoliation, electrochemical exfoliation and Intercalation compound exfoliation. The electrochemical method is environmentally friendly, however, the chemical exfoliation method is cost effective and suitable for commercial production of graphene. In oxidation-reduction method, the oxidation of graphite starts at point’s defects and the temperature has great effects on oxidation of graphite, at low-temperature oxidation is sensitive to impurities and at high-temperature oxidation increases with increasing temperature. Graphene can be incorporated into the polymer matrix by different approaches, such as in situ polymerization, solution, costing method, electrodeposition, and click chemistry method.
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3

Hashimoto, Hideki, Yusuke Muramatsu, Yuta Nishina, and Hidetaka Asoh. "Bipolar anodic electrochemical exfoliation of graphite powders." Electrochemistry Communications 104 (July 2019): 106475. http://dx.doi.org/10.1016/j.elecom.2019.06.001.

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4

Bourelle, E., J. Dougiade, and A. Metrot. "Electrochemical Exfoliation of Graphite in Trifluoroacetic Media." Molecular Crystals and Liquid Crystals Science and Technology. Section A. Molecular Crystals and Liquid Crystals 244, no. 1 (April 1994): 227–32. http://dx.doi.org/10.1080/10587259408050109.

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5

Nikiforov, A. A., M. S. Kondratenko, O. O. Kapitanova, and M. O. Gallyamov. "Electrochemical Exfoliation of Graphite in Supercritical Media." Doklady Physical Chemistry 492, no. 2 (June 2020): 69–73. http://dx.doi.org/10.1134/s0012501620060020.

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6

Destiarti, Lia, Riyanto Riyanto, Roto Roto, and Mudasir Mudasir. "Electrolyte effect in electrochemical exfoliation of graphite." Materials Chemistry and Physics 302 (July 2023): 127713. http://dx.doi.org/10.1016/j.matchemphys.2023.127713.

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7

Salverda, Michael, Antony Raj Thiruppathi, Farnood Pakravan, Peter C. Wood, and Aicheng Chen. "Electrochemical Exfoliation of Graphite to Graphene-Based Nanomaterials." Molecules 27, no. 24 (December 7, 2022): 8643. http://dx.doi.org/10.3390/molecules27248643.

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Here, we report on a new automated electrochemical process for the production of graphene oxide (GO) from graphite though electrochemical exfoliation. The effects of the electrolyte and applied voltage were investigated and optimized. The morphology, structure and composition of the electrochemically exfoliated GO (EGO) were probed by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), energy dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS), FTIR spectroscopy and Raman spectroscopy. Important metrics such as the oxygen content (25.3 at.%), defect density (ID/IG = 0.85) and number of layers of the formed EGO were determined. The EGO was also compared with the GO prepared using the traditional chemical method, demonstrating the effectiveness of the automated electrochemical process. The electrochemical properties of the EGO, CGO and other carbon-based materials were further investigated and compared. The automated electrochemical exfoliation of natural graphite powder demonstrated in the present study does not require any binders; it is facile, cost-effective and easy to scale up for a large-scale production of graphene-based nanomaterials for various applications.
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8

Coroş, Maria, Florina Pogăcean, Marcela-Corina Roşu, Crina Socaci, Gheorghe Borodi, Lidia Mageruşan, Alexandru R. Biriş, and Stela Pruneanu. "Simple and cost-effective synthesis of graphene by electrochemical exfoliation of graphite rods." RSC Advances 6, no. 4 (2016): 2651–61. http://dx.doi.org/10.1039/c5ra19277c.

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9

Lou, Fengliu, Marthe Emelie Melandsø Buan, Navaneethan Muthuswamy, John Charles Walmsley, Magnus Rønning, and De Chen. "One-step electrochemical synthesis of tunable nitrogen-doped graphene." Journal of Materials Chemistry A 4, no. 4 (2016): 1233–43. http://dx.doi.org/10.1039/c5ta08038j.

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10

Kurys, Ya I., O. O. Ustavytska, V. G. Koshechko, and V. D. Pokhodenko. "Structure and electrochemical properties of multilayer graphene prepared by electrochemical exfoliation of graphite in the presence of benzoate ions." RSC Advances 6, no. 42 (2016): 36050–57. http://dx.doi.org/10.1039/c6ra02619b.

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11

Ilnicka, Anna, Malgorzata Skorupska, Piotr Kamedulski, and Jerzy P. Lukaszewicz. "Electro-Exfoliation of Graphite to Graphene in an Aqueous Solution of Inorganic Salt and the Stabilization of Its Sponge Structure with Poly(Furfuryl Alcohol)." Nanomaterials 9, no. 7 (July 3, 2019): 971. http://dx.doi.org/10.3390/nano9070971.

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We demonstrate an accessible and effective technique for exfoliating graphite foil and graphite powder into graphene in a water solution of inorganic salt. In our research, we report an electrochemical cathodic exfoliation in an aqueous solution of Na2SO4. After electro-exfoliation, the resulting graphene was premixed with furfuryl alcohol (FA) and an inorganic template (CaCO3 and Na2CO3). Once FA was polymerized to poly(furfuryl alcohol) (PFA), the mixture was carbonized. Carbon bridges originating in thermally-decomposed PFA joined exfoliated graphene flakes and stabilized the whole sponge-type structure after the nano-template was removed. Gases evolved at the graphite electrode (cathode) played an important role in the process of graphene-flake splitting and accelerated the change of graphite into graphene flakes. Starting graphite materials and graphene sponges were characterized using Raman spectroscopy, SEM, high-resolution transmission electron microscopy (HRTEM), elemental analysis, and low-temperature adsorption of nitrogen to determine their structure, morphology, and chemical composition. The discovered manufacturing protocol had a positive influence on the specific surface area and porosity of the sponges. The SEM and HRTEM studies confirmed a high separation degree of graphite and different agglomeration pathways. Raman spectra were analyzed with particular focus on the intensities of ID and IG peaks; the graphene-type nature of the sponges was confirmed.
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12

Atrey, Isha, and Anupam Shukla. "Graphene Suspension from Modified Electrochemical Exfoliation of Graphite." ECS Meeting Abstracts MA2021-02, no. 7 (October 19, 2021): 1888. http://dx.doi.org/10.1149/ma2021-0271888mtgabs.

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13

Kochergin, V. K., R. A. Manzhos, N. S. Komarova, A. S. Kotkin, A. G. Krivenko, I. N. Krushinskaya, and A. A. Pelmenev. "Plasma-Electrochemical Exfoliation of Graphite in Pulsed Mode." High Energy Chemistry 56, no. 6 (December 2022): 487–92. http://dx.doi.org/10.1134/s0018143922060091.

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14

Shinde, Dhanraj B., Jason Brenker, Christopher D. Easton, Rico F. Tabor, Adrian Neild, and Mainak Majumder. "Shear Assisted Electrochemical Exfoliation of Graphite to Graphene." Langmuir 32, no. 14 (April 4, 2016): 3552–59. http://dx.doi.org/10.1021/acs.langmuir.5b04209.

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15

Jeon, Intak, Bora Yoon, Maggie He, and Timothy M. Swager. "Hyperstage Graphite: Electrochemical Synthesis and Spontaneous Reactive Exfoliation." Advanced Materials 30, no. 3 (December 2017): 1704538. http://dx.doi.org/10.1002/adma.201704538.

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16

Chen, Duhong, Fei Wang, Yijuan Li, Wei-Wei Wang, Teng-Xiang Huang, Jian-Feng Li, Kostya S. Novoselov, Zhong-Qun Tian, and Dongping Zhan. "Programmed electrochemical exfoliation of graphite to high quality graphene." Chemical Communications 55, no. 23 (2019): 3379–82. http://dx.doi.org/10.1039/c9cc00393b.

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We propose programed potential modulation strategies to balance the ion intercalation/deintercalation, surface tailoring and bubbling dispersion processes in the electrochemical exfoliation of graphite, resulting in high-quality graphene with high crystallinity, low oxidation degree, uniform size distribution and few layers.
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17

Li, Yueh-Feng, Shih-Ming Chen, Wei-Hao Lai, Yu-Jane Sheng, and Heng-Kwong Tsao. "Superhydrophilic graphite surfaces and water-dispersible graphite colloids by electrochemical exfoliation." Journal of Chemical Physics 139, no. 6 (August 14, 2013): 064703. http://dx.doi.org/10.1063/1.4817680.

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18

Dong, Yongqiang, Juanxia Su, Shuqing Zhou, Min Wang, Shuping Huang, Chun-Hua Lu, Hongbin Yang, and Fengfu Fu. "Carbon-based dots for the electrochemical production of hydrogen peroxide." Chemical Communications 56, no. 55 (2020): 7609–12. http://dx.doi.org/10.1039/c9cc09987e.

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Graphene/carbon-based dot nanohybrids were prepared by the ultrasonic exfoliation of natural graphite in the presence of single-layer carbon based dots, and used for the electrochemical production of hydrogen peroxide.
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19

Rodrigues, F. C., G. A. Nobre, E. E. da Silva, Mauro Cesar Terence, and Juan Alfredo Guevara Carrió. "Graphite/Metal Electrodes for Electrochemical Exfoliation: Few Layers Graphene with Low Defects." Defect and Diffusion Forum 371 (February 2017): 131–34. http://dx.doi.org/10.4028/www.scientific.net/ddf.371.131.

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Graphene was obtained by electrochemical exfoliation of graphite and metal/graphite electrodes of different compositions and electrical conductivities. Metal/graphite electrodes were prepared using high purity copper and nickel precursor and commercial graphite. Processes of rapid expansion and direct exfoliation of graphite in a H2SO4 solution were observed using voltages from 2V to 15V and currents of 0.03 mA to 0.08 mA. The total time for each process was one hour and the maximal concentration of few layers graphene flakes was 0.002 mg/mL. X rays powder diffraction of the expanded electrodes showed the effect of the electrochemical process in the crystallinity and the increasing of interlayer distance. A characterization of a large amount of graphene flakes was performed by Raman spectroscopy and optical microscopy. Typical size of the flakes are between 1 μm and 10 μm and the Raman spectra indicate number of layers from single or bilayers to approximately ten layers. The greatest variations in thickness of flakes are observed when the intercalation process concludes before the expansion of the layers. A low degree of oxidation and of structural defects was characteristic of the experiments with lower acid concentration.
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20

Fu, Yang, Guanyue Gao, and Jinfang Zhi. "Electrochemical synthesis of multicolor fluorescent N-doped graphene quantum dots as a ferric ion sensor and their application in bioimaging." Journal of Materials Chemistry B 7, no. 9 (2019): 1494–502. http://dx.doi.org/10.1039/c8tb03103g.

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A novel electrochemical strategy for simple and facile synthesis of semicarbazide functionalized nitrogen-doped graphene quantum dots (N-GQDs) was reported, based on direct exfoliation and oxidation from graphite rods.
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21

Punith Kumar, M. K., Monika Nidhi, and Chandan Srivastava. "Electrochemical exfoliation of graphite to produce graphene using tetrasodium pyrophosphate." RSC Advances 5, no. 32 (2015): 24846–52. http://dx.doi.org/10.1039/c5ra01304f.

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22

Parveen, Nazish, Mohd Omaish Ansari, Sajid Ali Ansari, and Moo Hwan Cho. "Correction: Simultaneous sulfur doping and exfoliation of graphene from graphite using an electrochemical method for supercapacitor electrode materials." Journal of Materials Chemistry A 4, no. 32 (2016): 12668–69. http://dx.doi.org/10.1039/c6ta90155g.

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Correction for ‘Simultaneous sulfur doping and exfoliation of graphene from graphite using an electrochemical method for supercapacitor electrode materials’ by Nazish Parveen et al., J. Mater. Chem. A, 2016, 4, 233–240.
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23

Hsieh, Chien-Te, and Jen-Hao Hsueh. "Correction: Electrochemical exfoliation of graphene sheets from a natural graphite flask in the presence of sulfate ions at different temperatures." RSC Advances 6, no. 98 (2016): 96015. http://dx.doi.org/10.1039/c6ra90090a.

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Correction for ‘Electrochemical exfoliation of graphene sheets from a natural graphite flask in the presence of sulfate ions at different temperatures’ by Chien-Te Hsieh et al., RSC Adv., 2016, 6, 64826–64831.
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24

AbdelHamid, Ayman A., Abdelaziz Elgamouz, and Abdel-Nasser Kawde. "Controlled electrochemical surface exfoliation of graphite pencil electrodes for high-performance supercapacitors." RSC Advances 13, no. 31 (2023): 21300–21312. http://dx.doi.org/10.1039/d3ra03952h.

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A controlled surface exfoliation for graphite electrodes was developed, achieving >300× increase in the electrochemical surface area, >50× decrease in total electrode resistance, and >2 orders of magnitude enhancement in energy storage capacity.
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25

Walkowiak, Mariusz, Daniel Waszak, Błażej Gierczyk, and Grzegorz Schroeder. "Impact of selected supramolecular additives on the initial electrochemical lithium intercalation into graphite in propylene carbonate." Open Chemistry 6, no. 4 (December 1, 2008): 600–606. http://dx.doi.org/10.2478/s11532-008-0058-8.

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AbstractImpact of silicon tripodand-type electrolyte additives and graphite pre-treatment agents on the electrochemical intercalation of lithium cations into graphite was investigated. Addition of Si-tripodand-type silanes to propylene carbonate-based electrolytes was found to suppress detrimental solvent co-intercalation and graphite exfoliation. Similar effects were observed for graphite pre-treated with the reported silane agents. It was observed that the presented supramolecular additives allow for the formation of effective passive layers on graphite during first charging, and thus can be considered as novel low-cost film-forming components for rechargeable lithium batteries.
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26

Lee, Hoyoung, Seung Woo Lee, and Kyungbin Lee. "High-Quality Electrochemically Exfoliated Graphene Protective Layer for Metal Batteries." ECS Meeting Abstracts MA2022-02, no. 8 (October 9, 2022): 663. http://dx.doi.org/10.1149/ma2022-028663mtgabs.

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Graphene has attracted substantial attention due to its exceptional mechanical, thermal, electrical, and chemical properties. There has been active research for the scalable production of high-quality graphene. Among various techniques, electrochemical exfoliation is facile, fast, and cost-effective for graphene production. Our previous finding on anodic exfoliation suggested that the binding energy between the intercalator and graphene sheet plays an important role in exfoliation efficiency.1 We further extended the hypothesis to the cathodic exfoliation process to produce high-quality graphene. The characteristics and morphologies of electrochemically exfoliated graphene using alkali metals (e.g. Na, K, and Cs) are compared. Then, we will employ the exfoliated graphene on lithium metal anodes as carbon support for efficient lithium deposition in lithium metal batteries. References Lee, H.; Choi, J. I.; Park, J.; Jang, S. S.; Lee, S. W. Role of anions on electrochemical exfoliation of graphite into graphene in aqueous acids. Carbon 2020, 167, 816-825.
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27

Roscher, Sarah, René Hoffmann, Mario Prescher, Peter Knittel, and Oliver Ambacher. "High voltage electrochemical exfoliation of graphite for high-yield graphene production." RSC Advances 9, no. 50 (2019): 29305–11. http://dx.doi.org/10.1039/c9ra04795f.

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28

Kim, Min Ji, Chang Hee Lee, Mun Hui Jo, and Soon Ki Jeong. "Electrochemical Decomposition of Poly(Vinylidene Fluoride) Binder for a Graphite Negative Electrode in Lithium-Ion Batteries." Materials Science Forum 893 (March 2017): 127–31. http://dx.doi.org/10.4028/www.scientific.net/msf.893.127.

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To clarify the electrochemical decomposition of poly (vinylidene fluoride) (PVdF) used as a binder for lithium-ion batteries while simultaneously verifying the correlation between electrode resistance and the PVdF content in graphite negative electrodes, in this study, we applied lithium bis (trifluoromethanesulfonyl) imide, which suppresses graphite exfoliation, as a salt. As a result, the electrochemical decomposition of PVdF was observed at a higher potential than that at which the electrolyte was decomposed during the reduction process. Additionally, this study demonstrated (through electrochemical impedance spectroscopy analysis) that electrode resistances such as solid electrolyte interface and charge transfer resistance proportionally increased with the PVdF content.
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29

Mir, Afkham, and Anupam Shukla. "Bilayer-rich graphene suspension from electrochemical exfoliation of graphite." Materials & Design 156 (October 2018): 62–70. http://dx.doi.org/10.1016/j.matdes.2018.06.035.

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30

Anwar, M. A., A. K. Zainal, T. Kurniawan, Y. P. Asmara, W. S. W. Harun, G. Priyadonko, and K. Saptaji. "Electrochemical Exfoliation of Pencil Graphite Core by Salt Electrolyte." IOP Conference Series: Materials Science and Engineering 469 (January 16, 2019): 012105. http://dx.doi.org/10.1088/1757-899x/469/1/012105.

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31

M. K., Punith Kumar, S. Shanthini, and Chandan Srivastava. "Electrochemical exfoliation of graphite for producing graphene using saccharin." RSC Advances 5, no. 66 (2015): 53865–69. http://dx.doi.org/10.1039/c5ra07846f.

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32

Yu, Pei, Sean E. Lowe, George P. Simon, and Yu Lin Zhong. "Electrochemical exfoliation of graphite and production of functional graphene." Current Opinion in Colloid & Interface Science 20, no. 5-6 (October 2015): 329–38. http://dx.doi.org/10.1016/j.cocis.2015.10.007.

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33

Chen, Chia-Hsuan, Shiou-Wen Yang, Min-Chiang Chuang, Wei-Yen Woon, and Ching-Yuan Su. "Towards the continuous production of high crystallinity graphene via electrochemical exfoliation with molecular in situ encapsulation." Nanoscale 7, no. 37 (2015): 15362–73. http://dx.doi.org/10.1039/c5nr03669k.

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A fast and continuous electrochemical method with melamine additives is able to efficiently exfoliate graphite into high-quality graphene sheets. The hydrophilic force facilitated exfoliation and protection, leading to high yield production of larger size crystallinity of graphene sheets.
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34

Gondosiswanto, Richard, Xunyu Lu, and Chuan Zhao. "Preparation of Metal-Free Nitrogen-Doped Graphene Via Direct Electrochemical Exfoliation of Graphite in Ammonium Nitrate." Australian Journal of Chemistry 68, no. 5 (2015): 830. http://dx.doi.org/10.1071/ch14447.

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Nitrogen-doped graphene (N-graphene) nanosheets have been synthesized via electrochemical intercalation and exfoliation of graphite rods in ammonium nitrate aqueous solutions. This method produces N-graphene free from possible metal contaminations that can be utilized as efficient electrocatalysts towards oxygen reduction reactions.
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35

Lei, Yuting, Benjamin D. Ossonon, Jiyun Chen, Jonathan Perreault, and Ana C. Tavares. "Electrochemical characterization of graphene-type materials obtained by electrochemical exfoliation of graphite." Journal of Electroanalytical Chemistry 887 (April 2021): 115084. http://dx.doi.org/10.1016/j.jelechem.2021.115084.

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36

LEI, Yuting, Benjamin Ossonon, Jonathan Perreault, and Ana C. Tavares. "Electrochemical Characterization of Graphene-like Materials Obtained By Electrochemical Exfoliation of Graphite." ECS Meeting Abstracts MA2020-01, no. 10 (May 1, 2020): 813. http://dx.doi.org/10.1149/ma2020-0110813mtgabs.

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37

Yang, Zilan, Jiaxiang Zhao, Graf Sullivan, and Shiqiang Zou. "Comprehensive Evaluation of Affordable Cathode Materials in Direct Electrochemical Selenite Reduction." ECS Meeting Abstracts MA2022-02, no. 27 (October 9, 2022): 1044. http://dx.doi.org/10.1149/ma2022-02271044mtgabs.

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Selenium (Se) is a naturally occurring metalloid that has been widely sourced for health care, clean energy technology development, and agricultural activities. These activities have accelerated Se release into the aquatic environment, urging engineered solutions to mitigate aquatic Se pollution and their ecological impact. Our lab previously demonstrated a direct electrochemical reduction approach to convert 97% of soluble selenite into elemental Se(0) on a gold cathode. This study builds upon our prior success in selenite separation to further explore alternative cathode materials to gold. Six economically competitive materials (Ni, graphite, Cu, Fe, stainless steel, and Ti) were evaluated for key performance parameters, including Se removal efficiency, Faradaic efficiency, energy consumption, and electrode durability. Preliminary cyclic voltammetry scans revealed that Ni and graphite could sustain Se(IV)/Se(0) reduction in diluted water matrices within their electrochemical window. The subsequent 24-h chronoamperometry (CA) test demonstrated 67% selenite removal using a Ni cathode, while graphite offered a better removal efficiency (92%). Separated selenite ions were primarily plated as elemental Se(0) on the cathode surface (Ni & graphite) or within the electrode structure (graphite). While graphite has better selenite removal than Ni, it demands more energy input and has lower Faradaic efficiency (C-3.7% vs. Ni-12.7%). Switching from a CA mode to a chronopotentiometry (CP) mode did not significantly impact selenite removal performance, and the energy consumption was increased by 15%. Continued exfoliation is observed on the graphite electrode surface, potentially due to the expansion of inner gas bubbles and the lattice destruction caused by Se(0) insertion. Our results suggest graphite offers comparable selenite separation performance to a gold cathode. Still, electrode exfoliation and higher energy input due to parasitic reactions must be appropriately addressed in future research efforts.
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38

Tan, Xiaoyun, Yunchao Li, Xiaohong Li, Shixin Zhou, Louzhen Fan, and Shihe Yang. "Electrochemical synthesis of small-sized red fluorescent graphene quantum dots as a bioimaging platform." Chemical Communications 51, no. 13 (2015): 2544–46. http://dx.doi.org/10.1039/c4cc09332a.

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We report water-soluble, 3 nm uniform-sized graphene quantum dots (GQDs) with red emission prepared by electrochemical exfoliation of graphite in K2S2O8 solution. Such GQDs show a great potential as biological labels for cellular imaging.
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39

Karbak, Mehdi, Ouassim Boujibar, Sanaa Lahmar, Cecile Autret-Lambert, Tarik Chafik, and Fouad Ghamouss. "Chemical Production of Graphene Oxide with High Surface Energy for Supercapacitor Applications." C 8, no. 2 (May 7, 2022): 27. http://dx.doi.org/10.3390/c8020027.

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The chemical exfoliation of graphite to produce graphene and its oxide is undoubtedly an economical method for scalable production. Carbon researchers have dedicated significant resources to developing new exfoliation methods leads to graphene oxides with high quality. However, only a few studies have been dedicated to the effect of the starting graphite material on the resulting GO. Herein, we have prepared two different GOs through chemical exfoliation of graphite materials having different textural and structural characteristics. All samples have been subjected to structural investigations and comprehensive characterizations using Raman, X-ray diffraction, scanning electron microscopy, TGA, N2 physisorption, and FTIR spectroscopy. Our results provide direct evidence of how the crystallite size of the raw graphite affects the oxidation degree, surface functionality, and sheet size of the resulting GO. Building on these significant understandings, the optimized GO achieves a highly specific capacitance of 191 F·g−1 at the specific current of 0.25 A·g−1 in an aqueous electrolyte. This superior electrochemical performance was attributed to several factors, among which the specific surface area was accessible to the electrolyte ions and oxygenated functional groups on the surface, which can significantly modify the electronic structure of graphene and further enhance the surface energy.
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40

Perumal, Suguna, Raji Atchudan, Thomas Nesakumar Jebakumar Immanuel Edison, Jae-Jin Shim, and Yong Rok Lee. "Exfoliation and Noncovalent Functionalization of Graphene Surface with Poly-N-Vinyl-2-Pyrrolidone by In Situ Polymerization." Molecules 26, no. 6 (March 11, 2021): 1534. http://dx.doi.org/10.3390/molecules26061534.

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Heteroatom functionalization on a graphene surface can endow the physical and structural properties of graphene. Here, a one-step in situ polymerization method was used for the noncovalent functionalization of a graphene surface with poly-N-vinyl-2-pyrrolidone (PNVP) and the exfoliation of graphite into graphene sheets. The obtained graphene/poly-N-vinyl pyrrolidone (GPNVP) composite was thoroughly characterized. The surface morphology of GPNVP was observed using field emission scanning electron microscopy and high-resolution transmission electron microscopy. Raman spectroscopy and X-ray diffraction studies were carried out to check for the exfoliation of graphite into graphene sheets. Thermogravimetric analysis was performed to calculate the amount of PNVP on the graphene surface in the GPNVP composite. The successful formation of the GPNVP composite and functionalization of the graphene surface was confirmed by various studies. The cyclic voltammetry measurement at different scan rates (5–500 mV/s) and electrochemical impedance spectroscopy study of the GPNVP composite were performed in the typical three-electrode system. The GPNVP composite has excellent rate capability with the capacitive property. This study demonstrates the one-pot preparation of exfoliation and functionalization of a graphene surface with the heterocyclic polymer PNVP; the resulting GPNVP composite will be an ideal candidate for various electrochemical applications.
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41

Krivenko, A. G., R. A. Manzhos, and A. S. Kotkin. "Plasma-Assisted Electrochemical Exfoliation of Graphite in the Pulsed Mode." High Energy Chemistry 52, no. 3 (May 2018): 272–73. http://dx.doi.org/10.1134/s0018143918030074.

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42

Singh, Randhir, and Chandra Charu Tripathi. "Electrochemical Exfoliation of Graphite into Graphene for Flexible Supercapacitor Application." Materials Today: Proceedings 5, no. 1 (2018): 1125–30. http://dx.doi.org/10.1016/j.matpr.2017.11.192.

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43

Zhou, Ming, Jie Tang, Qian Cheng, Gaojie Xu, Ping Cui, and Lu-Chang Qin. "Few-layer graphene obtained by electrochemical exfoliation of graphite cathode." Chemical Physics Letters 572 (May 2013): 61–65. http://dx.doi.org/10.1016/j.cplett.2013.04.013.

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44

P, Kavya, Soorya V. S, and Binitha N. Narayanan. "Ball-Mill Assisted Green One-Pot Synthesis of ZnO/Graphene Nanocomposite for Selective Electrochemical Sensing of aquatic pollutant 4-nitrophenol." Teknomekanik 4, no. 2 (October 20, 2021): 64–71. http://dx.doi.org/10.24036/teknomekanik.v4i2.10872.

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ZnO, having good transparency, high electron mobility and lower electrical noise, is an excellent material for electrochemical studies. Due to its high surface area and electrical conductivity, graphene is well suitable for the good dispersion of metal oxides for electronic/electrochemical applications. Graphene prevents particle agglomeration, whereas the addition of metal oxide prevents layer restacking in graphene. The bulk preparation of graphene via cost-effective and green methods are preferred. The aromatic conjugated π-network along the whole surface is not attained in large scale graphite oxide assisted production due to the defects and functional groups introduced during the hazardous synthetic procedure. Here, less defective graphene is synthesised via ball milling of graphite using metal oxalate as an exfoliating agent for the first time. Calcination of metal oxalate inserted graphite leads to the enormous evolution of gases thereby sliding the graphitic layers, leading to the formation of graphene sheets decorated with ZnO spherical nanoparticles’ bunches. The layer exfoliation and metal oxide incorporation are achieved here via a one-pot synthesis strategy. The use of ZnO/graphene in the selective sensing of 4-nitrophenol is investigated using cyclic voltammetric measurements in the presence of interfering compounds such as glucose, uric acid, ascorbic acid and H2O2.
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45

Khan, Yulian A., Tatyana P. Dyachkova, Evgeny S. Bakunin, Elena Yu Obraztsova, Artyom V. Rukhov, and Simone Morais. "A study of the structure and morphology of the graphite electrochemical exfoliation products." Image Journal of Advanced Materials and Technologies 6, no. 4 (2021): 267–78. http://dx.doi.org/10.17277/jamt.2021.04.pp.267-278.

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The paper presents a generalized analysis of the results of scanning electron microscopy, energy dispersive spectroscopy, and TG/DSC analysis of electrochemical exfoliation products from two types of initial graphite raw materials at different process temperatures in solutions of potassium hydroxide (KOH) and sulfuric acid (H2SO4). It is shown that an increase in the concentration of an alkaline electrolyte in the range from 0.1 to 1.0 molL–1 promotes the intensification of the process of separation and splitting of graphite into fragments. In the case of the formation of large fragments, the product contains a significant amount of intercalated potassium ions, which are not removed when the material is washed off. The products of electrochemical exfoliation of the spent electrocontact graphite material demonstrate structural heterogeneity, contain a significant amount of functional groups and impurities of the amorphous phase. Thermogravimetric curves have several sections of sample weight reduction. After heating these materials in an inert atmosphere to 900 °C, the total weight loss reaches 66 %. From a thermally expanded graphite foil, samples of nanographites, extremely homogeneous in chemical composition, with increased thermal stability and a minimum number of surface defects were obtained. The total weight loss of the samples when heated in an inert atmosphere to 900 °C does not exceed 17 %. It was shown that the replacement of an alkaline electrolyte with a sulfuric acid solution leads to an increase in the number of defects in the product.
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46

Aksoy, Canser, and Duygu Anakli. "Synthesis of Graphene Oxide Through Ultrasonic Assisted Electrochemical Exfoliation." Open Chemistry 17, no. 1 (August 27, 2019): 581–86. http://dx.doi.org/10.1515/chem-2019-0062.

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AbstractWe report a ‘green’, simple and efficient approach for the production of graphene oxide (GO) by ultrasonic assisted electrochemical exfoliation of graphite rods, and by using Improved Hummers’ graphene oxide (IGO) as an electrolyte. The effects of applied bias, electrolyte concentration and the duration of the electrochemical exfoliation on the quality of the GO nanosheets were investigated. The produced graphene oxide with a high yield (> 48%), and the lowest defect was obtained in the ultrasonic assisted electrochemical exfoliation performed at 0.05% IGO mass percent in DI water and 50 V applied bias for 1 hour at room temperature. The structural, morphological and physical properties of the obtained nanostructures were analyzed by XRD, Raman, FESEM, STEM techniques and thermal conductivity analysis, respectively. The characteristic Raman bands were observed at 1354 cm-1 and 1590 cm-1 for the prepared GO nanosheets. The produced graphene oxides exhibited a lateral dimension of 3-7 μm revealed by field emission scanning electron microscopy (FESEM). It was observed that the thermal conductivity enhancement of 14.95% was obtained for GO, which was higher than the other IGO nanofluid (7.64%) with respect to DI water at 20oC.
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47

Rico, J., M. Castaño-Soto, N. Lopez-Arango, and Y. Hernandez. "Influence of C=O groups on the optical extinction coefficient of graphene exfoliated in liquid phase." Journal of Physics: Condensed Matter 34, no. 10 (December 23, 2021): 105701. http://dx.doi.org/10.1088/1361-648x/ac3fd6.

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Abstract Liquid phase exfoliation of graphite is currently one of the most promising graphene production methods at large scale. For this reason, an accurate calculation of the concentration in graphene dispersions is important for standardization and commercialization. Here, graphene dispersions, at high concentrations, were produced by electrochemical exfoliation. Furthermore, a cleaner methodology to obtain graphene oxide by electrochemical exfoliation at high acid concentrations was implemented. The absorption coefficient for graphene and graphene oxide was determined in the optical range (α 660 nm = 1414 (±3%) ml mg−1 m−1 and α 660 nm = 648 (±7%) ml mg−1 m−1, respectively) with an exponential dependence with the wavelength. The difference in α for both materials is attributed to an increased presence of C=O groups as evidenced by Fourier transform infrared spectroscopy (FTIR), UV–vis and Raman spectroscopy, as well as, in the calculation of the optical extinction coefficient and optical band-gap via Tauc-plots.
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48

Lee, Wonk Yun, Shinya Suzuki, and Masaru Miyayama. "Electrode Properties of Defect-Introduced Graphenes for Lithium-Ion Batteries." Key Engineering Materials 582 (September 2013): 103–6. http://dx.doi.org/10.4028/www.scientific.net/kem.582.103.

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Electrochemical properties of defect-introduces graphenes for lithium ion batteries were investigated. Graphene sheets (GSs) were prepared from graphite through treating with oxidizing agent followed by rapid thermal exfoliation. Defect concentration was controlled by selecting the number of times of oxidation of graphite. GSs electrodes derived from 1, 2 and 3 times-oxidized graphite oxides exhibited a high charge capacity of 1250, 1790 and 2310 mAh g1, respectively, at the 20th cycle at a current density of 100 mA g1. The enhanced capacity is assumed to be due to additional lithium storage sites such as defects and edges.
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49

LEI, Yuting, Benjamin Ossonon, Jonathan Perreault, and Ana Tavares. "Electrochemical Characterization and Application of Graphene Oxide Materials Obtained By Electrochemical Exfoliation of Graphite." ECS Meeting Abstracts MA2022-01, no. 12 (July 7, 2022): 842. http://dx.doi.org/10.1149/ma2022-0112842mtgabs.

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Graphene oxide (GO) materials possess oxygen functional groups located at the edges and at the surface of the graphitic layers, confering them dispersibility in water, biocompatibility, and high affinity for specific molecules. These properties are highly appealing for their use in electrochemical sensors. However, the density and type of functional groups and defects in these materials also influence the heterogeneous electron transfer rate of redox processes occurring at the GO-based electrodes 1,2. In this respect, it is necessary to investigate the physicochemical and electrochemical properties of GO materials to choose the most suitable one for a target application. Here, we report a simple and facile platform for the electrochemical characterization of GO materials 3. The GO sheets are self-assembled on a glassy carbon electrode (GCE) through an aminophenyl-film linker (AP) through electrostatic interaction and pi-pi stacking, Figure 1a. Then, the modified electrodes are characterized by cyclic voltammetry with 1 mM [Fe(CN)6]3-/4- redox couple to determine the electrochemical surface area (ESA) through the Randles-Sevcik equation and to calculate the standard rate constant of electron transfer (k0) by the Nicolson method. In this work, series of GO materials were obtained by electrochemical exfoliation of graphite in 0.1 M H2SO4. The electrochemical exfoliation of graphite in aqueous solution is an easy and “green” method that allows the synthesis of large amounts (in the order of grams) of materials (EGO: electrochemically exfoliated graphene oxide) with tunable composition in a short time (few hours). The applied voltage and the distance between the graphite and the counter electrodes were varied, Figure 1b, to obtain EGOs with different physicochemical properties such as the number of layers, structural defects, type and content of oxygenated groups. Transmission electron microscopy, Raman spectroscopy and X-ray photoelectron spectroscopy analysis were used to investigate the physicochemical properties of the EGOs. As shown in Figure 1c, the measured ESA and k0 scale with each other and are sensitive to the physicochemical properties of EGOs. This confirms the suitability of the proposed platform to characterize the EGO materials 3. Finally, selected EGO materials were used to fabricate electrochemical aptasensors for the detection of cocaine. The influence of the EGO physicochemical properties on the performance of the aptasensors will be presented and discussed. References (1) Kampouris, D. K.; Banks, C. E. Chemical Communications 2010, 46, 8986-8988. (2) Ambrosi, A.; Bonanni, A.; Sofer, Z.; Cross, J. S.; Pumera, M. Chemistry – A European Journal 2011, 17, 10763-10770. (3) Lei, Y.; Ossonon, B. D.; Chen, J.; Perreault, J.; Tavares, A. C. Journal of Electroanalytical Chemistry 2021, 887, 115084. Figure 1
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50

Pogacean, Florina, Codruta Varodi, Maria Coros, Irina Kacso, Teodora Radu, Bogdan Ionut Cozar, Valentin Mirel, and Stela Pruneanu. "Investigation of L-Tryptophan Electrochemical Oxidation with a Graphene-Modified Electrode." Biosensors 11, no. 2 (January 28, 2021): 36. http://dx.doi.org/10.3390/bios11020036.

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A graphene sample (EGr) was prepared by electrochemical exfoliation of graphite rods in solution containing 0.05 M (NH4)2SO4 + 0.1 M H3BO3 + 0.05 M NaCl. The exfoliation was performed by applying a constant voltage (12 V) between the graphite rods, while the temperature was kept constant (18 °C) with a temperature-controlled cryostat. The structural investigation of the graphene sample, performed by X-ray powder diffraction (XRD), revealed that the sample consists of a mixture of few-layer (69%), multi-layer graphene (14%) and graphene oxide (17%). In addition, XPS analysis proved that the sample was triple-doped with heteroatoms such as nitrogen (1.7 at%), sulfur (2.5 at%), and boron (3 at%). The sample was deposited onto the surface of a clean, glassy carbon electrode (GC) and investigated for the non-enzymatic electrochemical detection of L-tryptophan (TRP). The electrocatalytic properties of the EGr/GC electrode led to a considerable decrease in the oxidation potential from +0.9 V (bare GC) to +0.72 V. In addition, the EGr/GC electrode has higher sensitivity (two times) and a lower detection limit (ten times) in comparison with the bare GC electrode.
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