Saeedi, S., Sargolzaei, J. (2024). Investigating The Effect of Various Parameters on The Yield of Graphene Obtained Through Graphite Exfoliation Using CO2 Supercritical Fluid. , 42(3), 337-355. doi: 10.30684/etj.2023.143211.1569
Shahab A. Saeedi; Javad Sargolzaei. "Investigating The Effect of Various Parameters on The Yield of Graphene Obtained Through Graphite Exfoliation Using CO2 Supercritical Fluid". , 42, 3, 2024, 337-355. doi: 10.30684/etj.2023.143211.1569
Saeedi, S., Sargolzaei, J. (2024). 'Investigating The Effect of Various Parameters on The Yield of Graphene Obtained Through Graphite Exfoliation Using CO2 Supercritical Fluid', , 42(3), pp. 337-355. doi: 10.30684/etj.2023.143211.1569
Saeedi, S., Sargolzaei, J. Investigating The Effect of Various Parameters on The Yield of Graphene Obtained Through Graphite Exfoliation Using CO2 Supercritical Fluid. , 2024; 42(3): 337-355. doi: 10.30684/etj.2023.143211.1569

Investigating The Effect of Various Parameters on The Yield of Graphene Obtained Through Graphite Exfoliation Using CO2 Supercritical Fluid

Engineering and Technology Journal
Article 2, Volume 42, Issue 3, March 2024, Pages 337-355    PDF (2.39 M)
Document Type: Research Paper
DOI: 10.30684/etj.2023.143211.1569
Authors
Shahab A. Saeedi; Javad Sargolzaei*
Department of Chemical Engineering, Faculty of Engineering, Ferdowsi University of Mashhad, Mashhad, Iran
Abstract
Due to its high penetration force and low viscosity, the Supercritical carbon dioxide (scCO2) can spread between the graphite layers, overcome van der Waals forces, and transform graphite into multilayer graphene. The results of the test plan with the Design Expert software and also the use of these results in the laboratory showed that the parameters of temperature, pressure, initial amount of graphite, addition of surfactant and solvent auxiliary, the duration of sample placement in the device, the duration of carbon dioxide gas release from the device, and the time and power of ultrasonic and centrifuge operations can accelerate the exfoliation process. The resulting graphene was characterized by TEM, RAMAN, XRD, and AFM techniques. Based on the obtained results, it was found that mono/bilayer graphene was obtained by applying optimum conditions. The results confirmed the formation of mono/bilayer graphene based on the G-Band of 1583 cm-1 in the Raman test, a wavelength of 26.44° in the XRD test, and a thickness of 1.5 nm in the AFM test. With a simple, low-cost approach, this method, without using toxic and expensive chemicals with high profitability, can replace other complex graphene production methods, such as chemical vapor leakage and plasma etching, and be chemically reduced.

Highlights
  • Conventional methods of graphene production are time-consuming and expensive.
  • The parameters affecting the extraction of graphene from graphite were investigated using Supercritical CO2.
  • Additives used in the synthesis process have the role of deactivating the surface.
  • The test design was done with "Design Expert" software and then tested in the laboratory.
  • The software results were in high agreement with the laboratory results, and mono/bilayer graphene was obtained.
Keywords
Graphite; scCO2; Exfoliation; Characterization; Design Expert
References
  1. Yi, Z. Shen, A review on mechanical exfoliation for scalable production of graphene, J. Mater. Chem. A, 35 (2015) 11700-11715. https://doi.org/10.1039/C5TA00252D
  2. K. Tiwari, S. Sahoo, N. Wang, A .Huczko, Graphene research and their outputs: Status and prospect, J. Sci. Adv. Mater. Devices., 5 (2020) 10-29. https://doi.org/10.1016/j.jsamd.2020.01.006
  3. M. da Costa, C.M. Hussain, Ethical, legal, social and economic issues of graphene, Compr. Anal. Chem., 91 (2020) 263-279. https://doi.org/10.1016/bs.coac.2020.08.010
  4. B. Wang, J.Z. Yin, Q.Q. Xu, J.T. Zhi, Insightful understanding of shear-assisted supercritical CO2 exfoliation for fabricating graphene nanosheets through the combination of kinetics and process parameters, Ind. Eng. Chem. Res., 59 (2020) 10967–10975. https://doi.org/10.1021/acs.iecr.0c01744
  5. Yan, F.Z. Nashath, S. Chen, S. Manickam, S.S. Lim, H. Zhao, E. Lester, T. Wu, C.H. Pang‏, Synthesis of graphene: Potential carbon precursors and approaches, J. Nanotechnol. Rev., 9 (2020) 1284-1314. https://doi.org/10.1515/ntrev-2020-0100
  6. S. Owuor, A. Khan, C.L. Leon, S. Ozden, R. Priestley, C. Arnold, N. Chopra, C.S. Tiwary‏, Roadblocks faced by graphene in replacing graphite in large-scale applications, Oxf. open mater. Sci., 40 (2021)1-19. https://doi.org/10.1093/oxfmat/itab004
  7. C. Lee, W.W. Liu, S.P. Chai, A.R. Mohamed, A. Aziz, C.S. Khe, N.M.S. Hidayah, U. Hashim‏, Review of the synthesis, transfer, characterization and growth mechanisms of single and multilayer graphene, J. RSC Adv., 7 (2017) 15644-15693. https://doi.org/10.1039/C7RA00392G
  8. Li, S.K. Cushing, X .Zhou, S. Guo, N. Wu , Fingerprinting photoluminescence of functional groups in graphene oxide, J. Mater. Chem., 22 (2012) 23374-23379. https://doi.org/10.1039/C2JM35417A
  9. Liu, G. Hu, H. Gao, Preparation of few-layer and single-layer graphene by exfoliation of expandable graphite in supercritical N,N-dimethylformamide, J. Supercrit. Fluids, 63 (2012) 99-104. https://doi.org/10.1016/j.supflu.2012.01.002
  10. P. Sasikala, P. Poulin, C. Aymonier, Prospects of Supercritical Fluids in Realizing Graphene-Based Functional Materials, J. Adv. Mater., 28 (2016) 2663-2691. https://doi.org/10.1002/adma.201504436
  11. Sun, Q. Fan, M. Zhang, S. Liu, H Tao, J. Texter‏, Supercritical Fluid-Facilitated Exfoliation and Processing of 2D Materials, Adv. Sci., 6 (2019) 1901084. https://doi.org/10.1002/advs.201901084
  12. Ahangari, J. Sargolzaei‏, Extraction of lipids from spent coffee grounds using organic solvents and supercritical carbon dioxide, J. Food Process. Preserv., 37 (2013) 1014-1021. https://doi.org/10.1111/j.1745-4549.2012.00757.x
  13. Ahangari, J. Sargolzaei, Extraction of pomegranate seed oil using subcritical propane and supercritical carbon dioxide, Theor. Found. Chem. Eng., 46 (2012) 258–265. https://doi.org/10.1134/S0040579512030013
  14. Ahangari, J. Sargolzaei, Supercritical Fluid Extraction of Oils from Pomegranate Seeds, J. Am. Oil. Chem. Soc., 94 (2017) 1415-1415. https://doi.org/10.1007/s11746-011-1789-9
  15. W. Pu, C.A. Wang, Y. Sung, Y.M. Liu, M.D. Ger, Production of few-layer graphene by supercritical CO2 exfoliation of graphite, Mater. Lett., 63 (2009) 1987-1989. https://doi.org/10.1016/j.matlet.2009.06.031
  16. H Gao, G Hu,‏ Graphene production via supercritical fluids, RSC Adv., 12 (2016) 10132-10143. https://doi.org/10.1039/C5RA15568A
  17. Sun, Q. Fan, M. Zhang, S. Liu, H. Tao, J. Texter‏, Supercritical fluid-facilitated exfoliation and processing of 2D materials, Adv. Sci., 6 (2019) 1-34. https://doi.org/10.1002/advs.201901084
  18. Rangappa, K .Sone, M .Wang, U.K. Gautam, D. Golberg, H. Itoh, M. Ichihara, I. Honma‏,Rapid and direct conversion of graphite crystals into high-yielding, good-quality graphene by supercritical fluid exfoliation, Journal of Chem. Europe. Chem. Eur. J., 16 (2010) 6488-6494. https://doi.org/10.1002/chem.201000199
  19. Zhu, J. Yin, Study on cloud point pressure of EmimTf2N in supercritical carbon dioxide microemulsions based on non-ionic surfactant and role of solubilized water, J. Mol. Liq., 310 (2020) 113299. https://doi.org/10.1016/j.molliq.2020.113299
  20. Zhu, Y. Li, D. Zhou, Q. Xu, J. Yin, Molecular dynamics study on microstructure of supercritical CO2 microemulsions containing ionic liquids, Colloids Surf. A Physicochem. Eng. Asp., 603 (2020) 125272. https://doi.org/10.1016/j.colsurfa.2020.125272
  21. Yu, Y. Liu, J. Yin, Separation of 1,3-propanediol using supercritical CO2 microemulsion with non-ionic surfactant Ls-54: experiment and simulation, Chem. Eng. J., 273 (2015) 197-204. https://doi.org/10.1016/j.cej.2015.03.082
  22. Navik, H. Tan, Z. Liu, Q. Xiang, Y. Zhao, Scalable production of high-quality exfoliated graphene using mechanical milling in conjugation with supercritical CO2, FlatChem, 33 (2022) 100374. https://doi.org/10.1016/j.flatc.2022.100374
  23. Kumar, H..S Farwaha, N. Ranjan, Use of Response Surface Methodology to Optimize the crystalline size of rice husk derived graphene produced by microwave process, IOP Conf. Ser.: Earth Environ. Sci., 1110,2023,012069. https://doi.org/10.1088/1755-1315/1110/1/012069
  24. L. Leong, H.N. Lim, I. Ibrahim, Graphene in rubber formulations: a comprehensive review and performance optimization insights, Mol. Syst. Des. Eng., 8 (2023) 1229-1251. https://doi.org/10.1039/D3ME00082F
  25. A. AbdulRazak, Z.M. Shakor, S. Rohani, Optimizing Biebrich Scarlet removal from water by magnetic zeolite 13X using response surface method, J. Environ. Chem. Eng., 6 (2012) 6175-6183. https://doi.org/10.1016/j.jece.2018.09.043
  26. Al-Dahri, A.A.J. AbdulRazak, I.H. Khalaf, S. Rohani‏, Response surface modeling of the removal of methyl orange dye from its aqueous solution using two types of zeolite synthesized from coal fly ash, Mater. Express, 8 (2018) 234-244. https://doi.org/10.1166/mex.2018.1433
  27. Wu, X. Yang, A molecular simulation of interactions between graphene nanosheets and supercritical CO2, J. Colloid Interface Sci., 361 (2011) 1-8. https://doi.org/10.1016/j.jcis.2011.05.021
  28. Gao, G. Hu‏, Graphene production via supercritical fluids, RSC Adv., 6 (2016) 10132-10143. https://doi.org/10.1039/C5RA15568A
  29. Li, J Xu, G. Li, X. Jia, Y. Li, F. Yang, L. Zhang, Preparation of graphene nanosheets by shear-assisted supercritical CO2 exfoliation, Chem. Eng. J., 284 (2016) 78-84. https://doi.org/10.1016/j.cej.2015.08.077
  30. Hadi, J. Karimi-Sabet, S.M.A. Moosavian, Optimization of graphene production by exfoliation of graphite in supercritical ethanol: A response surface methodology approach, J. Supercrit. Fluids, 107 (2016) 92-105. https://doi.org/10.1016/j.supflu.2015.08.022
  31. Xu, J.W. McGraw, F. Gao, M. Grundy, Z. Ye, Production of High-Concentration Graphene Dispersions in Low-Boiling-Point Organic Solvents by Liquid-Phase Noncovalent Exfoliation of Graphite with a Hyperbranched Polyethylene and Formation of Graphene/Ethylene Copolymer Composites, J. Phys. Chem. C, 117 (2013) 0730–10742. https://doi.org/10.1021/jp4008009
  32. Zhao, X. Pang, Z. Zhai, Preparation and Antiflame Performance of Expandable Graphite Modified with Sodium Hexametaphosphate, Hindawi Publishing Corporation, J. Polym., 2015 (2015) 5. http://dx.doi.org/10.1155/2015/821297
  33. J. Goldie, S. Bush, J.A. Cumming, A Statistical Approach to Raman Analysis of Graphene-Related Materials: Implications for Quality Control, ACS Appl. Nano Mater., 3 (2020) 11229–11239. https://doi.org/10.1021/acsanm.0c02361
  34. Adetayo, D. Runsewe, Synthesis and Fabrication of Graphene and Graphene Oxide: A Review, Open Journal of Composite Materials., 9 (2019) 207-229. https://doi.org/10.4236/ojcm.2019.92012
  35. Li, L. Deng, I.A. Kinloch, R.J. Young, Raman spectroscopy of carbon materials and their composites: Graphene, nanotubes and fibres, Prog. Mater. Sci., 135 (2023) 101089. https://doi.org/10.1016/j.pmatsci.2023.101089
  36. O. Yukhymchuk, M.Y. Valakh, O.M. Hreshchuk, Y.O. Havrylyuk, I.B. Yanchuk, A.V. Yefanov, Properties of Graphene Flakes Obtained by Treating Graphite with Ultrasound, Ukr. J. Phys., 62 (2017) 432-440. https://doi.org/10.15407/ujpe62.05.0432
  37. Lopez-Diaz, J.A. Delgado-Notario, V. Clerico, E. Diez, M.D. Merchan, M.M. Velazquez‏,Towards Understanding the Raman Spectrum of Graphene Oxide: The Effect of the Chemical Composition, Coatings, 10 (2020) 524. https://doi.org/10.3390/coatings10060524
  38. S. Khan, A. Shakoor, G.T. Khan, S. Sultana, A. Zia, A Study of Stable Graphene Oxide Dispersions in Various Solvents, J. Chem. Soc. Pak., 37 (2015) 62-67.
  39. Li, Z. Zhang, C. Zhong, Y. Liu, Q. Zhou, Solubility of solid solutes in supercritical carbon dioxide with and without co-solvents, Fluid Phase Equilib., 207 (2003) 183-192. https://doi.org/10.1016/S0378-3812(03)00022-0
  40. B. Mbayachi, E. Ndayiragije, T. Sammani, S. Taj, E.R. Mbuta, A.U. Khan, Graphene synthesis, Characterization and its applications: A review, Results Chem., 3 (2021) 100163. https://doi.org/10.1016/j.rechem.2021.100163
  41. Yi, Z. Shen, S. Ma, X. Zhang, A mixed-solvent strategy for facile and green preparation of graphene by liquid-phase exfoliation of graphite, J. Nanopart. Res., 14 (2012)1-9. https://doi.org/10.1007/s11051-012-1003-5
  42. A. Bhuyan, M.D. Nizam Uddin, M. Islam, F. A. Bipasha, S.S. Hossain, Synthesis of graphene, Int Nano Lett., 6 (2016) 65-83. https://doi.org/10.1007/s40089-015-0176-1
  43. Liu, Q. Tang, B. Huang, Y. Wang‏, Graphene Synthesis: Method, Exfoliation Mechanism and Large-Scale Production, Crystals, 12 (2022) 25. https://doi.org/10.3390/cryst12010025
  44. Li, J. Xu, G. Li, X. Jia, Y. Li, F. Yang, L. Zhang, Preparation of graphene nanosheets by shear-assisted supercritical CO2 exfoliation, Chem. Eng. J., 284 (2016) 78-84. https://doi.org/10.1016/j.cej.2015.08.077
  45. I. Silva, D.A. Mirabella, J.P. Tomba, C.C. Riccardi, Optimizing graphene production in ultrasonic devices, Ultrasonics, 100 (2020) 105989. https://doi.org/10.1016/j.ultras.2019.105989
  46. Liu, R. Navik, H. Tan, Q. Xiang, M. Goto, Graphene-based materials prepared by supercritical fluid technology and its application in energy storage, J. Supercrit. Fluids,188 (2022) 105672. https://doi.org/10.1016/j.supflu.2022.105672
  47. Xu, Q. Xu, N. Wang, Z. Chen, Q. Tian, H. Yang, Reverse-Micelle-Induced Exfoliation of Graphite into Graphene Nanosheets with Assistance of Supercritical CO2, Chem. Mater., 27 (2015) 3262–3272. https://doi.org/10.1021/acs.chemmater.5b00092
  48. Kumar, R. Salehiyan, V. Chauke, O.J. Botlhoko, K. Setshedi, M. Scriba, M. Masukume, S.S. Ray, Top-down synthesis of graphene: A comprehensive review, FlatChem, 27 (2021) 100224. https://doi.org/10.1016/j.flatc.2021.100224
  49. Saikam, P .Arthi, B. Senthil, M. Shanmugam, A review of exfoliated graphite: synthesis and applications, J.Inorg. Chem. Commun., 152 (2023) 110685. https://doi.org/10.1016/j.inoche.2023.110685
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