Environmentally friendly preparation of exfoliated graphite

H.M.A. Asghar; S.N. Hussain; H. Sattar; N.W. Brown; E.P.L. Roberts

Journal of Industrial and Engineering Chemistry, Vol.20, No.4, 1936-1941, July, 2014

DOI10.1016/j.jiec.2013.09.014 Export Citation

Environmentally friendly preparation of exfoliated graphite

H.M.A. Asghar^†, S.N. Hussain, H. Sattar¹, N.W. Brown², and E.P.L. Roberts³

Institute of Chemical Engineering & Technology, Punjab University, Quaid-e-Azam Campus, Lahore, Pakistan
¹School of Chemical Engineering and Analytical Science, The University of Manchester, M60 1QD, UK
²Arvia Technology Limited, Daresbury Innovation Centre, Keckwick Lane, Daresbury, Cheshire WA4 4FS, UK
³Department of Chemical and Petroleum Engineering, University of Calgary, 2500 University Dr NW, Calgary, AB T2N 1N4, Canada

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Graphite intercalation compounds (GIC) have received global attention in the last decade because of the growing number of applications of these materials. Conventionally, bisulfate intercalated graphite is synthesized by chemical intercalation; which requires concentrated sulfuric acid (98%) and an oxidizing agent such as H2O2 and HNO3. In this study, bisulfate intercalated graphite was prepared by electrochemical intercalation using dilute sulfuric acid with the aim to reduce the sulfur content in the final product. The electrochemical intercalation method required sulfuric acid with half of the concentration of that required for chemical intercalation, and without the need for an oxidizing agent. Chinese natural large flake graphite was used as the raw material for the electrochemical process. The GIC was characterized by the exfoliation volume obtained by thermal shock at a temperature of 850 ℃. The effect of sulfuric acid concentration, electrochemical treatment time, particle size and temperature on the exfoliation volume was investigated. It was found that the exfoliation volume of the GIC-bisulfate, which is a function of degree of intercalation, can be controlled using the sulfuric acid concentration and treatment time. A sulfuric acid concentration of 50% and an electrochemical treatment time of 60 min were found to produce a GIC with the maximum exfoliation volume for the range of conditions studied.

Keywords:Graphite intercalation compound;GIC;Graphite-bisulfate;Electrochemical intercalation;Exfoliation

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[Referenced By]

[1] Ebert LB, Annu. Rev. Mater. Sci., 6, 181 (1976)

[2] Chung DDL, J. Mater. Sci., 37(8), 1475 (2002)

[3] Vieira F, Cisneros I, Rosa NG, Trindade GM, Mohallem NDS, Carbon, 44, 2587 (2006)

[4] Sorokina NE, Leshin VS, Avdeev VV, J. Phys. Chem. Solids, 65, 185 (2010)

[5] Sorokina NE, Monyakina LA, Maksimova NV, Nikol IV, Avdeev VV, Inorg. Mater., 38(5), 589 (2002)

[6] Sorokina NE, Maksimova NV, Nikitin AV, Shornikova ON, Avdeev VV, Inorg. Mater., 37(6), 584 (2001)

[7] Dresselhaus MS, Dresselhaus G, Adv. Phys., 51(1), 1 (2002)

[8] Zabel H, Solin SA, Graphite Intercalation Compounds I: Structure and Dynamics, Vol. 14, Springer Series in Material Science, 1990 (in English).

[9] Jacobson AJ, Nazar LF, Encyclopedia of Inorganic Chemistry: Intercalation Chemistry, Wiley online library, John Wiley & Sons. Ltd., 2005 (in English).

[10] Hummers WS, Offeman RE, J. Am. Chem. Soc., 80, 1339 (1958)

[11] Chung DDL, J. Mater. Sci., 22, 4190 (1987)

[12] Brown NW, Development of a cleaner process for the manufacture of exfoliating graphite, in: Dissertation submitted as part of the Master of Science degree in Integrated Pollution Management, The University of Manchester, Institute of Science and Technology, Manchester, 1995.

[13] Li JH, Feng LL, Jia ZX, Mater. Lett., 60, 746 (2006)

[14] Ying ZR, Lin XM, Qi Y, Luo J, Mater. Res. Bull., 43(10), 2677 (2008)

[15] Inagaki M, Tashiro R, Washino Y, Toyoda M, J. Phys. Chem. Solids, 65, 133 (2004)

[16] Geim AK, Novoselov KS, Nat. Mater., 6 (2007)

[17] Lahde T, Mat. Res. Soc. (2010), Retrieved from: www.materialsforenergy.org (accessed on 18.12.12) (in English).

[18] Dreyer DR, Park S, Bielawski CW, Ruoff RS, Chem. Soc. Rev., 39, 228 (2010)

[19] Shao GL, Lu YG, Wu FF, Yang CL, Zeng FL, Wu QL, J. Mater. Sci., 47(10), 4400 (2012)

[20] Asbury Carbons, Carbon & Graphite, 2010 Retrieved from: www.asbury.com(02.02.10).

[21] Celzard A, Mareche JF, Furdin G, Carbon, 40, 2713 (2002)

[22] Celzard A, Schneider S, Mareche JF, Carbon, 40, 2185 (2002)

[23] Celzard A, Mareche JF, Furdin G, Prog. Mater. Sci., 50(1), 93 (2005)

[24] Celzard A, Mareche JF, Furdin G, J. Phys. Condens. Matter, 15, 7213 (2003)

[25] Minzhen C, Daniel T, Douglas AH, Hannes SC, J. Mater. Chem., 22 (2012)

[26] Bayat A, Aghamiri SF, Moheb A, Iran. J. Chem. Eng., 5(51), 51 (2008)