Synthesis of Graphene with Microwave Irradiation in Liquid Phase

doi:10.3724/SP.J.1077.2012.11521

Abstract

Abstract: Graphite oxide was synthesized with Hummers method using natural flake graphite as carbon source, and then graphene was prepared through microwave irradiation in N-methyl-2-pyrrolidinone (NMP) solvent. NMP solvent was heated selectively during the microwave irradiation process, meantime, the oxygen containing groups of graphite oxide were decomposed into CO, CO₂ and H₂O gases, resulting in the exfoliation and reduction of graphite oxide. XRD, SEM, EDS, TEM, HRTEM, SAED, XPS and Raman were performed to characterize the synthesized graphene. The results indicate that the synthesized graphene is transparent with several microns in size, which consists of 2–5 graphitic layers with high crystalline structure. The synthesized graphene can disperse homogenously in the NMP solvent.

Key words: graphene, microwave irradiation, synthesis in liquid phase

CLC Number:

TQ383

WANG Can, WANG Yan-Li, ZHAN Liang, YANG Guang-Zhi, YANG Jun-He, QIAO Wen-Ming, LING Li-Cheng. Synthesis of Graphene with Microwave Irradiation in Liquid Phase[J]. Journal of Inorganic Materials, 2012, 27(7): 769-774.

References

[1] Geim A K, Novoselov K S. The rise of graphene. Nature Materials, 2007, 6(3): 183?191.

[2] Novoselov K S, Geim A K, Morozov S V, et al. Electric field effect in atomically thin carbon films. Science, 2004, 306(5696): 666?669.

[3] Zhang Y, Tan Y W, Stormer H L, et al. Experimental observation of the quantum Hall effect and Berry's phase in graphene. Nature,2005, 438(7065): 201?204.

[4] Stankovich S, Dikin D A, Dommett G H B, et al. Graphene-based composite materials. Nature, 2006, 442(7100): 282?286.

[5] Heersche H, Jarilloherrero P, Oostinga J, et al. Induced superconductivity in graphene. Solid State Communications. 2007, 143(1/2): 72?76.

[6] Kim W Y, Kim K S. Prediction of very large values of magnetoresistance in a graphene nanoribbon device. Nature Nanotechnology, 2008, 3(7): 408?412.

[7] Balandin A A, Ghosh S, Bao W, et al. Superior thermal conductivity of single-layer graphene. Nano Letters, 2008, 8(3): 902?907.

[8] Lee C, Wei X, Kysar J W, et al. Measurement of the elastic properties and intrinsic strength of monolayer graphene. Science, 2008, 321(5887): 385?388.

[9] Gilje S, Han S, Wang M, et al. A chemical route to graphene for device applications. Nano Letters, 2007, 7(11): 3394?3398.

[10] Wang X, Zhi L, Müllen K. Transparent, conductive graphene electrodes for dye-sensitized solar cells. Nano Letters, 2008, 8(1): 323?327.

[11] Stoller M D, Park S, Zhu Y, et al. Graphene-based ultracapacitors. Nano Letters, 2008, 8(10): 3498?3502.

[12] Stankovich S, Dikin D A, Dommett G H B, et al. Graphene-based composite materials. Nature,2006, 442(7100): 282?286.

[13] Park N, Hong S, Kim G, et al. Computational study of hydrogen storage characteristics of covalent-bonded graphenes. Journal of the American Chemical Society, 2007, 129(29): 8999?9003.

[14] Hass J, Feng R, Li T, et al. Highly ordered graphene for two dimensional electronics. Applied Physics Letters, 2006, 89(14): 143106–1–3.

[15] Vázquez A L, Calleja F, Borca B, et al. Periodically rippled graphene: growth and spatially resolved electronic structure. Physical Review Letters, 2008,100(5): 056807–1–4.

[16] Park S, Ruoff R S. Chemical methods for the production of graphenes. Nature Nanotechnology, 2009, 4(4): 217–224.

[17] Schniepp H C, Li J L, McAllister M J, et al. Functionalized single graphene sheets derived from splitting graphite oxide. Journal of Physical Chemistry B, 2006, 110(17): 8535–8539.

[18] Lotya M, Hernandez Y, King P J, et al. Liquid phase production of graphene by exfoliation of graphite in surfactant/water solutions. Journal of the American Chemical Society, 2009, 131(10): 3611–3620.

[19] WANG Can, WANG Yan-Li, ZHAN Liang, et al. Synthesis of nitrogen doped graphene through microwave irridation. Journal of Inorganic Materials, 2012. 27(2): 146–150.

[20] Zhang W X, Cui J C, Tao C A, et al. A strategy for producing pure single-layer graphene sheets based on a confined self-assembly approach. Angewandte Chemie International Edition, 2009, 48(32): 5864–5868.

[21] Chen H Q, Müller M B, Gilmore K J, et al. Mechanically strong, electrically conductive, and biocompatible graphene paper. Advanced Materials, 2008, 20(18): 3557–3561.

[22] Zhou Y, Bao Q L, Tang L A L, et al. Hydrothermal dehydration for the “green” reduction of exfoliated graphene oxide to graphene and demonstration of tunable optical limiting properties. Chemical Materials, 2009, 21(13): 2950–2956.

[23] Zhu Y W, Stoller M D, Cai W W, et al. Exfoliation of graphite oxide in propylene carbonate and thermal reduction of the resulting graphene oxide platelets. ACS Nano, 2010, 4(2): 1227–1233.

[24] Stankovicha S, Dikina D A, Pinera R D, et al. Synthesis of graphene-based nanosheets via chemical reduction of exfoliated graphite oxide. Carbon, 2007, 45(7): 1558–1565.

[25] McAllister M J, Li J L, Adamson D H, et al. Single sheet functionalized graphene by oxidation and thermal expansion of graphite. Chemical Materials, 2007, 19(18): 4396–4404.

[26] Hernandez Y, Nicolosi V, Lotya M, et al. High yield production of graphene by liquid phase exfoliation of graphite. Nature Nanotechnology, 2008, 3(9): 563–568.

[27] Fan X B, Peng W C, Li Y, et al. Deoxygenation of exfoliated graphite oxide under alkaline conditions: a green route to graphene preparation. Advanced Materials, 2008, 20(23): 4490–4493.

[28] Lu W, Tang D M, He Y B, et al. Low-temperature exfoliated graphenes: vacuum-promoted exfoliation and electrochemical energy storage. ACS Nano, 2009, 3(11): 3730–3736.