Abstract
The synthesis of well-aggregated carbon nanotubes in the form of bundles was achieved by the catalytic reduction of 1,2-dichlorobenzene by a solvothermal approach. The use of 1,2-dichlorobenzene as a carbon source yielded a comparably good percentage of carbon nanotubes in the range of 60–70 %, at a low reaction temperature of 200°C. The products obtained were analysed by X-ray diffraction, Raman spectroscopy, scanning electron microscopy, and transmission electron microscopy techniques. The X-ray diffraction studies implied the presence of pure, crystalline, and well-ordered carbon nanotubes. The scanning electron and transmission electron microscopic images revealed the surface morphology, dimensions and the bundled form of the tubes. These micrographs showed the presence of multi-walled carbon nanotubes with an outer diameter of 30–55 nm, inner diameter of 15–30 nm, and lengths of several hundreds of nanometers. Brunauer-Emmett-Teller-based N2 gas adsorption studies were performed to determine the surface area and pore volume of the carbon nanotubes. These carbon nanotubes exhibit a better surface area of 385.30 m2 g−1. In addition, the effects of heating temperature, heating time, amount of catalyst and amount of carbon source on the product yield were investigated.
Similar content being viewed by others
References
Baughman, R. H., Cui, C. X., Zakhidov, A. A., Iqbal, Z., Barisci, J. N., Spinks, G. M., Wallace, G. G., Mazzoldi, A., De Rossi, D., Rinzler, A. G., Jaschinski, O., Roth, S., & Kertesz, M. (1999). Carbon nanotube actuators. Science, 284, 1340–1344. DOI: 10.1126/science.284.5418.1340.
Benito, A. M., Maniette, Y., Muñoz, E., & Martínez, M. T. (1998). Carbon nanotubes production by catalytic pyrolysis of benzene. Carbon, 36, 681–683. DOI: 10.1016/s0008-6223(98)00039-6.
Bera, D., Johnston, G., Heinrich, H., & Seal, S. (2006). A parametric study on the synthesis of carbon nanotubes through arc-discharge in water. Nanotechnology, 17, 1722–1730. DOI: 10.1088/0957-4484/17/6/030.
Bethune, D. S., Kiang, C. H., Devries, M. S., Gorman, G., Savoy, R., Vazquez, J., & Beyers, R. (1993). Cobalt-catalysed growth of carbon nanotubes with single-atomic-layer walls. Nature, 363, 605–607. DOI: 10.1038/363605a0.
Branca, C., Frusteri, F., Magazu, V., & Mangione, A. (2004). Characterization of carbon nanotubes by TEM and infrared spectroscopy. The Journal of Physical Chemistry B, 108, 3469–3473. DOI: 10.1021/jp0372183.
Brunauer, S., Emmett, P. H., & Teller, E. (1938). Adsorption of gases in multimolecular layers. Journal of the American Chemical Society, 60, 309–319. DOI: 10.1021/ja01269a023.
Cao, A. Y., Xu, C. L., Liang, J., Wu, D. H., & Wei, B. Q. (2001). X-ray diffraction characterization on the alignment degree of carbon nanotubes. Chemical Physics Letters, 344, 13–17. DOI: 10.1016/s0009-2614(01)00671-6.
Costa, S., Borowiak-Palen, E., Kruszyńska, M., Bachmatiuk, A., & Kalenczuk, R. J. (2008). Characterization of carbon nanotubes by Raman spectroscopy. Materials Science-Poland, 26, 433–441.
Dai, H., Rinzler, A. G., Nikolaev, P., Thess, A., Colbert, D. T., & Smalley, R. E. (1996). Single-wall nanotubes produced by metal-catalyzed disproportionation of carbon monoxide. Chemical Physics Letters, 260, 471–475. DOI: 10.1016/0009-2614(96)00862-7.
Herreyre, S., & Gadelle, P. (1995). Effect of hydrogen on the morphology of carbon deposited from the catalytic disproportionation of CO. Carbon, 33, 234–237. DOI: 10.1016/0008-6223(95)92803-m.
Iijima, S. (1991). Helical microtubules of graphitic carbon. Nature, 354, 56–58. DOI: 10.1038/354056a0.
Jian, S. R., Chen, Y. T., Wang, C. F., Wen, H. C., Chiu, W. M., Yang, C. S. (2008). The influences of H2 plasma pretreatment on the growth of vertically aligned carbon nanotubes by microwave plasma chemical vapor deposition. Nanoscale Research Letters, 3, 230–235. DOI: 10.1007/s11671-008-9141-5.
Jiang, Y., Wu, Y., Zhang, S. Y., Xu, C. Y., Yu, W. C., Xie, Y., & Qian, Y. T. (2000). A catalytic-assembly solvothermal route to multiwall carbon nanotubes at a moderate tem perature. Journal of the American Chemical Society, 122, 12383–12384. DOI: 10.1021/ja002387b.
Karmakar, S., Sharma, S. M., & Sood, A. K. (2005). Studies on high pressure behavior of carbon nanotubes: X-ray diffraction measurements using synchrotron radiation. Nuclear Instruments and Methods in Physics Research Section B, 238, 281–284. DOI: 10.1016/j.nimb.2005.06.064.
Kim, P., & Lieber, C. M. (1999). Nanotube nanotweezers. Science, 286, 2148–2150. DOI: 10.1126/science.286.5447.2148.
Kim, H. H., & Kim, H. J. (2007). New DC arc discharge synthesis method for carbon nanotubes using xylene ferrocene as floating catalyst. Japanese Journal of Applied Physics, 46, 1818–1820. DOI: 10.1143/jjap.46.1818.
Kong, J., Franklin, N. R., Zhou, C. W., Chapline, M. G., Peng, S., Cho, K. J., & Dai, H. J. (2000). Nanotube molecular wires as chemical sensors. Science, 287, 622–625. DOI: 10.1126/science.287.5453.622.
Liu, C., Fan, Y. Y., Liu, M., Cong, H. T., Cheng, H. M., & Dresselhaus, M. S. (1999). Hydrogen storage in single-walled carbon nanotubes at room temperature. Science, 286, 1127–1129. DOI: 10.1126/science.286.5442.1127.
Liu, J. W., Shao, M. W., Chen, X. Y., Yu, W. C., Liu, X. M., & Qian, Y. T. (2003). Large-scale synthesis of carbon nanotubes by an ethanol thermal reduction process. Journal of the American Chemical Society, 125, 8088–8089. DOI: 10.1021/ja035763b.
Mahanandia, P., Vishwakarma, P. N., Nanda, K. K., Prasad, V., Barai, K., Mondal, A. K., Sarangi, S., Dey, G. K., Subramanyam, S. V. (2008). Synthesis of multi-wall carbon nanotubes by simple pyrolysis. Solid State Communications, 145, 143–148. DOI: 10.1016/j.ssc.2007.10.020.
Manafi, S. A., Amin, M. H., Rahimipour, M. R., Salahi, E., & Kazemzadeh, A. (2009). High-yield synthesis of multiwalled carbon nanotube by mechanothermal method. Nanoscale Research Letters, 4, 296–302. DOI: 10.1007/s11671-008-9240-3.
Rodriguez, N. M. (1993). A review of catalytically grown carbon nanofibers. Journal of Materials Research, 8, 3233–3250. DOI: 10.1557/jmr.1993.3233.
Scott, C. D., Arepalli, S., Nikolaev, P., & Smalley, R. E. (2001). Growth mechanisms for single-wall carbon nanotubes in a laser-ablation process. Applied Physics A, 72, 573–580. DOI: 10.1007/s003390100761.
Shim, M., Javey, A., Kam, N. W. S., & Dai, H. (2001). Polymer functionalization for air-stable N-type carbon nanotube fieldeffect transistors. Journal of the American Chemical Society, 123, 11512–11513. DOI: 10.1021/ja0169670.
Tsang, S. C., Harris, P. J. F., & Green, M. L. H. (1993). Thinning and opening of carbon nanotubes by oxidation using carbon dioxide. Nature, 362, 520–522. DOI: 10.1038/362520a0.
Wang, X. J., Lu, J., Xie, Y., Du, G., Guo, Q. X., & Zhang, S. Y. (2002). A novel route to multiwalled carbon nanotubes and carbon nanorods at low temperature. Journal of Physical Chemistry B, 106, 933–937. DOI: 10.1021/jp0130719.
Wang, W. Z., Kunwar, S., Huang, J. Y., Wang, D. Z., & Ren, Z. F. (2005). Low temperature solvothermal synthesis of multiwall carbon nanotubes. Nanotechnology, 16, 21–23. DOI: 10.1088/0957-4484/16/1/005.
Wu, H. C., Chang, X. L, Liu, L., Zhao, F., & Zhao, Y. L. (2010). Chemistry of carbon nanotubes in biomedical applications. Journal of Materials Chemistry, 20, 1036–1052. DOI: 10.1039/b911099m.
Yuan, D. S., Liu, Y. L., Xiao, Y., & Chen, L. Q. (2008). Preparation and characterization of Z-shaped carbon nanotubes via decomposing magnesium acetate. Materials Chemistry and Physics, 112, 27–30. DOI: 10.1016/j.matchemphys.2008.04.040.
Zdrojek, M., Gebicki, W., Jastrzebski, C., Melin, T., & Huczko, A. (2004). Studies of multiwall carbon nanotubes using Raman spectroscopy and atomic force microscopy. Solide State Phenomena, 99, 265–268. DOI: 10.4028/www.scientific.net/ssp.99-100.265.
Zubizarreta, L., Arenillas, A., & Pis, J. J. (2009). Carbon materials for H2 storage. International Journal of Hydrogen Energy, 34, 4575–4581. DOI: 10.1016/j.ijhydene.2008.07.112.
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Krishnamurthy, G., Agarwal, S. Efficient synthesis of carbon nanotubes with improved surface area by low-temperature solvothermal route from dichlorobenzene. Chem. Pap. 67, 1396–1403 (2013). https://doi.org/10.2478/s11696-013-0397-6
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.2478/s11696-013-0397-6