Alignment of Vertically Grown Carbon Nanostructures Studied by X-Ray Absorption Spectroscopy
Jeannot Mane Mane1,2, François Le Normand1, Rolant Eba Medjo3,4, Costel Sorin Cojocaru1, Ovidiu Ersen1, Antoine Senger1, Carine Laffon5, Bridinette Thiodjio Sendja2,3, César Mbane Biouele3, Germain Hubert Ben-Bolie3, Pierre Owono Ateba3, Philippe Parent5
1IPCMS, UMR 7504 CNRS, Strasbourg, France.
2Ecole Nationale Supérieure Polytechnique (National Advanced School of Engineering), Department of Mathematics and Physical Sciences, The University of Yaoundé I, Yaounde, Cameroon.
3Physics Department, Faculty of Science, University of Yaoundé I, Yaounde, Cameroon.
4Physics Department, Faculty of Science, University of Douala, Douala, Cameroon.
5LURE, UMR CNRS, Centre Universitaire Paris Sud, Orsay, France.
DOI: 10.4236/msa.2014.513098   PDF   HTML   XML   2,998 Downloads   3,978 Views   Citations

Abstract

X-Ray Absorption Spectroscopy (XAS) on the carbon K edge of carbon nanostructures (nanotubes, nanofibers, nanowalls) is reported here. They are grown on plain SiO2 (8 nm thick)/Si(100) substrates by a Plasma and Hot Filaments-enhanced Catalytic Chemical Vapor Deposition (PE HF CCVD) process. The morphology and the nature of these carbon nanostructures are characterized by SEM, TEM and Raman spectroscopy. According to conditions of catalyst preparation and DC HF CCVD process, carbon nanotubes (CNTs), carbon nanofibers (CNFs), carbon nanowalls (CNWs), carbon nanoparticles (CNPs) with different orientation of the graphene plans or shells can be prepared. From the angular dependence of the incident light and geometrical morphology of the nanostructures, wide variations of the C K-edge intensity of the transitions to the empty π* and σ* states occur. A full lineshape analysis of the XAS spectra has been carried out using a home-made software, allowing estimating the relative proportion of π* and σ* transitions. A geometrical model of the angular dependence with the incidence angle of the light and the morphology of the carbon nanostructures is derived. With normalization to the HOPG (Highly Oriented Pyrolytic Graphite graphite) reference case, a degree of alignment can be extracted which is representative of the localized orientation of the graphitic carbon π bonds, accounting not only for the overall orientation, but also for local defects like impurities incorporation, structural defects ... This degree of alignment shows good agreement with SEM observations. Thus CNTs films display degrees of alignment around 50%, depending on the occurrence of defects in the course of the growth, whereas no special alignment can be detected with CNFs and CNPs, and a weak one (about 20%) is detected on CNWs.

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Mane, J. , Le Normand, F. , Medjo, R. , Cojocaru, C. , Ersen, O. , Senger, A. , Laffon, C. , Sendja, B. , Biouele, C. , Ben-Bolie, G. , Ateba, P. and Parent, P. (2014) Alignment of Vertically Grown Carbon Nanostructures Studied by X-Ray Absorption Spectroscopy. Materials Sciences and Applications, 5, 966-983. doi: 10.4236/msa.2014.513098.

Conflicts of Interest

The authors declare no conflicts of interest.

References

[1] Iijima, S. (1991) Helical Microtubules of Graphitic Carbon. Nature, 354, 56-58.
http://dx.doi.org/10.1038/354056a0
[2] Groning, O., Kuttel, O.M., Emmenegger, C., Groning, P. and Schlapbach, L. (1999) Field Emission Properties of Carbon Nanotubes. Journal of Vacuum Science & Technology B: Microelectronics and Nanometer Structures, 18, 665.
http://dx.doi.org/10.1116/1.591258
[3] Dresselhaus, M.S., Dresselhaus, G. and Avouris, P. (2001) Carbon Nanotubes: Synthesis, Structure, Properties and Applications. Springer, Berlin, 29.
http://dx.doi.org/10.1007/3-540-39947-X
[4] Wei, Y., Xie, C., Dean, K.A. and Coll, B.F. (2001) Stability of Carbon Nanotubes under Electric Field Studied by Scanning Electron Microscopy. Applied Physics Letters, 79, 4527-4529.
http://dx.doi.org/10.1063/1.1429300
[5] Dai, L.M., Patil, A., Gong, X., Guo, Z., Liu, L., Liu, Y. and Zhu, D. (2003) Aligned Nanotubes. ChemPhysChem, 4, 1150-1169.
http://dx.doi.org/10.1002/cphc.200300770
[6] Mane Mane, J., Cojocaru, C.S., Barbier, A., Deville, J.P., Sendja, T. and Le Normand, F. (2007) GISAXS Study of Carbon Nanotubes Grown by CVD. Physica Status Solidi (a), 204, 4209-4229.
[7] Cao, A., Xu, C., Liang, J., Wu, D. and Wie, B. (2001) X-Ray Diffraction Characterization on the Alignment Degree of Carbon Nanotubes. Chemical Physics Letters, 344, 13.
http://dx.doi.org/10.1016/S0009-2614(01)00671-6
[8] Pinault, M., Pichot, P., Khodja, H., Launois, P., Mayne-L’Hermite, M. and Reynaud, C. (2005) Evidence of Sequential Lift in Growth of Aligned Multiwalled Carbon Nanotube Multilayers. Nano Letters, 5, 2394-2398.
http://dx.doi.org/10.1021/nl051472k
[9] Comelli, G., Stohr, J., Jark, W. and Pate, B.B. (1988) Extended X-Ray-Absorption Fine-Structure Studies of Diamond and Graphite. Physical Review B, 37, 4383-4389.
http://dx.doi.org/10.1103/PhysRevB.37.4383
[10] Yang, X.Q., Ruckman, M.W., Skotheim, T.A., Den Boer, M., Zheng, Y., Badzian, A.R., Badzian, T., Messier, R. and Srivatsa, A.R. (1991) Optical spectroscopic investigation of segmented trans-polyacetylene. Journal of Vacuum Science & Technology A: Vacuum, Surfaces, and Films, 9, 1140.
http://dx.doi.org/10.1116/1.577591
[11] Edamatsu, K., Takata, Y., Yokoyama, T., Seki, K., Tohnan, M., Okada, T. and Ohta, T. (1991) Local Structures of Carbon Thin Films Synthesized by the Hot Filament Chemical Vapor Deposition Method X-Ray-Absorption NearEdge Structure and Raman Spectroscopic Studies. Japanese Journal of Applied Physics, 30, 1073-1083.
http://dx.doi.org/10.1143/JJAP.30.1073
[12] Fayette, L., Marcus, B., Mermoux, M., Tourillon, G., Parent, P., Laffon, K. and Le Normand, F. (1998) Local Order in CVD Diamond Films: Comparative Raman, X-Ray-Diffraction and X-Ray-Absorption Near-Edge Studies. Physical Review B, 57, 14123-14132.
http://dx.doi.org/10.1103/PhysRevB.57.14123
[13] Garcia, M.M., Jimenez, I., Vazquez, L.K., Gomez-Aleixandre, C., Albella, J.M., Sanchez, O., Terminello, L.J. and Himpsel, F.J. (1998) X-Ray Absorption Spectroscopy and Atomic Force Microscopy Study of Bias-Enhanced Nucleation of Diamond Films. Applied Physics Letters, 72, 2105.
http://dx.doi.org/10.1063/1.121290
[14] Jimenez, I., Mar Garcia, M., Albella, J.M. and Terminello, L.J. (1998) Orientation of Graphitic Planes during the Bias-Enhanced Nucleation of Diamond on Silicon: An X-Ray Absorption Near-Edge Study. Applied Physics Letters, 73, 2911.
http://dx.doi.org/10.1063/1.122627
[15] Ripalda, J.M., Roman, E., Diaz, N., Galan, L., Montero, I., Comelli, G., Baraldi, A., Lizzit, S., Goldoni, A. and Paolucci, G. (1999) Correlation of X-Ray Absorption and X-Ray Photoemission Spectroscopies in Amorphous Carbon Nitride. Physical Review B, 60, R3705-R3708.
http://dx.doi.org/10.1103/PhysRevB.60.R3705
[16] Shimoyama, I., Wu, G., Sekiguchi, T. and Baba, Y. (2000) Evidence for the Existence of Nitrogen-Substituted Graphite Structure by Polarization Dependence of Near-Edge X-Ray-Absorption Fine Structure. Physical Review B, 62, R6053-R6056.
http://dx.doi.org/10.1103/PhysRevB.62.R6053
[17] Jimenez, I., Gago, R., Albella, J.M., Caceres, D. and Vergara, I. (2000) Spectroscopy of Π Bonding in Hard Graphitic Carbon Nitride Films: Superstructure of Basal Planes and Hardening Mechanisms. Physical Review B, 62, 4261-4264.
http://dx.doi.org/10.1103/PhysRevB.62.4261
[18] Mubumbila, N., Bouchet-Favre, B., Godon, C., Marhic, C., Angleraud, B., Tessier, P.Y. and Minea, T. (2004) EELS and NEXAFS Structural Investigations on the Effects of the Nitrogen Incorporation in a-CNx Films Deposited by R.F. Magnetron Sputtering. Diamond and Related Materials, 13, 1433-1436.
http://dx.doi.org/10.1016/j.diamond.2003.11.055
[19] Hellgren, N., Guo, J., Luo, Y., Sathe, C., Agui, A., Kashtanov, S., Nordgren, J., Agren, H. and Sundgren, J.E. (2005) Electronic Structure of Carbon Nitride Thin Films Studied by X-Ray Spectroscopy Techniques. Thin Solid Films, 471, 19-34.
http://dx.doi.org/10.1016/j.tsf.2004.03.027
[20] Comelli, G., Stohr, J., Robinson, C.J. and Jark, W. (1988) Structural Studies of Argon-Sputtered Amorphous Carbon Films by Means of Extended X-Ray-Absorption Fine Structure. Physical Review B, 38, 7511-7519.
http://dx.doi.org/10.1103/PhysRevB.38.7511
[21] Gago, R., Jimenez, I. and Albella, J.M. (2001) Detecting with X-Ray Absorption Spectroscopy the Modifications of the Bonding Structure of Graphitic Carbon by Amorphisation, Hydrogenation and Nitrogenation. Surface Science, 482-485, 530-536.
http://dx.doi.org/10.1016/S0039-6028(01)00939-6
[22] Yueh, C.L., Chiou, J.W. and Pong, W.F. (2001) Electronic Structure of the Fe-Layer-Catalyzed Carbon Nanotubes Studied by X-Ray-Absorption Spectroscopy. Applied Physics Letters, 79, 3179.
http://dx.doi.org/10.1063/1.1416165
[23] Imamura, M., Shimada, H., Matsubayashi, H., Yumura, M., Uchida, K., Oshima, S., Kuriki, Y., Yoshimura, Y., Yoshimura, Y., Sato, T. and Nishijima, A. (1994) Electron Energy-Loss Spectra of Single-Shell Carbon Nanotubes. Japanese Journal of Applied Physics, 33, L1316-L1319.
http://dx.doi.org/10.1143/JJAP.33.L1316
[24] Coffman, F.L., Cao, R., Pianetta, P.A., Kapoor, S., Kelly, M. and Terminello, L.J. (1996) Near-Edge X-Ray Absorption of Carbon Materials for Determining Bond Hybridization in Mixed sp2/sp3 Bonded Materials. Applied Physics Letters, 69, 568-570.
http://dx.doi.org/10.1063/1.117789
[25] Tang, Y.H., Zhang, P., Kim, P.S., Sham, T.K., Hu, Y.F. and Sun, X.H., et al. (2001) Amorphous Carbon Nanowires Investigated by Near-Edge-X-Ray-Absorption-Fine-Structures. Applied Physics Letters, 69, 3773.
http://dx.doi.org/10.1063/1.1425462
[26] Enouz, S., Bantignies, J.L., Babaa, M.R., Alvarez, L., Parent, P., Le Normand, F., Stéphan, O., Poncharal, P., Loiseau, A. and Doyle, B.P. (2007) Spectroscopic Study of Nitrogen Doping of Multi-Walled Carbon Nanotubes. Journal of Nanoscience and Nanotechnology, 7, 3524-3527.
http://dx.doi.org/10.1166/jnn.2007.839
[27] Kuznetsova, A., Popova, I., Yates, J.T., Bronikowski, M.J., Huffman, C.B., Liu, J., Smalley, R.E., Hwu, H.H. and Chen, J.G. (2001) Oxygen-Containing Functional Groups on Single-Wall Carbon Nanotubes: NEXAFS and Vibrational Spectroscopic Studies. Journal of the American Chemical Society, 123, 10699-10704.
http://dx.doi.org/10.1021/ja011021b
[28] Babaa, M.-R., Bantignies, J.-L., Alvarez, L., Parent, P., Le Normand, F., Gulas, M., Mane Mane, J., Poncharal, P. and Doyle, B.P. (2007) NEXAFS Study of Multi-Walled Carbon Nanotubes Functionalization with Sulfonated Poly(ether ether ketone) Chains. Journal of Nanoscience and Nanotechnology, 7, 3463-3467.
http://dx.doi.org/10.1166/jnn.2007.816
[29] Rosenberg, R.A., Love, P.J. and Rehn, V. (1986) Polarisation-Dependant Near-Edge X-Ray-Absorption Fine Structure of Graphite. Physical Review B, 33, 4034-4037.
http://dx.doi.org/10.1103/PhysRevB.33.4034
[30] Batson, P.E. (1993) Carbon 1s Near-Edge-Absorption Fine Structure in Graphite. Physical Review B, 48, 2608-2610.
http://dx.doi.org/10.1103/PhysRevB.48.2608
[31] Bruhwiler, P.A., Karis, O. and Martensson, N. (2002) Charge-Transfer Dynamics Studied Using Resonant Core Spectroscopies. Reviews of Modern Physics, 74, 703-740.
http://dx.doi.org/10.1103/RevModPhys.74.703
[32] Stohr, J. (1992) NEXAFS Spectroscopy. Springer, Berlin.
http://dx.doi.org/10.1007/978-3-662-02853-7
[33] Schiessling, J., Kjeldgaard, L., Rohmund, F., Falk, L.K.L., Campbell, E.E.B., Nordgren, J. and Bruhwiler, P.A. (2003) Synchrotron Radiation Study of the Electronic Structure of Multiwalled Carbon Nanotubes. Journal of Physics: Condensed Matter, 15, 6563-6579.
http://dx.doi.org/10.1088/0953-8984/15/38/022
[34] Banerjee, S., Hemraj-Benny, T., Sambavisan, S., Fischer, D.A., Misewich, J.A. and Wong, S.S. (2005) Near-Edge X-Ray Absorption Fine Structure Investigations of Order in Carbon Nanotube-Based Systems. The Journal of Physical Chemistry B, 109, 8489-8495.
http://dx.doi.org/10.1021/jp047408t
[35] Minea, T., Bouchet-Fabre, B., Lazar, S., Point, S. and Zandbergen, H.W. (2006) Angular and Local Spectroscopic Analysis to Probe the Vertical Alignment of N-Doped Well-Separated Carbon Nanotubes. The Journal of Physical Chemistry B, 110, 15659-15662.
http://dx.doi.org/10.1021/jp0637072
[36] Chiou, J.W., Yueh, C.L., Jan, J.C., Tsai, H.M., Pong, W.F., et al. (2002) Electronic Structure of the Carbon Nanotube Tips Studied by X-Ray-Absorption Spectroscopy and Scanning Photoelectron Microscopy. Applied Physics Letters, 81, 4189.
http://dx.doi.org/10.1063/1.1523152
[37] Cojocaru, C.S., Senger, A. and Le Normand, F. (2006) A Nucleation and Growth Model of Vertically-Oriented Carbon Nanofibers or Nanotubes by Plasma-Enhanced Catalytic Chemical Vapor Deposition. Journal of Nanoscience and Nanotechnology, 6, 1331-1338.
http://dx.doi.org/10.1166/jnn.2006.144
[38] Cojocaru, C.S. and Le Normand, F. (2006) On the Role of Activation Mode in the Plasmaand Hot Filaments-Enhanced Catalytic Chemical Vapour Deposition of Vertically Aligned Carbon Nanotubes. Thin Solid Films, 515, 53-58.
http://dx.doi.org/10.1016/j.tsf.2005.12.137
[39] Mane Mane, J., Cojocaru, C.S., Barbier, A., Deville, J.P., Jean, B., Metzger, T.H., Thiodjio Sendja, B. and Le Normand, F. (2007) GISAXS Study of the Alignment of Oriented Carbon Nanotubes Grown on Plain SiO2/Si(100) Substrates by a Catalytically Enhanced CVD Process. Physica Status Solidi (A), 204, 4209-4229.
http://dx.doi.org/10.1002/pssa.200723201
[40] Eba Medjo, R., Thiodjio Sendja, B., Mane Mane, J. and Owono Ateba, P. (2009) A Study of Carbon Nanotube Contamination by XANES Spectroscopy. Physica Scripta, 80, Article ID: 045601, 6 p.
http://dx.doi.org/10.1088/0031-8949/80/04/045601
[41] Sette, F., Wertheim, G.K., Ma, Y., Meigs, G., Modesti, S. and Chou, C.T. (1990) Lifetime and Screening of the C 1s Photoemission in Graphite. Physical Review B, 41, 9766-9770. http://dx.doi.org/10.1103/PhysRevB.41.9766
[42] Willis, R.F., Fitton, B. and Painter, G.S. (1974) Secondary-Electron Emission Spectroscopy and the Observation of High-Energy Excited States in Graphite: Theory and Experiment. Physical Review B, 9, 1926-1937.
http://dx.doi.org/10.1103/PhysRevB.9.1926
[43] Fischer, D.A., Wentzcovitch, R.M., Carr, R.G., Continenza, A. and Freeman, A.J. (1991) Graphitic Interlayer States—A Carbon-K Nearedge X-Ray-Absorption Fine-Structure Study. Physical Review B, 44, 1427-1429.
http://dx.doi.org/10.1103/PhysRevB.44.1427
[44] Dravid, V.P., Lin, X., Wang, Y., Wang, X.K., Yee, A., Ketterson, J.B. and Chang, R.P.H. (1993) Buckytubes and Derivatives: Their Growth and Implications for Buckyball Formation. Science, 259, 1601-1602.
[45] Mintmire, J.W., Dunlap, B.I. and White, C.T. (1992) Are Fullerene Tubules Metallic? Physical Review Letters, 68, 631-634.
http://dx.doi.org/10.1103/PhysRevLett.68.631
[46] Kuzuo, R., Terauchi, M., Tanaka, M., Saito, Y. and Japn. J. (1994) Electron Energy-Loss Spectra of Single-Shell Carbon Nanotubes. Japanese Journal of Applied Physics, 33, L1316-L1319.
http://dx.doi.org/10.1143/JJAP.33.L1316
[47] Hanada, T., Okada, Y. and Yase, K. (1999) The Science and Technology of Carbon Nanotubes. Elsevier, Oxford.
[48] Suzuki, S., Watanabe, Y., Kiyokura, T., Nath, K.G., Ogino, T., Heun, S., Zhu, W., Bower, C. and Zhou, O. (2001) Electronic Structure at Carbon Nanotube Tips Studied by Photoemission Spectroscopy. Physical Review B, 63, 1-7.
[49] Suzuki, S., Watanabe, Y., Ogino, T., Heun, S., Gregoratti, L., Barinov, A., Kaulich, B., Kiskinova, M., Zhu, W., Bower, C. and Zhou, O. (2002) Electronic Structure of Carbon Nanotubes Studied by Photoelectron Spectromicroscopy. Physical Review B, 66, 1-4.

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