Absorption spectroscopy in the ultraviolet-visible-near infrared (UV-Vis-NIR) wavelength region has been used to quantify the aggregation factor of single-walled carbon nanotubes (SWCNTs) in liquid media through a series of controlled experiments. SWCNT bundles are dispersed in selected solvents using a calibrated ultrasonicator, which helps in determining the true amount of energy used in the exfoliation process. We also establish the selectivity of the centrifugation process, under the conditions used, in removing the nanotube aggregates as a function of the sonication time and the dispersion solvent. This study, along with the calibration of the sonication process, is shown to be very important for measuring the true aggregation factor of SWCNTs through a modified approach. We also show that the systematic characterization of SWCNT dispersions by optical spectroscopy significantly contributes to the success of dielectrophoresis (DEP) of nanotubes at predefined on-chip positions. The presence of individually dispersed SWCNTs in the dispersions is substantiated by dielectrophoretic assembly and post-DEP electromechanical measurements. 1. Introduction Single-walled carbon nanotubes (SWCNTs) have attracted significant interest in basic and applied nanomaterials research [1, 2] due to their exceptional electrical [3], mechanical [4], optical [5], and thermal properties [6]. In order to exploit these attractive properties [7], SWCNTs have been proposed as components in a variety of applications like sensors [8, 9], field effect transistors [10], interconnects in CMOS technology [11], electromechanical springs [12], and field emission sources [13], as additives in composite materials for enhanced mechanical properties [14], and as medical therapeutic agents [15]. In spite of their huge promise, the success of SWCNT devices still remains uncertain at a commercial level. This is because SWCNTs exist in a wide range of diameters, lengths, chiralities (the rollup axis), structural purity, and states of aggregation [16]. Therefore, fabrication schemes need good selectivity in order to control the physical properties of SWCNTs and thus their device properties. This selectivity can be obtained either through controlled growth to limit the variability among the as-grown nanotubes [17–19] or postgrowth purification and sorting techniques [20–22]. SWCNTs in the native form exist in a bundled state. For a number of the postgrowth SWCNT sorting techniques, it is desired to have the nanotubes dispersed uniformly in a liquid medium [20–22]. It is, however, difficult to
References
[1]
P. L. McEuen, “Single-wall carbon nanotubes,” Physics World, vol. 13, no. 6, pp. 31–36, 2000.
[2]
J. Kong, C. Zhou, A. Morpurgo et al., “Synthesis, integration, and electrical properties of individual single-walled carbon nanotubes,” Applied Physics A: Materials Science and Processing, vol. 69, no. 3, pp. 305–308, 1999.
[3]
C. Zhou, J. Kong, and H. Dai, “Intrinsic electrical properties of individual single-walled carbon nanotubes with small band gaps,” Physical Review Letters, vol. 84, no. 24, pp. 5604–5607, 2000.
[4]
J. Salvetat, G. A. D. Briggs, J. Bonard et al., “Elastic and shear moduli of single-walled carbon nanotube ropes,” Physical Review Letters, vol. 82, no. 5, pp. 944–947, 1999.
[5]
T. I. Jeon, K. J. Kim, C. Kang et al., “Optical and electrical properties of preferentially anisotropic single-walled carbon-nanotube films in terahertz region,” Journal of Applied Physics, vol. 95, no. 10, pp. 5736–5740, 2004.
[6]
J. Hone, M. Whitney, C. Piskoti, and A. Zettl, “Thermal conductivity of single-walled carbon nanotubes,” Physical Review B-Condensed Matter and Materials Physics, vol. 59, no. 4, pp. R2514–R2516, 1999.
[7]
C. T. White and J. W. Mintmire, “Fundamental properties of single-wall carbon nanotubes,” Journal of Physical Chemistry B, vol. 109, no. 1, pp. 52–65, 2005.
[8]
N. Sinha, J. Ma, and J. T. W. Yeow, “Carbon nanotube-based sensors,” Journal of Nanoscience and Nanotechnology, vol. 6, no. 3, pp. 573–590, 2006.
[9]
A. Star, V. Joshi, S. Skarupo, D. Thomas, and J. P. Gabriel, “Gas sensor array based on metal-decorated carbon nanotubes,” Journal of Physical Chemistry B, vol. 110, no. 42, pp. 21014–21020, 2006.
[10]
Ph. Avouris, “Molecular electronics with carbon nanotubes,” Accounts of Chemical Research, vol. 35, no. 12, pp. 1026–1034, 2002.
[11]
J. Robertson, G. Zhong, H. Telg et al., “Carbon nanotubes for interconnects in VLSI integrated circuits,” Physica Status Solidi (B) Basic Research, vol. 245, no. 10, pp. 2303–2307, 2008.
[12]
V. Sazonova, Y. Yalsh, I. üstünel, D. Roundy, T. A. Arlas, and P. L. McEuen, “A tunable carbon nanotube electrochemical oscillator,” Nature, vol. 431, no. 7006, pp. 284–287, 2004.
[13]
N. D. Jonge, M. Allioux, M. Doytcheva et al., “Characterization of the field emission properties of individual thin carbon nanotubes,” Applied Physics Letters, vol. 85, no. 9, pp. 1607–1609, 2004.
[14]
L. Ci, J. Suhr, V. Pushparaj, X. Zhang, and P. M. Ajayan, “Continuous carbon nanotube reinforced composites,” Nano Letters, vol. 8, no. 9, pp. 2762–2766, 2008.
[15]
A. A. Bhirde, V. Patel, J. Gavard et al., “Targeted killing of cancer cells in vivo and in vitro with EGF-directed carbon nanotube-based drug delivery,” ACS Nano, vol. 3, no. 2, pp. 307–316, 2009.
[16]
H. Dai, “Carbon nanotubes: synthesis, integration, and properties,” Accounts of Chemical Research, vol. 35, no. 12, pp. 1035–1044, 2002.
[17]
X. Li, X. Tu, S. Zaric et al., “Selective synthesis combined with chemical separation of single-walled carbon nanotubes for chirality selection,” Journal of the American Chemical Society, vol. 129, no. 51, pp. 15770–15771, 2007.
[18]
S. Pisana, A. Jungen, C. Zhang et al., “Flying and crawling modes during surface-bound single wall carbon nanotube growth,” Journal of Physical Chemistry C, vol. 111, no. 46, pp. 17249–17253, 2007.
[19]
Y. Li, S. Peng, D. Mann et al., “On the origin of preferential growth of semiconducting single-walled carbon nanotubes,” Journal of Physical Chemistry B, vol. 109, no. 15, pp. 6968–6971, 2005.
[20]
S. Ghosh, S. M. Bachilo, and R. B. Weisman, “Advanced sorting of single-walled carbon nanotubes by nonlinear density-gradient ultracentrifugation,” Nature Nanotechnology, vol. 5, no. 6, pp. 443–450, 2010.
[21]
F. Hennrich, S. Lebedkin, and M. M. Kappes, “Improving separation techniques for single-walled carbon nanotubes: towards monodisperse samples,” Physica Status Solidi (B) Basic Research, vol. 245, no. 10, pp. 1951–1953, 2008.
[22]
A. V. Naumov, O. A. Kuznetsov, A. R. Harutyunyan et al., “Quantifying the semiconducting fraction in single-walled carbon nanotube samples through comparative atomic force and photoluminescence microscopies,” Nano Letters, vol. 9, no. 9, pp. 3203–3208, 2009.
[23]
V. A. Davis, A. N. G. Parra-Vasquez, M. J. Green et al., “True solutions of single-walled carbon nanotubes for assembly into macroscopic materials,” Nature Nanotechnology, vol. 4, no. 12, pp. 830–834, 2009.
[24]
P. Angelikopoulos, A. Gromov, A. Leen, O. Nerushev, H. Bock, and E. E. B. Campbell, “Dispersing individual single-wall carbon nanotubes in aqueous surfactant solutions below the cmc,” Journal of Physical Chemistry C, vol. 114, no. 1, pp. 2–9, 2010.
[25]
L. Vaisman, H. D. Wagner, and G. Marom, “The role of surfactants in dispersion of carbon nanotubes,” Advances in Colloid and Interface Science, vol. 128–130, pp. 37–46, 2006.
[26]
M. C. Hersam, “Progress towards monodisperse single-walled carbon nanotubes,” Nature Nanotechnology, vol. 3, no. 7, pp. 387–394, 2008.
[27]
J. L. Bahr, E. T. Mickelson, M. J. Bronikowski, R. E. Smalley, and J. M. Tour, “Dissolution of small diameter single-wall carbon nanotubes in organic solvents?” Chemical Communications, no. 2, pp. 193–194, 2001.
[28]
C. A. Furtado, U. J. Kim, H. R. Gutierrez, L. Pan, E. C. Dickey, and P. C. Eklund, “Debundling and dissolution of single-walled carbon nanotubes in amide solvents,” Journal of the American Chemical Society, vol. 126, no. 19, pp. 6095–6105, 2004.
[29]
S. D. Bergin, V. Nicolosi, P. V. Streich et al., “Towards solutions of single-walled carbon nanotubes in common solvents,” Advanced Materials, vol. 20, no. 10, pp. 1876–1881, 2008.
[30]
Y. Hernandez, V. Nicolosi, M. Lotya et al., “High-yield production of graphene by liquid-phase exfoliation of graphite,” Nature Nanotechnology, vol. 3, no. 9, pp. 563–568, 2008.
[31]
S. D. Bergin, Z. Sun, P. Streich, J. Hamilton, and J. N. Coleman, “New solvents for nanotubes: approaching the dispersibility of surfactants,” Journal of Physical Chemistry C, vol. 114, no. 1, pp. 231–237, 2010.
[32]
S. Giordani, S. D. Bergin, V. Nicolosi et al., “Debundling of single-walled nanotubes by dilution: observation of large populations of individual nanotubes in amide solvent dispersions,” Journal of Physical Chemistry B, vol. 110, no. 32, pp. 15708–15718, 2006.
[33]
Q. Cheng, S. Debnath, L. O'Neill, T. G. Hedderman, E. Gregan, and H. J. Byrne, “Systematic study of the dispersion of swnts in organic solvents,” Journal of Physical Chemistry C, vol. 114, no. 11, pp. 4857–4863, 2010.
[34]
B. J. Landi, H. J. Ruf, J. J. Worman, and R. P. Raffaelle, “Effects of alkyl amide solvents on the dispersion of single-wall carbon nanotubes,” Journal of Physical Chemistry B, vol. 108, no. 44, pp. 17089–17095, 2004.
[35]
M. E. Itkis, D. E. Perea, R. Jung, S. Niyogi, and R. C. Haddon, “Comparison of analytical techniques for purity evaluation of single-walled carbon nanotubes,” Journal of the American Chemical Society, vol. 127, no. 10, pp. 3439–3448, 2005.
[36]
S. Ohmori, T. Saito, M. Tange et al., “Fundamental importance of background analysis in precise characterization of single-walled carbon nanotubes by optical absorption spectroscopy,” Journal of Physical Chemistry C, vol. 114, no. 22, pp. 10077–10081, 2010.
[37]
A. V. Naumov, S. Ghosh, D. A. Tsyboulski, S. M. Bachilo, and R. B. Weisman, “Analyzing absorption backgrounds in single-walled carbon nanotube spectra,” ACS Nano, vol. 5, no. 3, pp. 1639–1648, 2011.
[38]
P. Vichchulada, M. A. Cauble, E. A. Abdi, E. I. Obi, Q. Zhang, and M. D. Lay, “Sonication power for length control of single-walled carbon nanotubes in aqueous suspensions used for 2-dimensional network formation,” Journal of Physical Chemistry C, vol. 114, no. 29, pp. 12490–12495, 2010.
[39]
Q. Cheng, S. Debnath, E. Gregan, and H. J. Byrne, “Ultrasound-assisted SWNTs dispersion: effects of sonication parameters and solvent properties,” Journal of Physical Chemistry C, vol. 114, no. 19, pp. 8821–8827, 2010.
[40]
A. J. Blanch, C. E. Lenehan, and J. S. Quinton, “Optimizing surfactant concentrations for dispersion of single-walled carbon nanotubes in aqueous solution,” Journal of Physical Chemistry B, vol. 114, no. 30, pp. 9805–9811, 2010.
[41]
J. Shim, P. Vichchulada, Q. Zhang, and M. D. Lay, “Spectroscopic and scanning probe studies of a nondestructive purification method for SWNT suspensions,” Journal of Physical Chemistry C, vol. 114, no. 1, pp. 652–657, 2010.
[42]
A. Vijayaraghavan, S. Blatt, D. Weissenberger et al., “Ultra-large-scale directed assembly of single-walled carbon nanotube devices,” Nano Letters, vol. 7, no. 6, pp. 1556–1560, 2007.
[43]
H. Pathangi, G. Groeseneken, and A. Witvrouw, “Directed assembly of horizontal suspended carbon nanotubes for NEMS applications,” Microelectronic Engineering, 2011.
[44]
H. Pathangi, V. Cherman, A. Khaled, B. Soree, G. Groeseneken, and A. Witvrouw, “Towards CMOS-compatible single-walled carbon nanotube resonators,” Microelectronic Engineering, vol. 107, pp. 219–222, 2013.
[45]
A. R. Hall, M. R. Falvo, R. Superfine, and S. Washburn, “A self-sensing nanomechanical resonator built on a single-walled carbon nanotube,” Nano Letters, vol. 8, no. 11, pp. 3746–3749, 2008.