We have carried out a quantitative comparison of the dispersion quality for ultracentrifuged and diluted surfactant-stabilised single walled nanotube dispersions.We have characterised these dispersions at a set concentration of ~30 µg.mL -1 by absorption and photoluminescence spectroscopy as well as by statistical atomic force microscopy. Both the ultracentrifuged and the diluted samples contained significant quantities of bundles as well as individual nanotubes. The ultracentrifuged sample contained ~ 4 times more individualised SWNTs than the diluted sample with partial concentrations of individual nanotubes of 4.8 and 1.1 µg.mL -1 respectively.
IntroductionIn recent years, a significant amount of research has been carried out in the area of dispersion and exfoliation of single walled nanotubes (SWNTs) in the liquid phase. In general, pristine nanotubes can be dispersed in a small number of special solvents(1-5) or in a wider range of solvents, but particularly water, with the aid of third phase dispersants such as polymers(6,7), surfactants(8-11) or biomolecules like . Alternatively, nanotubes can be dispersed in super-acids(21) or by covalent functionalisation (22,23).However, the most common technique is to disperse SWNTs in water with the aid of surfactants or DNA. Ultrasonication is generally used to promote exfoliation followed by vigorous ultracentrifugation (UCF) to remove most of the bundles (10,11,19,24,25). This produces a dispersion that is significantly enriched in individual nanotubes, but at the cost of typically more than 80% of the starting nanotube mass(10). While this has been a very successful method, it is also a very inefficient one, especially given the high cost of high-quality nanotubes. An alternative to ultracentrifugation is to control the population of individual nanotubes in a dispersion by controlling nanotube concentration (1,2,4,8,12,16,26,27). This relies on the observation that nanotubes tend to debundle as the concentration is lowered. This technique is less wasteful and allows the researcher greater control over the properties of the final sample, however, highly exfoliated samples often only exist at low concentrations which limits potential applications. mg.mL -1 was shown to be the minimum SDBS-concentration necessary to obtain high fractions of dispersed nanotubes(27). Purified HiPCO SWNTs (www.cnanotech.com, Lot number PO342) were dispersed in the SDBS solution at a concentration of 1 mg.mL -1 as described elsewhere (27). Briefly, the dispersion was sonicated for 5 min with a high power sonic tip (Vibra Cell CVX; 750 W, 38%, 20 kHz), followed by 1 hr in a Branson 1510 sonic bath (frequency 42 kHz, rated power output 80 W), followed by a further 5 min under the sonic tip. Ice-water cooling was used throughout to prevent heating in the sample. The dispersion was left to stand for 24 hrs to equilibrate. It should be noted that, throughout this paper, the word concentration refers to the nanotube concentration unless otherwise stated.
ACCEPTED MANUSCRIPTMild centrifugation...