Search

Single-walled carbon nanotubes (SWNTs) show great promise for use in a wide range of applications. One of the most promising avenues for attaining these applications is the dispersion of SWNTs at high concentrations in superacids, and their processing into macroscopic articles such as fibres or films. Fibres spun from SWNT/superacid dispersions indicate that the morphology of the starting SWNT material is reflected in the final morphology of the as-spun fibre. Here, we describe a method (termed disentanglement) of dispersing SWNTs in superacids and treating them using a high-shear, rotor/stator homogenizer, followed by coagulation to recover the solid SWNT material for use in fibre spinning. Several lines of experimental evidence (rheology and optical microscopy of the SWNTs in solution, scanning electron microscopy (SEM) of the coagulated material, and SEM of fibres spun from the coagulated material) show that this treatment radically improves the degree of alignment in the SWNTs' morphology, which in turn improves the dispersibility and processability. Raman microscopy and thermogravimetric analysis (TGA) before and after homogenization show that the treatment does not damage the SWNTs. Although this technique is particularly useful as a pre-processing step for fibre spinning of neat SWNT fibres, it is also useful for neat SWNT films, SWNT/polymer composites, and surfactant- or polymer-stabilized SWNT dispersions.

Well-aligned macroscopic fibers composed solely of single-walled carbon nanotubes (SWNTs) were produced by conventional spinning. Fuming sulfuric acid charges SWNTs and promotes their ordering into an aligned phase of individual mobile SWNTs surrounded by acid anions. This ordered dispersion was extruded via solution spinning into continuous lengths of macroscopic neat SWNT fibers. Such fibers possess interesting structural composition and physical properties.

Translating the unique characteristics of individual single-walled carbon nanotubes into macroscopic materials such as fibres and sheets has been hindered by ineffective assembly. Fluid-phase assembly is particularly attractive, but the ability to dissolve nanotubes in solvents has eluded researchers for over a decade. Here, we show that single-walled nanotubes form true thermodynamic solutions in superacids, and report the full phase diagram, allowing the rational design of fluid-phase assembly processes. Single-walled nanotubes dissolve spontaneously in chlorosulphonic acid at weight concentrations of up to 0.5 wt%, 1,000 times higher than previously reported in other acids. At higher concentrations, they form liquid-crystal phases that can be readily processed into fibres and sheets of controlled morphology. These results lay the foundation for bottom-up assembly of nanotubes and nanorods into functional materials.

Single-walled carbon nanotube (SWCNT) fibers were engineered to become a scaffold for the storage of hydrogen. Carbon nanotube fibers were swollen in oleum (fuming sulfuric acid), and organic spacer groups were covalently linked between the nanotubes using diazonium functionalization chemistry to provide 3-dimensional (3-D) frameworks for the adsorption of hydrogen molecules. These 3-D nanoengineered fibers physisorb twice as much hydrogen per unit surface area as do typical macroporous carbon materials. These fiber-based systems can have high density, and combined with the outstanding thermal conductivity of carbon nanotubes, this points a way toward solving the volumetric and heat-transfer constraints that limit some other hydrogen-storage supports.

Soluble, ultra-short (length < 60 nm), carboxylated, single-walled carbon nanotubes (SWNTs) have been prepared by a scalable process. This process, predicated on oleum's (100% H2SO4 with excess SO3) ability to intercalate between individual SWNTs inside SWNT ropes, is a procedure that simultaneously cuts and functionalizes SWNTs using a mixture of sulfuric and nitric acids. The solubility of these ultra-short SWNTs (US-SWNTs) in organic solvents, superacid and water is about 2 wt %. The availability of soluble US-SWNTs could open opportunities for forming high performance composites, blends, and copolymers without inhibiting their processibility.

Electron spin resonance investigations on the angular dependence of carbon nanotubes are reported. It is proved that the resonance line is a convolution of three lines one due to electron delocalized over carbon nanotubes, the second assigned either to amorphous carbon or to conducting electrons in interaction with metallic impurities, and the last one originating from catalyst residues.