Single-wall fullerene nanotubes were converted from nearly endless, highly tangled ropes into short, open-ended pipes that behave as individual macromolecules. Raw nanotube material was purified in large batches, and the ropes were cut into 100- to 300-nanometer lengths. The resulting pieces formed a stable colloidal suspension in water with the help of surfactants. These suspensions permit a variety of manipulations, such as sorting by length, derivatization, and tethering to gold surfaces.
We describe, in detail, a readily scalable purification process capable of handling single-wall carbon nanotube (SWNT) material in large batches. Characterization of the resulting material by SEM, TEM, XRD, Raman scattering, and TGA shows it to be highly pure. Resistivity measurements on freestanding mats of the purified tubes are also reported. We also report progress in scaling up SWNT production by the dual pulsed laser vaporization process. These successes enable the production of gram per day quantities of highly pure SWNT, which should greatly facilitate investigation of material properties intrinsic to the nanotubes.
Strong interfacial bonding and homogenous dispersion have been found to be necessary conditions to take full advantage of the extraordinary properties of nanotubes for reinforcement of composites. We have developed a fully integrated nanotube composite material through the use of functionalized single‐walled carbon nanotubes (SWNTs). The functionalization was performed via the reaction of terminal diamines with alkylcarboxyl groups attached to the SWNTs in the course of a dicarboxylic acid acyl peroxide treatment. Nanotube‐reinforced epoxy polymer composites were prepared by dissolving the functionalized SWNTs in organic solvent followed by mixing with epoxy resin and curing agent. In this hybrid material system, nanotubes are covalently integrated into the epoxy matrix and become part of the crosslinked structure rather than just a separate component. Results demonstrated dramatic enhancement in the mechanical properties of an epoxy polymer material, for example, 30–70 % increase in ultimate strength and modulus with the addition of only small quantities (1–4 wt.‐%) of functionalized SWNTs. The nanotube‐reinforced epoxy composites also exhibited an increased strain to failure, which suggests higher toughness.
We found that multiwalled carbon nanotubes (MWNTs) can be opened longitudinally by intercalation of lithium and ammonia followed by exfoliation. Intercalation of open-ended tubes and exfoliation with acid treatment and abrupt heating provided the best results. The resulting material consists of: (i) multilayered flat graphitic structures (nanoribbons), (ii) partially open MWNTs, and (iii) graphene flakes. We called the completely unwrapped nanotubes ex-MWNTs, and their large number of edge atoms makes them attractive for many applications.
Vapor-grown carbon fibers (VGCFs), a practical model nanofiber for single-walled carbon nanotubes, were combined with an acrylonitrile-butadiene-styrene (ABS) copolymer to create a composite material for use with fused deposition modeling (FDM). Continuous filament feedstock materials were extruded from Banbury mixed composites with a maximum composition of 10 wt % nanofibers. Issues of dispersion, porosity, and fiber alignment were studied. SEM images indicated that the VGCFs were well dispersed and evenly distributed in the matrix and that no porosity existed in the composite material following FDM processing. VGCFs aligned both in the filament feedstock and in the FDM traces suggested that nanofibers, in general, can be aligned through extrusion/shear processing. The feedstock materials were processed into test specimens for mechanical property comparisons with unfilled ABS. The VGCF-filled ABS swelled less than did the plain ABS at similar processing conditions due to the increased stiffness. The tensile strength and modulus of the VGCF-filled ABS increased an average of 39 and 60%, respectively, over the unfilled ABS. Storage modulus measurements from dynamic mechanical analysis indicated that the stiffness increased 68%. The fracture behavior of the composite material indicated that the VGCFs act as restrictions to the chain mobility of the polymer.
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