Processing, spinning, and fabrication of continuous fibers of single-walled carbon nanotubes
Booker, Richard DeLane
Doctor of Philosophy
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 processing into macroscopic articles such as fibers or films. Fibers spun from SWNT/superacid dispersions indicate that the morphology of the starting SWNT material influences the final morphology of the as-spun fiber. 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 fiber 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 fibers spun from the coagulated material) show that this disentanglement 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 important as a pre-processing step for fiber spinning of neat SWNT fibers, it is also useful for neat SWNT films, SWNT/polymer composites, and surfactant- or polymer-stabilized SWNT dispersions. Macroscopic neat SWNT fibers were successfully produced and characterized. Studies on coagulated fiber morphology suggest that slow acid removal is crucial to minimizing voids. Better SWNT coalescence and alignment were obtained by using appropriate coagulant and dope concentration. SWNTs were disentangled and dissolved at high concentrations (8 - 10 wt%) in 102% sulfuric acid. Fibers were subsequently extruded by dry-jet wet spinning into ice water and polyvinyl alcohol (PVA) / ice water. Drawing the fiber continuously while spinning further aligned the SWNTs within the fiber. The use of PVA (< 1%) in the coagulant slowed acid removal allowing better SWNT coalescence without damaging the SWNT electrical properties. The resulting combination of pre-processing and fiber drawing shows a threefold improvement in fiber tensile strength.
Organic chemistry; Polymer chemistry; Engineering; Materials science