This study focuses on the processing, structure, and properties of gel spun polyacrylonitrile (PAN) and polyacrylonitrile/carbon nanotube (PAN/CNT) carbon fibers. Gel spun PAN based carbon fibers are manufactured beginning with a study of PAN dissolution in an organic solvent (dimethylformamide, DMF). Homogeneity of the PAN/DMF solution is determined through dynamic shear rheology, and the slope of the Han Plot (log G’ vs log G’’). Solutions were then extruded into gel spun fibers using a 100 filament fiber spinning apparatus in a class 1000 cleanroom. Fibers were then subjected to fiber drawing, stabilization, and carbonization, to convert the PAN precursor fiber into carbon fiber. Carbon fiber tensile strength was shown to scale with the homogeneity of the PAN/DMF solution, as determined by the slope of the log G’ vs log G’’ plot. After the development of the understanding between the homogeneity of the PAN/DMF solutions on the gel spun PAN based carbon fiber tensile properties, the effect of altering the fiber spinning processing conditions on the gel spun PAN based carbon fiber structure and properties is pursued. Cross-sectional shape of the gel spun PAN precursor fiber, characterized with a stereomicroscope, was found to become more circular in cross-section as the gelation bath temperature was increased, the amount of solvent in the gelation bath was increased, and when the solvent was switched from DMF to dimethylacetamide (DMAc). Gel spun fibers were then subjected to fiber drawing, stabilization, and carbonization to manufacture the carbon fiber. Carbon fibers were characterized to determine single filament tensile properties and fiber structure using wide-angle x-ray diffraction (WAXD) and high resolution transmission electron microscopy (HRTEM). It was found that the carbon fiber tensile properties decreased as the carbon fiber circularity increased, as a result of the differences in microstructure of the carbon fiber that result from differences in fiber spinning conditions. In the second half of this study, the addition of CNT into the PAN precursor and carbon fiber is investigated. CNT addition occurs during the solution processing phase, prior to gel spinning. As a first study, Raman spectroscopy is employed to investigate the bundling behavior of the CNT after gel spinning and drawing of the PAN/CNT fibers. By monitoring the peak intensity of the (12,1) chirality in the as-received CNT powder, and in differently processed PAN/CNT fibers, the quality of CNT dispersion can be quickly monitored. PAN/CNT fibers were then subject to single filament straining, with Raman spectra collected as a function of PAN/CNT filament strain. As a result of the PAN/CNT strain, stress induced G’ Raman band shifts were observed in the CNT, indicating successful stress transfer from the surrounding PAN matrix to the dispersed CNT. Utilization of the shear lag theory allows for the calculation of the interfacial shear strength between the PAN and incorporated CNT, which is found to increase as the quality of CNT (higher aspect ratio, increased graphitic perfection, and reduced impurity content), quality of CNT dispersion, and fiber drawing increase. PAN/CNT fibers were then subjected to stabilization and carbonization for the manufacture of gel spun PAN/CNT based carbon fibers. These fibers were then characterized to investigate the effect of CNT incorporation on the structure and properties of the carbonized fibers. The gel spun PAN/CNT based carbon fibers were compared to commercially produced T300 (Toray) and IM7 (Hexcel) carbon fibers, and gel spun PAN based carbon fiber. Fiber structure was determined from WAXD and HRTEM. Carbon fibers properties investigated include tensile properties, and electrical and thermal conductivity. PAN/CNT based carbon fibers exhibited a 103% increase in room temperature thermal conductivity as compared to commercially available IM7, and a 24% increase in electrical conductivity as compared to IM7. These studies provide a further understanding of the processing, structure, property relationships in PAN and PAN/CNT based carbon fibers, beginning at the solution processing phase. Through the manufacture of more homogeneous PAN/DMF solutions and investigations of the fiber spinning process, gel spun PAN based carbon fibers with a tensile strength and modulus of 5.8 GPa and 375 GPa, respectively, were successfully manufactured in a continuous carbonization facility. Gel spun PAN/CNT based carbon fibers exhibit room temperature electrical and thermal conductivities as high as 74.2 kS/m and 33.5 W/m-K.

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Multiwall carbon nanotubes filled with continuous single-crystals of the ferromagnetic phase -Fe were produced with two new synthesis methods: the boundary layer chemical vapour synthesis and the perturbed vapour chemical vapour deposition. In the first method, the nanotubes nucleate and grow radially from a central agglomeration of homogeneously nucleated spherical particles in a randomly fluctuating vapour created in the viscous boundary layer between a rough surface and a laminar pyrolyzed-ferrocene/Ar vapour flow. In the second method, the nanotubes nucleate and form in a flower-like arrangement departing from homogeneously nucleated particles. These particles are produced by the creation of a local perturbation in a vapour with a high density of Fe and C species obtained from the pyrolysis of ferrocene in a laminar Ar flow. Electron microscopy investigations revealed that the continuous single crystals obtained with both methods exhibit diameters much lower than the critical diameter for a single magnetic domain of -Fe (~ 66 nm). In the radial structures, the single-crystal diameter is in the range of ~ 17-37 nm, while in the flower-like structures the single crystals show mainly a diameter of ~ 30 nm and ~ 55 nm. The average single crystals length is 7-8 m in the case of the radial structures and 19-21 m in the case of the flower-like structures. DC magnetization measurements at 5 K show different magnetic behaviours. The flower-like structures present a very high saturation magnetization of 189.5 emu/g and a high coercivity of 580 Oe. The radial structures exhibit an exchange-coupled ferromagnetic/antiferromagnetic system despite only 2% of -Fe is present inside the nanotubes. The radial structures obtained at flow-rates of 3.5 ccm and 20 ccm, show saturation-magnetizations of 31emu/g and 13 emu/g, and coercivities of 790 Oe and 843 Oe respectively.

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Carbon based materials such as CNTs and graphene have been widely studied over the last few years. The outstanding electrical and mechanical properties of these materials attracted researchers to find ways to grow and use them in nano-devices. Among the different techniques, PECVD is a relatively simple and low temperature process. It facilitates the growth of CNTs and graphene on particular sites of the substrate. The objective of this research project was to study the growth of CNTs and graphene using PECVD system and to employ them in renewable energy devices. Excimer laser processed materials were also the focus for flexible material for fuel cells and other applications to show the way to a one step manufacturing process that lends itself to large area and low cost processing using standard tools.In the growth of CNTs, the roll of a buffer layer and catalyst materials were studied in depth. Different metals were tested for best results in optimising nanotube growth for the selected applications. The role of the buffer layer in the formation of nanoparticles and their surface adhesion was studied. Different materials were used as a catalyst and analysed for best performance in the PECVD system. Growth parameters such as temperature, pressure, gas flow rate and plasma power were studied during the growth of CNTs in the PECVD system. The growth of graphene has been conducted in two ways: firstly, by the traditional mechanical exfoliation technique (with the help of Manchester University) and second by PECVD techniques.Polymer materials are promising flexible substrates for electronic and energy devices. An excimer laser was used to transform thin metallic films into nanoparticles which could play the role of the catalyst in proton exchange membrane fuel cells. In this study experiments have been conducted into a single step process to convert the poly ethylene naphthalate (PEN) surface to a robust mesoporous carbon material that conducts electrons, whilst depositing the catalyst. Such a technique has been developed for the first time in this work. Laser modification here produced a conical carbon structure and dense arrays of well defined catalysts.A prototype fuel cell was designed and crafted to employ the laser processed PEN as a proton exchange membrane. Some experiments were conducted regarding the transport of protons through laser processed PEN and the conventionally used fuel cell electrolyte, Nafion. It has been observed that the hydrophilic property of Nafion allowed proton transport across this material. It was also observed that PEN is not a good membrane for protonic transport. This material does not have free sites for vehicle transport. The catalytic activity of laser ablated Ni nanoparticles on PEN substrate was studied in temperature programme reaction (TPR) and it was observed that the metallic nanoparticles had some activity at higher temperature. Both Ni and Pt nanoparticles were tested as catalysts on the standard Nafion electrolyte. It was observed that Pt is active for the hydrogen combustion reaction and Ni has less activity for this purpose.It was not expected in this work that efficient hydrogen transport through the polymer would occur, but that future modification of the internal chemistry of PEN can be developed.

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