Ever since the discovery of carbon nano materials like carbon nanotube (CNT) and graphene, this class of materials has gained significant attention due to their exotic properties. The principle idea of my present research project is to understand the novel improvements induced in polymer matrices with inclusion of the nanofillers. This thesis is thematically divided into three parts. In the first part we introduce principle materials that we use for preparation of composites. Methods of nanofiller preparation and different nanocomposites as previously reported in literature are discussed to formulate the basis of our study. Different dispersion techniques are discussed which facilitate uniform nanofiller distribution. A variety of experimental methods are described which were employed to investigate the structure and properties of the composites. In the second part we discuss in details polyamide-12 (PA12) composites using CNT and graphene as fillers. A marked improvement is recorded in the toughness of the films with incorporation of CNT, dispersed in PA12 using a surfactant. Electrical percolation is also achieved in the otherwise insulating matrix. With PA-12 fibers we explored the effect of fiber processing and CNT incorporation in the mechanical properties. Extensive wide angle x-ray diffraction was carried out to interpret the structural modifications brought about by CNT in the matrix. The final part of the thesis deals with a thermosetting polymer, epoxy composites. CNT, Graphene and also a mixture of the two nanofillers were used as reinforcing agents. Appreciable improvement was recorded in the mechanical properties, electrical and thermal conductivity of the composites. Detailed optical and electron microscopy was carried out to get a vivid idea of the micro-structure and dispersion. The presented work demonstrates the significant ability of carbon nanofillers to reinforce polymer matrices enhancing their mechanical, electrical and thermal properties and opening a wide horizon for a variety of applications.

Preventative immunotherapeutic treatments have been an area of great interest to combat infectious disease because of the ability to stimulate the hosts immune system which prepares the host to fight pathogenic microbes. The immunotherapeutic approach requires the use of an immune stimulating molecule that is able to boost the hosts immune response. A major problem exists that these immune stimulating molecules are often very expensive and require a large dose to be effective. To reduce the cost of using these molecules, a delivery system can be used which is able to lower the effective dose of the immune stimulant while not causing any toxic effects towards the hosts health. In this study, the immune stimulating molecules synthetic unmethylated cytidine-phosphate-guanosine oligodeoxynucleotides were attached non-covalently to multi-walled carbon nanotubes. The use of carbon nanotubes as a delivery mechanism could result in a lower effective dose able to stimulate a protective immune response in a chicken model. In this study, we first assessed which of the non-covalant linkages was ideal for linking the immune stimulant to the carbon nanotubes. This was conducted by looking at which method of linkage would allow the best cellular proliferation and transcriptional activation of selected innate immune genes. Once an appropriate linkage method had been selected, cellular uptake studies were conducted to establish that cytidine-phosphate-guanosine oligodeoxynucleotides were delivered to intracellular target receptors. After cellular uptake was demonstrated, it was important that the carbon nanotubes linked to the immune stimulant do not cause toxicity towards the host. To measure toxicity, in vitro studies were conducted to observe cell viability post treatment with carbon nanotube linked immune stimulant. Further studies were conducted on any alterations to the immune stimulants ability to activate immune cells by studying the pathway of macrophage activation. The protective ability of the molecules was then measured by the ability to protect chickens from a lethal challenge with S. typhimurium. Once the protective nature of the molecules was established, the mechanism of immune stimulation was examined by in vivo cell recruitment and in vitro cytokine production. These studies indicate that linking cytidine-phosphate-guanosine oligodeoxynucleotides to carbon nanotubes can lower the effective dose of the immune stimulant without altering the biological function of the molecule.

In this study, a novel polyimide (PI) film, consisting of multiwall carbon nanotubes (MWCNTs) dispersed in an Ionic Liquid (IL), were demonstrated to be high shielding effectiveness (SE). The film was potentially useful for screening electromagnetic interference(EMI) in an optical transceiver module. The experimental results showed MWCNT-PI composite dispersed well in IL exhibits a high far-field SE of 38 ~ 45 dB within the frequency range of 1 ~ 3 GHz. It was also demonstrated the MWCNT-PI composite prepared with IL dispersed process have higher SE and lower weight percentage of MWCNTs than those with non-IL-dispersed process. Their intermolecular forces were carefully examined in order to understand dispersion mechanisms among MWCNTs. The aggregation phenomenon of MWCNTs was known, resulting from van der Waals forces. In our study, IL was employed to disperse MWCNTs. A proposal reason was that the attractive force between cation of the IL and £k electrons of MWCNTs is greater than the van der Waals forces among MWCNTs. From conductivity measurement, percolation threshold of the IL-dispersed MWCNT-PI composite was 5.2 wt%; percolation threshold of the non-IL-dispersed MWCNT-PI composite was 11.5 wt%. Given the lower percolation threshold ,we demonstrated the successful dispersion of MWCNT by adding IL. From the results of Raman spectrometer analyses, the IL dispersion was proved to be a physical interaction. Furthermore, the IL-dispersed MWCNT-PI composite was used as package material in monopole antenna and got a near-field SE of 37dB within the frequency of 2.8 GHz. It implied that the IL-dispersed MWCNT-PI composite has an excellent EMI performance.The IL-dispersed MWCNT-PI composite is suitable for packaging low-cost and high-performance optical transceiver modules in the application of the fiber-to-the-home (FTTH) lightwave transmission systems.

This dissertation presents research on synthesis, high-power microwave post-synthetic purification and high frequency characterization of Carbon Nanotubes (CNT). First, CNTs are synthesized using a Chemical Vapor Deposition system. The impact of substrate and methane flow rate on CNT growth is studied using Scanning Electron Microscopy, Transmission Electron Microscopy and Raman microscopy. Second, the microwave irradiation effects on purified HiPCO and CoMoCat Single-Walled CNT thin films are investigated. The measured drastic THz power transmission increase (>10 times) indicates a significant metallic content reduction after the irradiation. The Raman spectra also confirm the metallic-to-semiconducting ratio of Raman-active CNTs decreases by up to 33.3%. The observed microwave-induced effects may potentially lead to a convenient scheme for CNT demetalization. Third, Multi-Walled CNT papers are characterized from 8 to 50 GHz by rectangular waveguide measurements using a vector network analyzer. A rigorous algorithm is developed to extract the samples' effective complex permittivity and permeability from the measured S-parameters. Unlike other reported work, this method does not impose the unity permeability assumption. The algorithm is verified by finite-element simulations and the uncertainties for the characterization method are analyzed. The effective medium theory is then applied to obtain the intrinsic CNT properties. Furthermore, Terahertz Time-Domain Spectroscopy is used to characterize the samples from 50 to 370 GHz. Both transmission and reflection experiments are performed to simultaneously extract the permittivity and permeability. The extracted permittivity is fitted with a Drude-Lorentz model from 8 to 370 GHz. Finally, individual CNT characterizations at microwave frequency are studied. The impacts from impedance mismatching and parasitics on measurement sensitivity are systematically studied, revealing that the parasitic effect is possibly dominant above 10 GHz. A tapered coplanar waveguide test fixture is designed using Advanced Design System (ADS) to improve the impedance mismatching and minimize the test fixture parasitics, therefore optimize the measurement sensitivity. A de-embedding procedure to obtain the CNT's intrinsic electrical properties is presented and demonstrated with ADS simulations. In addition, the test fixture fabrication process is discussed, which is an ongoing research work. At the end, the conclusions of this dissertation are drawn and possible future works are discussed.

Carbon nanotubes (CNTs) have been successfully grafted onto the surfaces of spherical silica gels via a floating-catalyst chemical vapour deposition method. Two types of silica gels were used as substrates; SG6 (6 – 8 nm pore size) and SG26 (26 – 34 nm pore size). The optimum growth conditions were found to be 760 °C growth temperature, 3 hours growth time, and 5 wt .% of ferrocene catalyst (dissolved in toluene) injected into the furnace at a rate of 0.04 ml/min. Under these conditions, CNTs coated the exterior surface of the gels with growth occurring from both the pores and from the surface. The geometry and porosity of the silica gel were also found to influence the alignment and density of the grafted CNTs, with SG6 producing the best quality hybrid particle under the above conditions (labelled SG6_3). Thermal Gravimetric Analysis showed the yield of CNTs grown under these optimum condition was 33.6 + 0.37 wt. %. As the CNTs remained strongly attached to the surface of the gel, the grafting process produced excellent dispersion of the CNTs within polymer matrices as CNT bundle formation was prevented. The inclusion of micron size silica introduced a large excluded volume within polymer matrices, with the dispersion of CNTs restricted to a region along the silica surface. This arrangement aided the formation of an electrically conductive network in a poly (vinyl) alcohol matrix, where the critical percolation threshold (pc) was calculated as 0.62 wt. % of SG6_3, equivalent to a CNT content of 0.2 wt. %.The inclusion of SG6_3 into an epoxy resin suspension did not alter the rheological behaviour of the resin up to the highest loading employed (5 wt. %, ≈1.65 wt. % of CNTs). Within the linear viscoelastic region the viscoelastic moduli of the neat resin remained within the same magnitude, whilst the addition of 1.65 wt. % of commercially available CNTs into the same resin increased the storage and loss moduli by up to seven and three orders of magnitude, respectively. The complex viscosity of the suspension remained unchanged regardless of the amount of SG6_3 added; whereas an increase in viscosity of up to five orders of magnitude resulted from the addition of 1.65 wt. % non – grafted CNTs.Grafting of CNTs onto the surface of micron size spherical silica gel has been shown to provide a means of incorporating CNTs into a polymer without increasing viscosity. In addition, the SG6_3 also formed an electrically-conductive percolated network in an epoxy resin composite at low levels of addition, with pc = 0.16 wt. % of CNTs (i.e. 0.5 wt. % SG6_3).

Carbon nanotubes (CNTs) possess exceptional mechanical, thermal and electrical properties along their main axis, superior to those of most materials. These can be exploited on a macroscopic scale by assembling the CNTs into a fibre with the nanotubes preferentially oriented parallel to each other and to the fibre axis. CNT fibres can be produced continuously, directly from the gas phase during CNT synthesis by chemical vapour deposition (CVD), and spun at rates of up to 70 m/min. Their combination of outstanding mechanical, electrical and thermal properties and low density (1 g/cm3) makes CNT fibres a potential candidate for high-performance applications. The fibre specific strength and stiffness are typically 1 GPa/SG and 50 GPa/SG, respectively; however, at small gauge lengths (> 2mm) they also show values of 6-9 GPa/SG strength and 180-390 GPa/SG stiffness. The electrical conductivity of the CNT fibres is approximately 8 x 10 5 S/m and their thermal conductivity of the order of 50 W/mK. These properties derive from the long length, high alignment and efficient packing of the nanotubes in the fibre. Further improvements to the fibre structure and properties at long gauge lengths are possible through removal of impurities from the fibre by annealing.

Electrochemical Supercapacitors (ES), also known as Supercapacitor or Ultracapacitor, has been regarded as an advanced electrical energy storage device for decades. Fabrication of advanced electrode materials is of critical importance for advanced ES. Among various materials used for ES electrode, polypyrrole (PPy) is found to be a promising material due to high specific capacitance, good electrical conductivity, low cost and ease of processing. The use of advanced anionic dopants and addition of multiwall carbon nanotube (MWCNT) have been proved an .effective approach towards advanced PPy based ES with improved electrochemical behaviors. In this research, chemical polymerization of PPy powders and PPy/MWCNT composite materials have been successfully accomplished in presence of advanced anionic dopants, including chromotrope families, amaranth, pyrocatechol violet, eriochrome cyanine R and acid fuchsin. The influence of polyaromatic dopants with different molecular size, charges and charge to mass ratios on the microstructure and electrochemical characteristics has been discussed. PPy coated MWCNT with uniform microstructures was successfully achieved in simple chemical methods. The results showed PPy powders with enhanced microstructures and electrochemical behaviors can be obtained by using such advanced anionic dopants. Multi-charged polyaromatic dopants with larger molecular size benefitted PPy powders with smaller particle size, improved specific capacitance, and enhanced cycling stability, at high electrode mass loadings. Moreover, advanced aromatic dispersant and chemical synthesis was proved a simple and effective method for fabrication of PPy/MWCNT composite materials at different PPy/MWCNT mass ratio, among which the powder with PPy/MWCNT mass ratio of 7:3 showed optimum electrochemical performance. Last but not the least, the use of advanced high porosity current collector (Ni foam) allowed high electrode mass loading and good electric conductivity. As a result, advanced PPy/MWCNT composite materials which allows improved electrochemical behaviors, especially at high mass loading, are promising electrode materials for ES. / Thesis / Master of Applied Science (MASc)

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