Lead-tin solder has been widely used as interconnection material in electronics packaging for a long time. In response to environmental legislation, the lead-tin alloys are being replaced with lead-free alloys and electrically conductive adhesives in consumer electronics. Lead-free solder usually require higher reflow temperatures than the traditional lead-tin alloys, which can cause die crack and board warpage in assembly process, thereby impacting the assembly yields. The high tin content in lead-free solder forms tin whiskers, which has the potential to cause short circuits failure. Conductive adhesives are an alternative to solder reflow processing, however, conductive adhesives require up to 80 wt% metal filler to ensure electrical and thermal conductivity. The high loading content degrades the mechanical properties of the polymer matrix and reduces the reliability and assembly yields when compared to soldered assemblies. Carbon nanotubes (CNTs) have ultra high aspect ratio as well as many novel properties. The high aspect ratio of CNTs makes them easy to form percolation at low loading and together with other novel properties make it possible to provide electrical and thermal conductivity for the polymer matrix while maintaining or even reinforcing the mechanical properties. Replacing the metal particles with CNTs in conductive adhesive compositions has the potential benefits of being lead free, low process temperature, corrosion resistant, electrically/thermally conductive, high mechanical strength and lightweight. In this paper, multiwall nanotubes (MWNTs) with different dimensions are mixed with epoxy. The relationships among MWNTs dimension, volume resistivity and thermal conductivity of the composite are characterized. Different loadings of CNTs, additives and mixing methods were used to achieve satisfying electrical and mechanical properties and pot life. Different assembly technologies such as pressure dispensing, screen and stencil printing are used to simplify the processing method and raise the assembly yields. Contact resistance, volume resistivity, high frequency performance, thermal conductivity and mechanical properties were measured and compared with metal filled conductive adhesive and traditional solder paste.

Research in carbon nanotubes (CNTs) has become a very active field in the past decades, with much interest in their electronic and mechanical properties. However, the thermal properties of CNTs are still not well understood, in particular the process of annealing; i.e. purification of samples by desorption of internal and external impurities. Understanding the response of carbon nanotubes to high temperatures is critical for proper characterization of CNTs and CNT-based materials; especially because purportedly non-destructive characterization techniques such as Raman spectroscopy can induce high temperatures through laser heating. This thesis delineates an experiment aimed at elucidating the annealing and destruction process of carbon nanotubes. The experiment consists of heat treatments of single-walled nanotubes (SWNTs), monitoring nanotube abundance and purity by Raman spectroscopy. The samples are HiPCO-produced SWNTs of very high purity, separated in open and closed (end-capped) tubes. They are wetted with H2O in order to fill the open tubes, but are otherwise kept in their raw (as-produced) form of flakes of bundled tubes. This means that they have a low thermal conductivity as compared to dispersed CNTs, making them sensitive to overheating. The samples are heated in both air and argon environments in order to study the effect of oxidation. It is found that all tubes exhibit some annealing after heat treatment at temperatures as low as 100 °C. Temperatures higher than that are sufficient to degrade the samples in the case of closed tubes, which are found to be more thermally sensitive than open tubes, especially in air environments as oxidation is found to be a major component of the destructive mechanisms of CNTs. With higher temperature heat treatments at 500 °C, some of the open tubes exhibit a further step of annealing. This correlates with tube diameter, thus indicating that this annealing step can be associated with the desorption water from the CNTs' interior. A transition is found after heat treatment at 600 °C, although the new phase is not conclusively established, with evidence pointing to either charge transfer (by way of intercalation of dopant atoms in CNTs) or graphitization.

Extrapolating the properties of individual carbon nanotubes (CNTs) into macro-scale CNT materials using a continuous and cost effective process offers enormous potential for a variety of applications. The floating catalyst chemical vapour deposition (FCCVD) method discussed in this dissertation bridges the gap between generating nano- and macro-scale CNT material and has already been adopted by industry for exploitation. A deep understanding of the phenomena that occur within the FCCVD reactor and how to control the formation of the catalyst nanoparticles is, therefore, essential to producing a desired CNT product and successfully scaling up the FCCVD process. This dissertation connects information on the decomposition of reactants, axial catalyst nanoparticle dynamics and the morphology of the resultant CNTs and demonstrates how these factors are strongly related to the temperature and chemical availability of reactants within the reactor. For the first time, in-situ measurements of catalyst particle size distributions paired with reactant decomposition profiles and detailed axial SEM studies of formed CNT materials revealed specific temperature domains that have important implications for scaling up the FCCVD process. A novel observation was that the evaporation and re-condensation of catalyst nanoparticles results in the formation, disappearance and reformation of the nanoparticles along the reactor axis. The combined influences of pyrolytic carbon species and catalytic nanoparticles are shown to influence CNT aerogel formation. This work also examines the source of carbon in the formed CNTs and the location of aerogel formation. Axial measurements using isotopically-labelled methane (C13H4) demonstrate that carbon within all CNTs is primarily derived from CH4 rather than some of the early-forming CNTs being predominantly supplied with carbon from decomposed catalytic precursor components. Quantification of CNT production along the axis of the reactor dispels the notion that injection parameters influence CNT formation and shows that bulk CNT formation occurs near the reactor exit regardless of the carbon source (CH4, toluene or ethanol). By supplying carbon to different reactor locations, it was discovered that CNT aerogel formation will occur even when carbon is delivered near the exit of the reactor provided the carbon source reaches a temperature sufficient to induce pyrolysis (>1000°C). Furthermore, experimental studies that identify a new role of sulphur (S) in the CNT formation process are discussed in this work. Analogous to effects observed in other aerosol systems containing S, in the FCCVD reactor, S lowers the nucleation barrier of the catalyst nanoparticles and enhances not only CNT growth but catalyst particle formation itself. The new concept of critical catalyst mass concentration for CNT aerogel formation was identified by implementing the novel approach of completely decoupling catalyst particle formation from CNT aerogel production. Rather than aerogel formation being dependent on a critical particle number concentration and ideal sized catalyst nanoparticles at the entrance of the reaction furnace, it was identified that the important metric is instead a minimum critical catalyst mass concentration. Application of the principle using other catalyst precursors such as cobaltocene, with continuous CNT aerogel formation from cobalt based catalyst nanoparticles being reported for the first time, and iron-based nanoparticles from a spark generator, provides proof of the new principle’s robustness and ubiquity. In addition to the experimental studies above, theoretical studies have been carried out to understand the agglomeration occurring in a CNT aerosol. The agglomeration eventually leads to a gas phase synthesized CNT aerogel at the end of the reactor, which can be collected and spun continuously. The results of this work are not only scientifically interesting, they also provide a strong foundation for further research aimed at optimizing and controlling large-scale CNT reactors by modifying downstream dynamics.

In this research, manganese oxide based nanoparticles were synthesized by sol-gel process. Methanol, ethanol, and propanol were used as alternative solvents during sol-gel process with manganese acetate as precursor for the preparation of pristine manganese oxide. Hybrid manganese oxide modified by additions of carbon nanotubes was further prepared. The effects of different solutions and heat treatment temperatures on the morphology, physical characteristics, and electrochemical properties of the manganese oxide based materials were investigated. Particle size of pristine manganese oxide samples prepared from methanol, ethanol, and propanol were compared by SEM and TEM image analysis. Smallest particle size was observed for manganese oxide prepared from propanol, with diameters range from 16 nm to 50nm. XRD results showed that the as-prepared manganese oxide based samples treated at calcination temperature of 300ºC and above were composed of Mn2O3 as dominant phase, with Mn3O4 as minor phase. Specific capacitance of manganese oxide prepared from methanol, ethanol, and propanol at scan rate of 10 mV/s measured using two electrode systems were 88.3, 66.0, and 104.8 F/g, respectively and that for the hybrid sample was 140.5 F/g. Results from electrochemical impedance spectroscopy (EIS) also showed superior electrochemical properties of the hybrid sample over pristine manganese oxide samples. It is evident that the addition of carbon nanotubes not only improved the specific capacitance but also the overall electrochemical properties of the manganese oxide supercapacitor.

abstract: This research focuses on the benefits of using nanocomposites in aerospace structural components to prevent or delay the onset of unique composite failure modes, such as delamination. Analytical, numerical, and experimental analyses were conducted to provide a comprehensive understanding of how carbon nanotubes (CNTs) can provide additional structural integrity when they are used in specific hot spots within a structure. A multiscale approach was implemented to determine the mechanical and thermal properties of the nanocomposites, which were used in detailed finite element models (FEMs) to analyze interlaminar failures in T and Hat section stringers. The delamination that first occurs between the tow filler and the bondline between the stringer and skin was of particular interest. Both locations are considered to be hot spots in such structural components, and failures tend to initiate from these areas. In this research, nanocomposite use was investigated as an alternative to traditional methods of suppressing delamination. The stringer was analyzed under different loading conditions and assuming different structural defects. Initial damage, defined as the first drop in the load displacement curve was considered to be a useful variable to compare the different behaviors in this study and was detected via the virtual crack closure technique (VCCT) implemented in the FE analysis. Experiments were conducted to test T section skin/stringer specimens under pull-off loading, replicating those used in composite panels as stiffeners. Two types of designs were considered: one using pure epoxy to fill the tow region and another that used nanocomposite with 5 wt. % CNTs. The response variable in the tests was the initial damage. Detailed analyses were conducted using FEMs to correlate with the experimental data. The correlation between both the experiment and model was satisfactory. Finally, the effects of thermal cure and temperature variation on nanocomposite structure behavior were studied, and both variables were determined to influence the nanocomposite structure performance. / Dissertation/Thesis / Doctoral Dissertation Aerospace Engineering 2014

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The growing demand for compact and compliant mobility assistive devices has driven interest in low-profile actuating technologies. With the increasing mobility needs of an aging population, such devices could meet this growing market if they can provide low power capabilities, high strength, and compatibility with standard industrial fabrication processes. As a result, researchers have been investigating smart materials, such as carbon nanotube (CNT) and their higher-order structures, as potential components for soft actuator systems. However, reported works using this material within actuators have remained limited due to the material's prohibitive cost and fabrication complexity. Furthermore, presented actuator designs are difficult to compare due to custom fabrication procedures and inconsistent characterizations. The recent availability of commercial higher-order CNT products and the superior material consistency they provide present an opportunity to comprehensively analyze these materials in actuators without the challenges faced in previous work. This thesis addressed this opportunity by evaluating a stiffness-variable actuator design leveraging a commercially available CNT fibre. The evaluation focused on the effects on the mechanical and electrical properties in addition to its electrothermal and electromechanical responses when changing selected actuator design and operational parameters. The findings highlight the importance of optimal coating and embedded pre-stretch to achieve optimal contractile stress and contractile strain performance, while increased fibre diameter diminishes these properties. Furthermore, the usage of commercial CNT yarn ensured consistent mechanical and electrical properties during the fabrication and testing of actuator prototypes. This in-depth understanding of this actuator design's strengths, weaknesses, and the influence of selected operational and design parameters on performance establishes a foundation for future CNT-based actuator research within a repeatable framework.