Magister Scientiae - MSc (Chemistry) / Drinking water with high concentrations of inorganic and organic contaminants can cause adverse health defects. Specifically methyl orange dye is an organic water contaminant that has been known (along with others like methyl blue etc.) to have an increase in our water systems over the past few years due to increasing demand in industrial processes. It is therefore of utmost importance to remediate organic contaminants and ultimately enable prevention. The contaminants can be removed by photocatalysis. Anatase TiO2 is known for its photocatalytic degradation of environmental pollutants and photoelectro-chemical conversion of solar energy. However its application is limited since it is a wide band gap semiconductor, (Eg = 3.2 eV). The following study deals with the enhancement of the photocatalytic properties of TiO2 for remediation of organic water contaminants.

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Due to their unique properties, carbon fiber reinforced polymers (CFRP) are becoming ever more prevalent in today's society. Unfortunately, CFRP suffer from a wide range of failure modes and structural health monitoring methods are currently insufficient to predict these failures. It is apparent that self-sensing structural health monitoring could be advantageous to protect consumers from catastrophic failure in CFRP structures. Previous research has shown that embedded nickel nanostrand nanocomposites can be used to instantaneously measure strain in carbon fiber composites, but these methods have been severely limited and can induce high stress concentrations that compromise the structural integrity of the carbon fiber structure. In this research the strain sensor material and the connective circuitry to the sensor are analyzed to improve the practicality of in situ strain sensing of carbon fiber structures. It has been found that the use of nickel nanostrands embedded directly onto carbon fiber as a strain sensor material has no advantages over a carbon fiber strain sensor alone. Additionally, it has been shown that the circuitry to the strain sensor plays a critical role in obtaining a strong, consistent piezoresistive signal that can be related to strain. The use of nickel coated carbon fiber in the circuitry has been evaluated and shown to reduce the noise in a piezoresistive signal while allowing for remote strain sensing from greater distances away from the strain location. The piezoresistive strain sensing utilized in the tested sensor designs relies on electrons tunneling through an insulting barrier between two conductors. This phenomenon is known as quantum tunneling. Two factors - tunneling barrier height and gap distance - affect the probability of quantum tunneling occurring. Thus, to accurately model and predict the piezoresistivity of nanocomposites these two parameters must be known. Through the use of dielectric spectroscopy the gap distance can be determined. Using nanoindenting, the barrier height for various polymers was also determined. The measured values can be used, in future work, to improve the modeling of nickel nanostrand nanocomposite.

UV-LIGA is a microfabrication process realzed by material deposition through microfabricated molds. UV photolithography is conducted to pattern precise thick micro molds using UV light sensitive materials, mostly SU-8, and electroforming is performed to fabricate micro metallic structures defined by the micro molds. Therefore, UV-LIGA is a bottom-up in situ material-addition process. UV-LIGA has received broad attention recently than LIGA – a micro molding fabrication process using X-ray to pattern the micro molds. LIGA is an expansive and is limited in access. In comparing to LIGA, the UV-LIGA is a cost effective process, and is widely accessible and safe. Therefore, it has been extensively used for the fabrication of metallic micro-electro-mechanical-systems (MEMS). The motivation of this research was to study micro mechanical systems fabricated with nano-structured metallic materials via UV-LIGA process. Various micro mechanical systems with high-aspect-ratio and thick metallic structures have been developed and are presented in this desertation. A novel micro mechanical valve has been developed with nano-structured nickel realized with UV-LIGA fabrication technique. Robust compact valves are crucial for space applications where payload and rubstaness are critically concerned. Two types of large flow rate robust passive micro check valve arrays have been designed, fabricated and tested for robust hydraulic actuators. The first such micro valve developed employs nanostructured nickel as the valve flap and single-crystal silicon as the substrates to house inlet and outlet channels. The Nano-structured nickel valve flap was fabricated using the UV-LIGA process developed and the microchannels were fabricated by deep reactive etching (DRIE) method. The valves were designed to operate under a high pressure (>10MPa), able to operate at high frequencies (>10kHz) in cooperating with the PZT actuator to produce large flow rates (>10 cc/s). The fabricated microvalves weigh 0.2 gram, after packing with a novel designated valve stopper. The tested results showed that the micro valve was able to operate at up to 14kHz. This is a great difference in comparison to traditional mechanical valves whose operations are limited to 500 Hz or less. The advantages of micro machined valves attribute to the scaling laws. The second type of micro mechanical valves developed is a in situ assembled solid metallic (nickel) valves. Both the valve substrates for inlet and outlet channels and the valve flap, as well as the valve stopper were made by nickel through a UV-LIGA fabrication process developed. Continuous multiple micro molds fabrication and molding processes were performed. Final micro mechanical valves were received after removing the micro molds used to define the strutures. There is no any additional machining process, such as cutting or packaging. The alignment for laminated fabrication was realized under microscope, therefore it is a highly precise in situ fabrication process. Testing results show the valve has a forward flow rate of19 cc/s under a pressure difference of 90 psi. The backward flow rate of 0.023 cc/s, which is negligible (0.13%). Nano-structured nickel has also been used to develop laminated (sandwiched) micro cryogenic heater exchanger with the UV-LIGA process. Even though nickel is apparently not a good thermal conductor at room temperature, it is a good conductor at cryogentic temerpature since its thermal conductivity increases to 1250 W/k·m at 77K. Micro patterned SU-8 molds and electroformed nickel have been developed to realize the sandwiched heat exchanger. The SU-8 mold (200mm x 200mm x50mm) array was successfully removed after completing the nickel electroforming. The second layer of patterned SU-8 layer (200mm x 200mm x50mm, as a thermal insulating layer) was patterned and aligned on the top of the electroformed nickel structure to form the laminated (sandwiched) micro heat exchanger. The fabricated sandwiched structure can withstand cryogenic temperature (77K) without any damages (cracks or delaminations). A study on nanocomposite for micro mechanical systems using UV-LIGA compatible electroforming process has been performed. Single-walled carbon nanotubes (SWNTs) have been proven excellent mechanical properties and thermal conductive properties, such as high strength and elastic modulus, negative coefficient of thermal expansion (CTE) and a high thermal conductivity. These properties make SWNT an excellent reinforcement in nanocomposite for various applications. However, there has been a challenge of utilizing SWNTs for engineering applications due to difficulties in quality control and handling – too small (1-2nm in diameter). A novel copper/SWNT nanocomposite has been developed during this dissertational research. The goal of this research was to develop a heat spreader for high power electronics (HPE). Semiconductors for HPE, such as AlGaN/GaN high electron mobility transistors grown on SiC dies have a typical CTE about 4~6x10-6/k while most metallic heat spreaders such as copper have a CTE of more than 10x10-6/k. The SWNTs were successfully dispersed in the copper matrix to form the SWNT/Cu nano composite. The tested composite density is about 7.54 g/cm3, which indicating the SWNT volumetric fraction of 18%. SEM pictures show copper univformly coated on SWNT (worm-shaped structure). The measured CTE of the nanocomposite is 4.7 x 10-6/°C, perfectly matching that of SiC die (3.8 x 10-6/°C). The thermal conductivity derived by Wiedemann-Franz law after measuring composit's electrical conductivity, is 588 W/m-K, which is 40% better than that of pure copper. These properties are extremely important for the heat spreader/exchanger to remove the heat from HPE devices (SiC dies). Meanwhile, the matched CTE will reduce the resulted stress in the interface to prevent delaminations. Therefore, the naocomposite developed will be an excellent replacement material for the CuMo currently used in high power radar, and other HPE devices under developing. The mechanical performance and reliability of micro mechanical devices are critical for their application. In order to validate the design & simulation results, a direct (tensile) test method was developed to test the mechanical properties of the materials involved in this research, including nickel and SU-8. Micro machined specimens were fabricated and tested on a MTS Tytron Micro Force Tester with specially designed gripers. The tested fracture strength of nanostructured nickel is 900±70 MPa and of 50MPa for SU-8, resepctively which are much higher than published values.

This thesis reports the development, synthesis and characterization of a ceramic-ceramic nanocomposite system for its possible application as structural and electronic biomaterial in the biomedical industry. The study selected and synthesized alumina-aluminum titanate-titania (Al2O3-Al2TiO5-TiO2) nanoceramic composite using a simple Sol-Gel technique, which can be easily reproduced. Aluminum propoxide and titanium propoxide were used as precursor chemicals. Propanol and 2- methoxy ethanol were used as solvent and stabilizer, respectively. Thermal analyses were performed for a systematic understanding of phase evolution from the synthesized gel. X-Ray diffraction technique was used to confirm the phase evolution, phase purity, crystallite size and crystal structure(s) of the phase(s). Calcination of the powder at low temperatures (700°C) leads to formation of Al2O3-TiO2 nanocomposite and at higher temperatures into Al2O3-Al2TiO5-TiO2 nanocomposite confirmed by XRD analysis. Electron microscopic techniques were used to investigate powder morphology, crystallite size and inter-planner spacing. High Resolution Transmission Electron Microscopy images of the calcined powder showed agglomerates of powder particles with particle size in 15-20 nm range. As-synthesized powder was uniaxially pressed into cylindrical pellets and sintered at elevated temperatures (1000-1400oC) to study the sintering behavior, densification characteristics, and measurement of mechanical and electrical properties and assessment of bioactivity. Phase transformation induced by the sintering process was analyzed by X-ray powder diffraction technique. The effects of nanosize of powder particles and multi-phases on densification, and mechanical and electrical properties were investigated. Vickers hardness and biaxial flexural strength tests were used to determine mechanical properties. Bioactivity of the nanocomposite was assessed in Simulated Body Fluid (SBF), which has the same ionic concentration as that of human plasma. Effects of biodegradation and change in mechanical properties of the composite when kept in SBF and maintained in a static condition were studied in terms of weight loss, change in the pH of the acellular solution and change in mechanical properties (hardness and biaxial strength). Scanning Electron Microscopy was used to observe the formation of apatite crystals on the surface of the nanocomposite specimens soaked in SBF. The results obtained throw light on biocompatibility and bioactivity of Al2TiO5 phase, which has not been reported so far in the literature to the best of our knowledge. Dielectric constant and dissipation factor of the sintered nanocomposite pellets were measured using HP 4284A impedance-capacitance-resistance meter and 16451 B dielectric test fixture at 1 MHz frequency. The effects of sintering time, temperature and phases present on the electrical properties were studied and are reported in the thesis.

This dissertation demonstrated that the manipulation of substances at the molecular or nanometer level can lead to the discovery and development of new materials with interesting properties and important applications. Chapter 1 describes the development of a nanoscale molecular thin film material for corrosion protection. By using a self-assembled monolayer film with a thickness of only about 1 nanometer as a linkage, a covalent bonding was achieved between a polyurethane top coating and an aluminum alloy substrate. This covalent bonding between polymer top coating and the aluminum alloy substrate significantly improved the corrosion resistance of the substrate. Chapter 2 and Chapter 3 describe the development of a gold nanoparticle-polymer composite material in different forms with a number of applications. Gold nanoparticles are among one of the most extensively studied nanomaterials. When the size of gold is shrunk to the nanometer scale, many interesting and new physical properties start to appear from gold nanoparticles. The optical properties of gold nanoparticles, particularly the surface plasmon resonance absorption, have been investigated in this dissertation for the development of multifunctional nanocomposite materials. Chapter 2 presents the preparation of a gold nanoparticle/poly(methyl methacrylate) (PMMA) nanocomposite film and the application of such films for microstructure fabrication using a direct laser writing technique. Gold nanoparticles are excellent photon-thermal energy converters due to their large absorption cross section at the surface plasmon resonance region. Upon laser irradiation of the nanocomposite film, the thermal energy converted from the absorbed photon energy by gold nanopaticles induced a complete decomposition of PMMA, leading to the formation of various microstructures on the nanocomposite films. Chapter 3 reports the further development of a nanoparticle/polymer composite nanofiber material fabricated through an electrospinning process. The matrix of the nanofiber is made of two polyelectrolytes, poly(acrylic acid) (PAA) and poly(allylamine hydrochloride) (PAH). Three methods were developed to incorporate gold nanoparticles into the polymer matrix. The composite nanofiber materials developed in this study demonstrate multifunctional properties, including good electrical conductivity, photothermal response, and surface-enhanced IR absorption. This material may be used for many important applications including catalysis, chemical and biological sensors, and scaffold materials for tissue engineering. In Chapter 4, another most important nanomaterial, carbon naotubes (CNTs), were introduced as fillers to prepare polymer nanocomposites. A dispersion method for multi-walled carbon nanotubes (MWCNTs) using a conjugated conducting polymer, poly(3-hexylthiophene) (P3HT) as the third component and trifluoroacetic acid (TFA) as a co-solvent was developed. Due to the excellent dispersion of carbon nanotubes in PMMA and enhanced conductivity of the nanocomposites by the conjugated conducting polymers, the prepared composite materials has an extremely low percolation threshold of less than 0.006 wt% of MWCNT content. The potential use of MWCNT/conducting polymer composites for energy storage applications such as suppercapacitors was further investigated by Cyclic Voltammetry (CV), Electrochemical Impedance Spectroscopy (EIS) and charging-discharging cycles. Compared to pure carbon nanotubes, the nanocomposite materials have significantly improved properties and are promising for supercapacitor applications.

Medium-voltage silicon carbide power devices, due to their higher operational temperature, higher blocking voltage, and faster switching speed, promise transformative possibilities for power electronics in grid-tied applications, thereby fostering a more sustainable, resilient, and reliable electric grid. The pursuit of increasing power density, however, escalates the blocking voltage and shrinks the module size, consequently posing unique insulation challenges for the medium voltage power module packaging. The state-of-the-art solutions, such as altering the geometry of the insulated-metal-substrates or thickening or stacking them, exhibit limited efficacy, inflate manufacturing costs, raise reliability concerns, and increase thermal resistance. This dissertation explores a material-based approach that utilizes a nonlinear resistive polymer nanocomposite field-grading coating to enhance insulation performance without compromising thermal performance for medium-voltage power modules. The studied polymer nanocomposite is a mutual effort of this research and NBE Technologies. Instead of using field-grading materials as encapsulation, a thin film coating (about 20 μm) can be achieved by painting the polymer nanocomposite solution to the critical regions to grade the electric field and extend the range of the applicability of the bulk encapsulation. A polymer nanocomposite's electrical properties were characterized and found theoretically and experimentally to be effective in improving the insulation performance or increasing the partial discharge inception voltage, of direct-bonded-copper substrates for medium-voltage power modules. By applying the polymer nanocomposite coating on the direct-bonded- copper triple-point edges, the partial discharge inception voltages of a wide range of direct-bonded-coppers increased by 50-100%. To assure its effectiveness for heated power modules during operation, this field-grading effect was then evaluated at elevated temperatures up to 200°C and found almost unchanged. The nanocomposite's long-term efficacy was further corroborated by voltage endurance tests. Building on these promising characterizations, functional power modules were designed, fabricated, and tested, employing the latest packaging techniques, including double-sided cooling and silver-sintering. Prototypes of 10-kV and 20-kV silicon carbide diode modules confirmed the practicality and efficacy of the polymer nanocomposite. The insulation enhancements observed at the module level mirrored those at the substrate level. Moreover, the polymer nanocomposite coating enabled modules to use insulated-metal-substrates with at least 100% thinner ceramic, resulting in a reduction of at least 30% in the junction-to-case thermal resistance of the module. Subsequently, to test the nanocomposite's performance during fast-switching transients (> 300 V/ns), 15-kV silicon carbide MOSFET modules were designed, fabricated, and evaluated. These more complex modules passed blocking tests, partial discharge tests, and double-pulse tests, further validating the feasibility of the nonlinear resistive polymer nanocomposite field-grading for medium-voltage power modules. In summary, this dissertation presents a comprehensive evaluation of a nonlinear resistive polymer nanocomposite field-grading coating for medium-voltage power modules. The insights and demonstrations provided in this work bring the widespread adoption of this packaging concept for medium-voltage power modules significantly closer to realization. / Doctor of Philosophy / This dissertation delves into a novel approach to improving the resilience and reliability of our electric grid by employing medium-voltage silicon carbide power devices. These power devices, due to their superior performance at higher temperatures and faster switching speeds, can revolutionize grid-tied power electronics. However, the challenge lies in safely packaging these devices, given their high blocking voltage and compact size. To address this, the study explores an innovative solution that uses a material called a nonlinear resistive polymer nanocomposite. This nanocomposite can improve insulation and endure high temperatures, promising a significant boost in performance for these power devices. The study reveals that applying this nanocomposite coating to the edges of direct- bonded-copper, a component of the power module, can enhance the insulation performance by 50-100%. Building on these findings, we designed, made, and tested functional power modules, using cutting-edge packaging techniques that we developed. The tests confirmed the practicality and effectiveness of the polymer nanocomposite, leading to insulation improvements on both the substrate and module levels. Importantly, this coating also reduced the thermal resistance of the module by at least 30%, signifying a more efficient operation. Then we evaluated the nanocomposite's performance during fast-switching transients in more complex silicon carbide modules. The modules passed multiple tests, further validating the feasibility of the nanocomposite coating for medium-voltage power modules. In essence, this dissertation uncovers a promising approach to more efficient and resilient power module packaging, paving the way for potential widespread adoption in the power electronics industry.

This dissertation describes the development and application of various mechanical characterization techniques to four types of polymer composite materials. The composite nature of these materials ranges from molecular to macro-scale, as do the size scales probed by the techniques chosen. The two main goals of this work are to evaluate the suitability of existing characterization methods to new composite materials (and augment the methods as needed), and to use these methods to determine optimal composite system parameters to maximize the desired mechanical response. Chapter 2 employs nondestructive ultrasonic spectroscopy for characterizing the stiffness response of both micron-scale woven composites and macro-scale glass-polymer-glass laminates. Both traditional wavespeed measurement as well as aspects of resonant ultrasonic spectroscopy are applied to determine material parameters. The laminates are also examined in Chapter 3, which utilizes both large-scale and small-scale quasi-static and dynamic puncture tests to elucidate the size- and rate-dependence of dynamic behavior. Because of limitations encountered with these methods, a smaller-scale, more fundamental test is developed and applied which focuses solely on the deformation and delamination of the polymer. These two processes, which account for the vast majority of energy absorbed during a puncture event, can be evaluated in terms of self-similar process zone propagation process models. Identifying and optimizing the relevant model parameters can promote the design of systems with maximum energy absorption. Exploratory work on nanocomposite systems is presented in Chapter 4. The polymer matrix from the laminated systems of the previous chapter is used to produce nanosilica composites. A range of techniques are employed to determine the level of dispersion and the mechanical reinforcement provided. The final project presented investigates copolycarbonates, or molecular composites, that have been developed to lessen the detrimental effect of aging on mechanical properties. Mechanical and thermal measurements can elucidate the effect of structure, specifically molecular mobility, on susceptibility to physical aging. The differences in molecular mobility contribute to differences in energy absorption by plastic deformation and damage, which is required for material toughness. Thus, understanding the molecular structure allows for determination of an optimal structure or copolymer concentration to maximize fracture toughness.