Metal oxide nanocrystals have attracted significant interests due to their unique chemical, physical, and electrical properties which depend on their size and structure. In this study, a continuous flow microreactor system was employed to synthesize metal oxide nanocrystals in aqueous solution. Assembly of nanocrystals is considered one of the most promising approaches to design nano-, microstructures, and complex mesoscopic architectures. A variety of strategies to induce nanocrystal assembly have been reported, including directed assembly methods that apply external forces to fabricate assembled structures. In this study ZnO nanocrystals were synthesized in an aqueous solution using a continuous flow microreactor. The growth mechanism and stability of ZnO nanocrystals were studied by varying the pH and flow conditions of the aqueous solution. It was found that convective fluid flow from Dean vortices in a winding microcapillary tube could be used for the assembly of ZnO nanocrystals. The ZnO nanocrystal assemblies formed three-dimensional mesoporous structures of different shapes including a tactoid, a retangle and a sphere. The assembly results from a competing interaction between electrostatic forces caused by surface charge of nanocrystals and collision of nanocrystals associated with Dean vortices. The as synthesized colloidal ZnO nanocrystals or assembly were directly deposited onto a substrate to fabricate ZnO nanostructured surfaces. The rectangular assembly led to flower-like ZnO nanostructured films, while the spherical assembly resulted in amorphous ZnO thin film and vertical ZnO nanowire (NW) arrays. In contrast to the formation of flower structure or amorphous thin film, only colloidal ZnO nanocrystals were used as the building blocks for forming vertical ZnO NW arrays. This study demonstrates the versatility of the microreactor-assisted nanomaterial synthesis and deposition process for the production of nanostrucuturesres with various morphologies by tuning the physical parameters while using the same chemical precursors for the synthesis. ZnO flower structure was coated on a microwick structure to improve the capillary flow. The coated microwick structure showed an enhanced capillary rise, which was attributed to the hydrophilic property and geometrical modification of ZnO nanostructure. Two-phase boiling heat transfer was performed using ZnO nanostructured surfaces. ZnO nanocoating altered the important characteristics including surface roughness and wettability. Hydrophilic nature of the ZnO nanocoating generally enhanced the boiling heat transfer performance, resulting in higher heat transfer coefficient (HTC), higher critical heat flux (CHF), and lower surface superheat comparing to the bare surface. Octahedral SnO and porous NiO films, fabricated by a continuous flow microreactor system, were suggested as potential boiling surfaces for the high porosity and irregularity of their structures. / Graduation date: 2013

A novel surface structure comprising dendritically ordered nano-particles of copper was developed during the duration of this thesis research project. A high current density electrodeposition process, where hydrogen bubbles functioned as a dynamic mask for the materials deposition, was used as a basic fabrication method. A post processing annealing treatment was further developed to stabilize and enhance the mechanical stability of the structure. The structure was studied quite extensively in various pool boiling experiments in refrigerants; R134a and FC-72. Different parameters were investigated, such as; thickness of the porous layer, presence of vapor escape channels, annealed or non-annealed structure. Some of the tests were filmed with a high speed camera, from which visual observation were made as well as quantitative bubble data extracted. The overall heat transfer coefficient in R134a was enhanced by about an order of magnitude compared to a plain reference surface and bubble image data suggests that both single- and two-phase heat transfer mechanisms were important to the enhancement. A quantitative and semi-empirical boiling model was presented where the main two-phase heat transfer mechanism inside the porous structure was assumed to be; micro-layer evaporation formed by an oscillating vapor-liquid meniscus front with low resistance vapor transport through escape channels. Laminar liquid motion induced by the oscillating vapor front was suggested as the primary single-phase heat transfer mechanism. The structure was applied to a standard plate heat exchanger evaporator with varying hydraulic diameter in the refrigerant channel. Again, a 10 times improved heat transfer coefficient in the refrigerant channel was recorded, resulting in an improvement of the overall heat transfer coefficient with over 100%. A superposition model was used to evaluate the results and it was found that for the enhanced boiling structure, variations of the hydraulic diameter caused a change in the nucleate boiling mechanism, which accounted for the largest effect on the heat transfer performance. For the standard heat exchanger, it was mostly the convective boiling mechanism that was affected by the change in hydraulic diameter. The structure was also applied to the evaporator surface in a two-phase thermosyphon with R134a as working fluid. The nucleate boiling mechanism was found to be enhanced with about 4 times and high speed videos of the enhanced evaporator reveal an isolated bubble flow regime, similar to that of smooth channels with larger hydraulic diameters. The number and frequency of the produced bubbles were significantly higher for the enhanced surface compared to that of the plain evaporator. This enhanced turbulence and continuous boiling on the porous structure resulted in decreased oscillations in the thermosyphon for the entire range of heat fluxes. / QC 20111111

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<p dir="ltr">Boiling processes have long had an important role in power generation and air conditioning applications. The efficient and reliable heat dissipation afforded through the phase change process in the boiling has led to their generation of a substantial body of work in this field over several decades. Despite decades of efforts, the heat transfer performance prediction in boiling has been highly empirical with models working only for a narrow range of surface/fluids or other operating conditions. The limitation in these models is a result of a lack of mechanistic understanding of the underlying heat and mass transfer process. Surface dryout or boiling crisis is a process wherein there is a spontaneous formation of vapor film on top of the surface causing a catastrophic increase in surface temperature. The heat flux at which this formation of vapor film occurs is called critical heat flux (CHF). The CHF demarcates the upper limit to the regime of stable nucleating bubbles called nucleate boiling. The mechanism causing dryout is under debate for over half a century and several conflicting theories that cause dryout have been suggested since the 1950s including hydrodynamic, irreversible dryspot expansion, macrolayer dryout/liftoff, critical bubble distributions, vapor-recoil based theories and more. The lack of consensus is due to limitation in the information collected on the dynamic multiscale and chaotic bubble interactions. Recent advances in high-fidelity spatiotemporal phase, temperature, and heat flux measurements now enable diagnostic tools that can be leveraged to understand the complex heat transfer processes emerging from bubble-surface interaction on the boiling surface. In this work, we develop such techniques to understand various transport mechanisms underlying boiling and its crisis.</p><p dir="ltr">In this work, an experimental technique for collecting synchronized through-substrate visual and infrared (IR) measurements of a boiling surface is developed. An IR and visually transparent sapphire substrate with an IR-opaque indium-tin-oxide (ITO) heater layer is used to measure the phase (liquid and vapor areas) and temperature of the ITO layer. The visual camera collects the light reflected off the substrate from a red LED and the images collected show a contrast between liquid and vapor areas that is used to generate binarized phase maps. The temperature from the IR camera is used as boundary condition to solve a conduction problem for heat fluxes going into the fluid. Four distinct heat flux signatures corresponding to liquid, contact line, vapor and rewetting regions are observed. A post-processing methodology utilizing synchronous phase measurements to identify and partition these regions is introduced. The high-fidelity phase measurements allow for detection of fine features that are not discernable using heat flux maps alone. Analysis of the heat flux and temperature maps of partitioned regions for HFE-7100 fluid on the ITO surface show qualitative agreement with the trends in mechanisms underlying those areas. The experiment and post-processing methodology introduced in this work is the first to provide partitioning of underlying heat transfer mechanisms for multi-bubbles throughout the entire range of the boiling curve during both steady and transient scenarios.</p><p dir="ltr">The technique developed is used to probe the mechanisms underlying the boiling crisis. Theories suggested in the literature for boiling crisis are carefully evaluated and evidence against hydrodynamic instability, macrolayer dryout, vapor recoil, irreversible expansion of dryspots, macrolayer liftoff model, and bifurcations from critical distributions is observed. The signature in the peak of the spatially averaged fluid heat flux is observed to precede any other signs of dryout. Beyond the peak heat flux an increase in superheat leads to reduced heat dissipated by boiling and further increases the temperature causing a thermal runaway in the substrate that eventually leads to dryout. Hence, the boiling crisis is found to be a consequence of a peak in the nucleate boiling curve. The cause for the peak in the boiling heat flux for the surface-fluid combination tested was due to degradation of heat transfer caused by the replacement of high-heat-transfer contact line region with lower-heat-transfer vapor covered regions, among the multiple competing mechanisms. Hence, we propose that mechanistically modeling the boiling crisis rests on prediction of the peak in the upper portion of the nucleate boiling curve by considering all underlying heat transfer mechanisms. A modeling framework based on heat flux partitioning, where the overall heat transferred during boiling is calculated as the sum of the heat transferred by individual mechanisms is demonstrated as potential pathway to predict the upper portion of the nucleate boiling curve and thereby critical heat flux. Based on the terms involved in summation for individual mechanisms, we propose that the boiling curve for any given surface be interpreted as a path on a multidimensional surface (boiling manifold). Estimation of such a boiling manifold allows for prediction of the boiling curve for any surface, given development of the relations between these parameters and surface-fluid properties, and can further be used to backtrack relevant thermophysical or nucleation properties for enhanced boiling performance.</p><p dir="ltr">Enhancement of pool boiling heat transfer performance using surface modifications is of major interest to applications and this work further delves into characterizing the boiling performance using traditional surface averaged measurements of microstructured surfaces using HFE-7100. We find that microlayer evaporation from the imbibed liquid layer underneath the growing vapor bubbles is the key mechanism of boiling heat transfer enhancement in microstructures. Further, this implies that characterization of microstructured surfaces for evaporative performance can serve as an important proxy to enable heat transfer coefficient enhancement prediction during pool boiling. Hence, we also developed an easily calculated Figure of Merit (FOM) that characterizes the efficacy of evaporation from microstructured surfaces.</p><p dir="ltr">To summarize, in this work we developed an experimental technique using synchronous through-substrate high-speed visual and IR imaging methods. New post-processing techniques for partitioning of different heat transfer mechanisms are proposed and used to analyze boiling on an ITO-coated sapphire substrate with HFE-7100 as the working fluid. We reveal thermal runaway in the substrate caused due to a negative-sloping boiling curve as the mechanism of dryout. Mechanistic modeling of the critical heat flux thus involves calculating the peak in the nucleate boiling curve. A framework to predict the nucleate boiling curve and subsequently critical heat flux is proposed based on the partitioning analysis. The experimental method developed lays the groundwork for measuring heat flux and superheats associated with various mechanisms, and hence, enables validation of future partitioning-based boiling heat transfer models that intrinsically enable prediction of the peak.</p>