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<p>The impinging jets atomizer is widely used in engineering applications. As two liquid jetsimpinging to each other, a liquid sheet is first formed and then breaks up into small dropletsto comply the atomization. The features such as size, shape, velocity, thickness, etc., of thesheet/droplet are controlled by various impingement parameters such as impinging angle,jet velocity, and physical properties of the liquid. Since the sheet generation is prior to thedroplet, the modeling of the sheet is the premise of the droplet modeling. Therefore, to studythe atomization of the impinging jet atomizer, it is important to pay effort on the research ofimpinging sheet both experimentally and theoretically. In this research, the characterizationof the impinging sheet formed by two jets is given in two specific aspects, the thicknessand the velocity. A non-intrusive measurement technique, partial coherent interferometry(PCI) is developed and applied to measure the thickness of the impinging sheet dynamically.The PCI unitizes the calibrated linear relationship between the optical path difference andthe degree of coherence to measure the impinging sheet thickness. By placing the sheet inone of the two branches of the designed interferometer, the optical path is altered basedon the sheet thickness and shown as the change of the degree of coherence of interferencepattern recorded by the camera. With a calibration process, the thickness of the sheet is thencan be measured via a designed interferometer. The velocity measurement of the impingingsheet is implemented via particle tracking velocimetry (PTV) adopted with the shadowgraphtechnique. To implement the particle tracking velocimetry, seeding particles are added intothe fluid and with the aid of an imaging acquiring system and the post-processing algorithm,the locations of those particles in different frames are identified. Thus, the velocity of the fluidis estimated as the velocity of the particles calculated from the recorded images. However,while applying the PTV to investigate the impinging sheet studied in this research, theparticles can be recorded at a large field of view with insufficient magnification. This is ownedto the so-called "particle induced lens effect" found when applying the small particles to athin liquid sheet. When the seeding particles move to the region where the sheet thicknesshas a similar scale as the particle, the fluid will wrap around the particle and act as a positivelens. For shadowgraph imaging, the collimated light forms an enlarged shadow at the image plane by passing through such lens. Experimentally, the thickness measurements via PCIare implied to the impinging sheet generated under a range of Reynolds number between 269to 370 and velocity measurements via PTV are implied to the ones under Reynolds numberof 362 to 430. The measured results for both thickness and velocity are different from thetheoretical model of the impinging sheet which implies the need for a review of sheet model.Therefore, in this research, the author proposed a revised impinging sheet model considerthe friction effect due to the air over the sheet. A theoretical analysis is made base on theboundary layer equation under the cylindrical coordinate with unique boundary conditionsassumed for the impinging sheet. By introducing the unique similarity variable found byauthor, the equation could be transformed to an ordinary differential equation and solvednumerically. The revised model first predict the air boundary layer profile over the sheet,then, estimate the sheet velocity profile as a function of the distance to the impinging pointand the azimuth angle. As a parameter of the revised sheet model, the jet velocity profilebefore the impingement is also assumed as a free jet gradually developed from a Posieuilleflow and estimated in advance. The revised model is compared with the experimental resultsand some key parameters are identified empirically.</p> <p>Other than the thickness and velocity, this research is also interested in measuring thegeometry of the sheet and the detached droplets. Thus, a multi-view digital inline holography(DIH) technique is developed to capture the three-dimensional shape of the impinging sheetand the locations of the droplets. The DIH determines the shape and location of the targetin a detection volume base on the recorded hologram. The MvDIH, as the name suggested,combines the DIH results from multiple orientations to reconstruct the shape and the locationof the target. Two reconstruction ideologies, cross-section based one and the outline basedone, are proposed. The former estimates the target by finding the intersection of the recordedcross-sections of the target from different views. The latter estimates the target geometryby combining the outlines determined by DIH at different views. To evaluate the feasibilityof such technique, a test model which imitates the droplet and liquid ligament structure isapplied to the measurement in this research. Yet, the application on a real impinging sheetis not implemented.</p>

The characterization of the material’s deformation is nowadays common in transmission electron microscopy. The ability to resolve the crystalline lattice enables the strain to be linked with the deformation of the crystal unit cells. Imaging the crystal unit cells imposes the sampling scheme to oversample the resolved crystal periodicities and, thus, limits the field of view (FOV) of the micrograph. Therefore, alternative methods were developed (electron diffraction and holography) to overcome the FOV limitation. The method presented in this thesis is part of the large FOV challenge. Its principle is based on the coherent interference of the sampling grid with the crystalline lattices of the material in scanning transmission electron microscopy (STEM). The interference results to a set of Moiré fringes embedding the structural properties of the material such as a strain field. The STEM Moiré hologram (SMH) formation can be elegantly described using the concept of Moiré sampling in STEM imaging. The STEM Moiré fringes reveals to be undersampling artefacts commonly known as aliasing artefacts. The SMH is, therefore, violating the sampling theorem and is not a proper representation of the crystal unit cells. However, an oversampled representation can be recovered from the SMH using a set of prior knowledge. The SMH becomes suitable to characterize the 2D strain field giving birth to a new dedicated method, called STEM Moiré GPA (SMG), that is using the Geometric Phase Analysis method on the SMH directly. After detailing the theory of SMG, the technique is validated experimentally by comparing it to other strain characterization methods and to Finite Element Method simulations. The characteristics of SMG (resolution, precision and accuracy) and its limits are then detailed. Finally, the SMG method is applied on semiconductor devices to highlight the typical capabilities of the technique. / Thesis / Doctor of Philosophy (PhD)

A dual-frequency system is needed to better understand natural processes that constitute the environment and seasonal cycles of the Earth. A system working at two different wavelengths acquiring data simultaneously will give a valuable dataset since the conditions on the ground will be exactly the same. Hence, elements such as wind, soil moisture or any other changes on the ground will not interfere in the mea- surements. This thesis explains how an S-band radar was built and tested. Moreover, the experiments done with a Ka-band radar used as a scatterometer are explained as well as the data processing and analysis. Finally, the two systems are used to get dual-frequency measurements from an airborne platform. The dual-frequency data is explored, showing the differences in normalized radar cross-section between frequencies and discussing the interferometric measurements.

The effect of thermal-cycling-induced microcracking in fiber-reinforced polymer matrix composites is studied. Specific attention is focused on microcrack density as a function of the number of thermal cycles, and the effect of microcracking on the dimensional stability of composite materials. Changes in laminate coefficient of thermal expansion (CTE) and laminate stiffness are of primary concern. Included in the study are materials containing four different Thornel fiber types: a PAN-based T50 fiber and three pitch-based fibers, P55, P75, and P120. The fiber stiffnesses range from 55 Msi to 120 Msi. The fiber CTE's range from -0.50x10⁻⁶/°F to -0.80x10⁻⁶/°F. Also included are three matrix types: Fiberite's 934 epoxy, Amoco's ERL1962 toughened epoxy, and YLA's RS3 cyanate ester. The lamination sequences of the materials considered include a cross-ply configuration, [0/90]2s, and two quasi-isotropic configurations, [0/+45/-45/90]s and [0/+45/90/-45]s. The layer thickness of the materials range from a nominal 0.001 in. to 0.005 in. In addition to the variety of materials considered, three different thermal cycling temperature ranges are considered. These temperature ranges are ±250°F, ±150°F, and ±50°F. The combination of these material and geometric parameters and temperature ranges, combined with thermal cycling to thousands of cycles, makes this one of the most comprehensive studies of thermal-cycling-induced microcracking to date. Experimental comparisons are presented by examining the effect of layer thickness, fiber type, matrix type, and thermal cycling temperature range on microcracking and its influence on the laminates. Results regarding layer thickness effects indicate that thin-layer laminates microcrack more severely than identical laminates with thick layers. For some specimens in this study, the number of microcracks in thin-layer specimens exceeds that in thick-layer specimens by more than a factor of two. Despite the higher number of microcracks in the thin-layer specimens, small changes in CTE after thousands of cycles indicate that the thin-layer specimens are relatively unaffected by the presence of these cracks compared to the thick-layer specimens. Results regarding fiber type indicate that the number of microcracks and the change in CTE after thousands of cycles in the specimens containing PAN-based fibers are less than in the specimens containing comparable stiffness pitch-based fibers. Results for specimens containing the different pitch-based fibers indicate that after thousands of cycles, the number of microcracks in the specimens does not depend on the modulus or CTE of the fiber. The change in laminate CTE does, however, depend highly on the stiffness and CTE of the fiber. Fibers with higher stiffness and more negative CTE exhibit the lowest change in laminate CTE as a result of thermal cycling. The overall CTE of these specimens is, however, more negative as a result of the more negative CTE of the fiber. Results regarding matrix type based on the ±250°F temperature range indicate that the RS3 cyanate ester resin system exhibits the greatest resistance to microcracking and the least change in CTE, particularly for cycles numbering 3000 and less. Extrapolations to higher numbers of cycles indicate, however, that the margin of increased performance is expected to decrease with additional thermal cycling. Results regarding thermal cycling temperature range depend on the matrix type considered and the layer thickness of the specimens. For the ERL1962 resin system, microcrack saturation is expected to occur in all specimens, regardless of the temperature range to which the specimens are exposed. By contrast, the RS3 resin system demonstrates a threshold effect such that cycled to less severe temperature ranges, microcracking does not occur. For the RS3 specimens with 0.005 in. layer thickness, no microcracking or changes in CTE are observed in specimens cycled between between ±150°F or ±50°F. For the RS3 specimens with 0.002 in. layer thickness, no microcracking or changes in CTE are observed in specimens cycled between ±50°F.. Results regarding laminate stiffness indicate negligible change in laminate stiffness due to thermal cycling for the materials and geometries considered in this investigation. The study includes X-ray examination of the specimens, showing that cracks observed at the edge of the specimens penetrate the entire width of the specimen. Glass transition temperatures of the specimens are measured, showing that resin chemistry is not altered as a result of thermal cycling. Results are also presented based on a one-dimensional shear lag analysis developed in the literature. The analysis requires material property information that is difficult to obtain experimentally. Using limited data from the present investigation, material properties associated with the analysis are modified to obtain reasonable agreement with measured microcrack densities. Based on these derived material properties, the analysis generally overpredicts the change in laminate CTE. Predicted changes in laminate stiffness show reasonable correlation with experimentally measured values. / Ph. D.

Measurement of physical parameters in harsh environments (high pressure, high temperature, highly corrosive, high electromagnetic interference) is often desired in a variety of areas, such as aerospace, automobile, energy, military systems, and industrial processes. Pressure and temperature are among the most important of these parameters. A typical example is pressure monitoring in jet engine compressors to help detect and control undesirable air flow instabilities, namely rotating stall and surge. However, the temperatures inside a compressor could reach beyond 600°C for today's large engines. Current fiber-optic sensor can operate up to about 300°C and even the most widely employed semiconductor sensors are limited below 500°C. The objective of this research is to push the limit of fiber-optic sensing technology in harsh environment applications for both pressure and temperature measurements by developing novel sensing structures, fabrication techniques, and signal processing algorithms. An all-fused-silica pressure sensor has been demonstrated which is fabricated on the tip of a fiber with a diameter no larger than 125μm. The sensor was able to function beyond the current limit and operate into the 600~700°C range. Also a temperature sensor has been developed using sapphire fibers and wafers for ultra-high temperature measurement as high as 1600°C. This effort will generate more understanding regarding sapphire fiber's high temperature properties and could possibly lead to novel designs of pressure sensor for beyond 1000°C. Both sensors have been field tested in real-world harsh environments and demonstrated to be reliably and robust. In this dissertation, the design, fabrication, and testing of the sensors are discussed in detail. The system and signal processing techniques are presented. The plan and direction for future work are also suggested with an aim of further pushing the operating limit of fiber-optic sensors. / Ph. D.

Fiber-optic Fabry-Perot interferometric (FFPI) sensors have been widely used due to their high sensitivity, ease of fabrication, miniature size, and capability for multiplexing. However, direct measurement of self-assembled thin films, receptor immobilization process or biological reaction is limited in the FFPI technique due to the difficulty of forming Fabry-Perot cavities by the thin film itself. Novel methods are needed to provide an accurate and reliable measurement for monitoring the thin-film growth in the nanometer range and under various conditions. In this work, two types of fiber-optic multicavity Fabry-Perot interferometric (MFPI) sensors with built-in temperature compensation were designed and fabricated for thin-film measurement, with applications in chemical and biological sensing. Both the tubing-based MFPI sensor and microgap MFPI sensor provide simple, yet high performance solutions for thin-film sensing. The temperature dependence of the sensing cavity is compensated by extracting the temperature information from a second multiplexed cavity. This provides the opportunity to examine the thin-film characteristics under different environment temperatures. To demonstrate the potential of this structure for practical applications, immunosensors were fabricated and tested using these structures. Self-assembled polyelectrolytes served as a precursor film for immobilization of antibodies to ensure they retain their biological activity. This not only provides a convenient method for protein immobilization but also presents the possibility of increasing the binding capacity and sensitivity by incorporating multilayers of antibodies into polyelectrolyte layers. The steady-state measurement demonstrated the surface concentration and binding ratio of the immunoreaction. Analysis of the kinetic binding profile provided a fast and effective way to measure antigen concentration. Monitoring the immunoreaction between commercially available immunoglobulin G (IgG) and anti-IgG demonstrated the feasibility of using the MFPI sensing system for immunosensing applications. / Ph. D.

Corrosion-related degradation incurs a significant cost to infrastructure and society. In 2016, the direct corrosion cost was estimated at $276 billion, which is 3.1% of the U.S. gross domestic product. Despite the known consequences of corrosion damage, many unknowns still exist, such as the mechanisms and rates of chloride-induced corrosion initiation and propagation. There is also a lack of high-quality quantitative kinetic data and analysis that can obtain the fundamental micro- and nanostructural mechanisms and initiation of metal corrosion. The corrosion initiation in metals is considered to be governed by dynamic processes that take place at the nanoscale. Thus, the measurement of nanoscale surface structures correlated with electrochemical properties in metals is critical in the understanding of corrosion initiation, and microstructure-corrosion relationship, as well as efforts toward materials design for corrosion mitigation. As a fundamental approach to this study, a systematic review of different surface characterization techniques was initially discussed. This entailed their principles, applications, and perspectives for surface corrosion monitoring, enabling the development of next-generation inhibition technologies, and improving corrosion predictive models. Unprecedented, this research study presented a novel application of a quantitative phase microscopy technique, spectral modulation interferometry (SMI), for in situ nanoscale characterization of corrosion of different alloys in real-time. SMI offers high sensitivity, rapid image acquisition, and speckle-free images; thus, real-time quantification of surface topography evolution during corrosion can be obtained accurately to evaluate the temporally- and spatially-dependent corrosion rates. With an innovative additive-manufactured fluid cell, experiments were performed under flowing solution conditions. Electrochemical tests via stepwise polarization and solution chemistry through collected aliquots of outflow solution were also performed alongside the nanoscale SMI experiment to simultaneously provide corroborating corrosion rate measurements. This innovative approach to measuring dissolution rates of metal at three levels can provide highly quantitative kinetic data of reacting surfaces that are rarely explored in the literature. First, the in situ SMI combined with the stepwise potentiostatic tests and the solution chemistry analysis was used to investigate the nanoscale characterization of corrosion of an AA6111-T4 aluminum alloy in real-time. The corrosion experiment was conducted in a 0.5 wt.% NaCl flowing solution acidified to pH ⁓2.9 by acetic acid. Based on the quantitative 3D height profiles across the corroded surface, pit formation resulting from rapid local corrosion was predominant, which is heterogeneously distributed and was appearing at different times. The computed time-dependent dissolution rates of aluminum also varied as the experiment proceeded, with the combination of linear and nonlinear surface normal distributions. An initial mean linear dissolution rate of (0.40 ± 0.007) μmol m−2 s−1 transitioned to a more rapid mean rate of (1.95 ± 0.035) μmol m−2 s−1, driven by the anodic polarization. Dissolution rates from the three performed methods follow similar trends and there is the visibility of linking the nanoscale in situ SMI data to the electrochemical corrosion measurements and ex situ chemical solution analysis. At the end of the corrosion period, rates of 118, 71, and 2.45 μmol m−2 s−1 were obtained from electrochemical measurements, ex situ solution analyses, and in situ SMI corrosion measurements, respectively. In addition, SMI–electrochemical experiments were performed to evaluate the effect of thermal history on corrosion modes and rates of AA6111. Quantitative estimates of the corrosion initiation and propagation in the alloy were also assessed. A single coil of AA6111 alloy that was solution heat treated at a temperature above 500°C and quenched with 2 different water quench rates (i.e., slow-quenched at 131ºC/s and fast-quenched at 506ºC/s) with each in T4 and T82 temper condition was investigated in this study. Irrespective of the quenched and/or temper conditions, the electrochemical potential-current (E-i) results showed a similar pattern in the polarization curve and similar current response over the immersed time, and a small difference in their corrosion behavior will be difficult to detect due to the dissolution kinetics that takes place on the nanoscale. As revealed from the SMI topography map, the corrosion modes at the nanoscale were very distinct despite having similar electrochemical responses and chemical compositions. Primarily, heterogeneous dissolution of intergranular corrosion (IGC) and crystallographic pitting was observed in the tested alloy substrates, with the slow-quenched samples susceptible to IGC and the fast-quenched samples susceptible to crystallographic pitting. The nucleation of IGC sites is triggered by the increased coarsening and formation of precipitates in the grain boundary, while the pitting corrosion is attributed to the coarsening of the precipitates in the grain bodies. The quantitative analysis of topography evolution from the SMI data revealed a non-uniform (i.e., heterogenous) surface dissolution, as is typical for aluminum alloys. Notably, the fast-quenched material resisted corrosion initiation for a longer time and showed great resistance even at higher anodic polarization. However, an instant breakdown then occurred after 60mV of polarization and corrosion accelerated faster, relative to the slow-quenched material which initiated sooner (i.e. with less overpotential). In this setup, it is now possible to detect and evaluate these differences quantitatively through a quick corrosion test with the combined electrochemical-SMI technique. Therefore, this work showed that the corrosion susceptibility of AA6111 alloy is influenced by the thermal history, which can be controlled with a proper quench rate and further tempering. Additionally, this research also utilized the novel SMI techniques to investigate in situ chloride-induced corrosion of A615 low-carbon steel at the nanoscale. Along with surface topography monitoring, a potentiostat was connected to simultaneously monitor the bulk electrochemical activity of the carbon steel. Experiments were conducted in chloride-free and chloride-enriched solutions at pH 5 to investigate the role of chloride on topography evolution, dissolution mode, and corrosion kinetics. The 3D topography map acquired from the SMI showed an early formation of localized shallow pits on the surface subjected to the chloride free-solution. A more detrimental form of corrosion was obtained on the samples in chloride-enriched solution, which revealed early-age microcracks or intergranular defective sites associated with the heterogeneous roughening of the sample surface. The presence of chloride ions also influenced the initiation period of corrosion. Indeed, higher grain defects were obtained in samples immersed in 5.0 wt.% NaCl solution than the sample in 1.0 wt.% NaCl solution. The quantitative analysis of the height profile data (acquired from SMI) verified the heterogeneity of the corrosion process of both samples either susceptible to pitting corrosion and/or intergranular corrosion behavior. A faster dissolution rate was acquired on the sample immersed in 5.0 wt.% NaCl solution, with the rate of (3.53 ± 0.103) μmol m−2 s−1 and (5.64 ± 0.0225) μmol m−2 s−1 computed at the initiation and propagation stages, respectively. Likewise, the estimated volume loss followed a similar trend to the 3D surface topography data, but a distinct behavior in the volume loss was observed when compared to the void volume obtained from the electrochemical monitoring. This confirmed that the electrochemical measurement overestimates metal loss and does not present a good representation of material dissolution on the nanoscale. Finally, a different perspective of corrosion mitigation in the metallic alloy was presented. The extensive application of deicing salts has led to significant deterioration in many transportation infrastructures and automobiles due to corrosion. In this regard, the work investigated the corrosion inhibition performance of 2 corn-derived polyols, namely: sorbitol, and mannitol, on reinforced steel rebar. The results demonstrated that the incorporation of polyols in the deicing solution reduced the corrosion initiation while the inhibition rate increased as the polyol content increased from 0% to 5wt.%. The outcome of this study contributed to the search for mitigation strategies to minimize the impact of deicing chemicals on steel infrastructures. Overall, it is evident that corrosion is a huge durability problem and requires significant consideration when designing metals or alloys that are usually exposed to hostile environments. Understanding the nanostructural and kinetics of corrosion at both the initiation and propagation periods, as well as its thermodynamics, is important for designing a suitable protection strategy. This dissertation is expected to present the application of the surface technique to directly quantify the dynamic evolution of site-specific local corrosion of metals during early initiation stages at the nanoscale. / Doctor of Philosophy / Corrosion-related degradation incurs a significant cost to infrastructure and society. In 2016, the direct corrosion cost was estimated at $276 billion, which is 3.1% of the U.S. gross domestic product. Despite the known consequences of corrosion damage, many unknowns still exist, such as the mechanisms and rates of chloride-induced corrosion initiation and propagation. There is also a lack of high-quality quantitative kinetic data and analysis that can obtain the fundamental micro- and nanostructural mechanisms and initiation of metal corrosion. The corrosion initiation in metals is considered to be governed by dynamic processes that take place at the nanoscale. Thus, the measurement of nanoscale surface structures correlated with electrochemical properties in metals is critical in the understanding of corrosion initiation, and microstructure-corrosion relationship, as well as efforts toward materials design for corrosion mitigation. As a fundamental approach to this study, a systematic review of different surface characterization techniques was initially discussed. This entailed their principles, applications, and perspectives for surface corrosion monitoring, enabling the development of next-generation inhibition technologies, and improving corrosion predictive models. Unprecedented, this research study presented a novel application of a quantitative phase microscopy technique, spectral modulation interferometry (SMI), for in situ nanoscale characterization of corrosion of different alloys in real-time. SMI offers high sensitivity, rapid image acquisition, and speckle-free images; thus, real-time quantification of surface topography evolution during corrosion can be obtained accurately to evaluate the temporally- and spatially-dependent corrosion rates. With an innovative additive-manufactured fluid cell, experiments were performed under flowing solution conditions. Electrochemical tests via stepwise polarization and solution chemistry through collected aliquots of outflow solution were also performed simultaneously with the nanoscale SMI experiment to provide corroborating corrosion rate measurements. This innovative approach to measuring dissolution rates of metal at three levels simultaneously can now provide highly quantitative kinetic data of reacting surfaces that are not explored in the literature.