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In frequency-domain photothermal radiometry (FD-PTR) a low-power intensity-modulated optical excitation generates thermal-wave field inside the sample and the subsequent infrared radiation from the sample is analyzed to detect material’s inhomogeneities. The non-contact nature of FD-PTR makes it very suitable for non-destructive evaluation of broad range of materials. Moreover, the methodology is based on intrinsic contrast of light absorption which can be used as a diagnostic tool for inspection of malignancy in biological tissues. Nevertheless, the bottom line is that the physics of heat diffusion allows for a highly damped and dispersive propagation of thermal-waves. As a result, the current FD-PTR modalities suffer from limited inspection depth and poor axial/depth resolution. The main objective of this thesis is to show that using alternative types of modulation schemes (such as linear frequency modulation and binary phase coding) and radar matched filter signal processing, one can obtain localized responses from inherently diffuse thermal wave fields. In this thesis, the photothermal responses of turbid, transparent, and opaque media to linear frequency modulated and binary phase coded excitations are analytically derived. Theoretical simulations suggest that matched-filtering in diffusion-wave field acts as constructive interferometry, localizing the energy of the long-duty excitation under a narrow peak and allowing one to construct depth resolved images. The developed technique is the diffusion equivalent of optical coherence tomography and is named thermal coherence tomography. It was found that the narrow-band binary phase coded matched filtering yields optimal depth resolution, while the broad-band linear frequency modulation can be used to quantify material properties through the multi-parameter fitting of the experimental data to the developed theory. Thermophotonic detection of early dental caries is discussed in detail as a potential diagnostic application of the proposed methodologies. The performance of the diagnostic system is verified through a controlled demineralization protocol as well as in teeth with natural caries.

In frequency-domain photothermal radiometry (FD-PTR) a low-power intensity-modulated optical excitation generates thermal-wave field inside the sample and the subsequent infrared radiation from the sample is analyzed to detect material’s inhomogeneities. The non-contact nature of FD-PTR makes it very suitable for non-destructive evaluation of broad range of materials. Moreover, the methodology is based on intrinsic contrast of light absorption which can be used as a diagnostic tool for inspection of malignancy in biological tissues. Nevertheless, the bottom line is that the physics of heat diffusion allows for a highly damped and dispersive propagation of thermal-waves. As a result, the current FD-PTR modalities suffer from limited inspection depth and poor axial/depth resolution. The main objective of this thesis is to show that using alternative types of modulation schemes (such as linear frequency modulation and binary phase coding) and radar matched filter signal processing, one can obtain localized responses from inherently diffuse thermal wave fields. In this thesis, the photothermal responses of turbid, transparent, and opaque media to linear frequency modulated and binary phase coded excitations are analytically derived. Theoretical simulations suggest that matched-filtering in diffusion-wave field acts as constructive interferometry, localizing the energy of the long-duty excitation under a narrow peak and allowing one to construct depth resolved images. The developed technique is the diffusion equivalent of optical coherence tomography and is named thermal coherence tomography. It was found that the narrow-band binary phase coded matched filtering yields optimal depth resolution, while the broad-band linear frequency modulation can be used to quantify material properties through the multi-parameter fitting of the experimental data to the developed theory. Thermophotonic detection of early dental caries is discussed in detail as a potential diagnostic application of the proposed methodologies. The performance of the diagnostic system is verified through a controlled demineralization protocol as well as in teeth with natural caries.

Experiments at the University of Maryland Plasma Physics Laboratory have discovered an unusual temperature response in the form of a "thermal wave" which begins at the center and propagates towards the surface of a zinc oxide sample, when heated in a microwave cavity without the presence of oxygen. This effect is believed to be caused by the irregular temperature dependence of the dielectric properties of zinc oxide, particularly dielectric loss. Two thermocouple probes were used to measure the temperature response in a small cylindrical sample of zinc oxide packed in powder insulation, and heated in a microwave oven. In order to determine if the unusual response is caused by the dielectric properties, this work uses a finite-difference mathematical model to simulate the experiments, both for the case of zinc oxide heated in ordinary air, as well as for the case of zinc oxide heated in nitrogen. A revised version of the model is used to determine if the thermocouple probe has any effect on the temperature of the sample. The spatial and temporal temperature distribution results from the model indicate that the thermocouple probe has a negligible effect on the results and that the "thermal wave" can be attributed to the irregular temperature dependence of the dielectric loss of the material. / Master of Science

Nanocomposites with expandable smectites such as montmorillonite layered silicates (MLS) in polymer matrices have attracted extensive application interest. Numerous MLS concentrations have been used with no particular justification. Here, we investigate the effects of MLS dispersion within the matrix and on mechanical performance. The latter is resolved through a three-prong investigation on rate dependent tensile results, time dependent creep results and the influence of a sharp notch in polypropylene (PP) nanocomposites. A fixed concentration of maleated polypropylene (mPP) was utilized as a compatibilizer between the MLS and non-polar PP. Analysis of transmission electron micrographs and X-ray diffraction patterns on the surface and below the surface of our samples revealed a unique skin-core effect induced by the presence of clay. Differential scanning calorimetric and polarized optical microscopic examination of spherulites sizes showed changes in nucleation and growth resulting from both the maleated PP compatibilizer and the MLS. These structural changes resulted in a tough nanocomposite, a concept not reported before in the PP literature. Nonlinear creep analysis of the materials showed two concentrations 3 and 5 % wt of PP, which reduced the compliance in the base PP. The use of thermal wave imaging allowed the identification of ductile failure among materials, but more important, aided the mapping of the elastic and plastic contributions. These are essential concepts in fracture analysis.

In the near future, Gen II, III, and IV nuclear reactors will be in operation. UO2 is a common fuel for reactors in each of these generations and molten salts are used as coolant/fuel in Gen IV molten salt reactors. This thesis investigates potential ways to measure thermal conductivity for these materials: Raman thermometry for UO2 and a needle probe for molten salts. Four Raman thermometry techniques are investigated in this thesis: The Two Laser Raman (TLR), Time Differential Domain Raman (TDDR), Frequency Resolved Raman (FRR), and Frequency Domain Raman (FDR). The TLR is a steady state method used with a thin film. The TDDR and FRR are both time domain methods used with thin cantilever samples. The FDR is a frequency domain method used with a thermally thick sample. Monte Carlo like simulations are performed for each technique. In the simulations, the affect introduced uncertainty has on the measurement of thermal conductivity and thermal diffusivity is measured. From the results, it is recommended that the TLR should be used for measuring thermal conductivity and the FRR used for measuring thermal diffusivity. The TDDR and FDR were heavily affected by the uncertainty which resulted in inconsistent measured thermal properties. For measuring the thermal conductivity of molten salt, a needle probe was designed and manufactured to withstand the corrosive environment found in using molten salts. The probe uses modulated joule heating and measures the temperature rise in a thermocouple. The phase delay and temperature amplitude of the thermocouple are used in determining the thermal conductivity. A new thermal quadrupole based analytical solution, which takes into consideration convection and radiation, to the temperature rise of the probe is presented. The analytical solution is verified using a numerical solution found using COMSOL. Preliminary data was obtained with the probe in water.

Gas Turbine manufacturers strive for increased operating temperatures of gas turbine engines to improve efficiency and performance. One method of increasing the temperature beyond material limits is by applying thermal barrier coatings (TBCs) to hot section components. TBCs provide a thermal gradient between the hot gases and metallic substrate, and allow an increase in turbine inlet temperatures of 100-150ºC. However, spallation of TBCs can cause catastrophic failure of turbine engines by incipient melting of the substrate. To prevent such an occurrence, non-destructive evaluation (NDE) techniques are critical for quality control, health monitoring, and life assessment of TBCs. Two techniques in development for this purpose are thermal wave imaging (TWI) and photostimulated luminescence (PL) spectroscopy. TWI is a promising NDE technique with the ability to detect integrity and thickness of TBCs. In this study, TWI was employed as an NDE technique to examine as-coated TBCs with varying thicknesses, and thermally-cycled TBCs for initiation and progression of subcritical-subsurface damage as a function of thermal cycling. TWI and thermal response amplitude were correlated to the microstructural characteristics and damage progression of TBCs based on phenomenological expressions of thermal diffusion. The TBC specimens examined consisted of air plasma sprayed ZrO2 - 7wt.% Y2O3 on NiCoCrAlY bond coats with Haynes 230 superalloy substrate. As-coated specimens of varying thicknesses were evaluated by TWI to examine its applicability as a thickness measurement tool. It was found that heat dissipation through the TBC following pulsed excitation by xenon flash lamps initially followed the 1-D law of conduction and deviated from it as a function of thickness and time. The deviation resulted from quick dissipation of heat into the conductive metallic substrate. Therefore, with calibration, TWI can be used as a tool for YSZ thickness measurements of APS TBCs in the as-coated condition for quality control measures. Specimens of uniform thickness were evaluated as a function of thermal cyclic oxidation for subcritical-subsurface damage detection. Thermal cycling was carried out in air with 30-minute heat-up, 10-hour dwell at 1150°C, 30-minute air-quench and 1-hour hold at room temperature. During thermal cycling, TBC specimens were evaluated non-destructively by TWI at room temperature every 10 to 20 thermal cycles, and selected specimens were removed from thermal cycling for microstructural analysis by scanning electron microscopy (SEM). Higher thermal response amplitude associated with disrupted heat transfer was observed where localized spallation at or near the YSZ/TGO interface occurred. The health of the TBC was monitored by a rise in thermal response amplitude which may indicate a coalescence of microcracks to a detectable level. PL has been developed to measure stress, and detect subsurface damage and polymorphic transformation within the thermally grown oxide (TGO) of TBCs. PL was employed in this study as an NDE technique for TBCs to correlate subsurface damage as a function of thermal cyclic oxidation. The TBCs consisted of ZrO2 – 7 wt.% Y2O3 applied by electron beam physical vapor deposition with an as-coated (Ni,Pt)Al bond coat on a CMSX-4 superalloy substrate. Specimens were thermally cycled with a 10 minute ramp to a peak temperature of 1121°C, 40 minute hold at peak temperature, and 10 minute forced air quench. The TBCs were periodically removed from thermal cycling for NDE using PL until failure. Two specimens were removed from thermal oxidation after 10% and 70% of the average lifetime for microstructural analysis by SEM. During initial thermal cycling, metastable phases and polymorphic transformations of the Al2O3 scale were examined by PL. The polymorphic transformation from a metastable phase to equilibrium a-Al2O3 was detected. Since metastable phases are thought to be detrimental to coating lifetime, detection of these phases by PL can be used as a quality control tool. Nearing end-of-life, relief of the TGO from the compressive residual stress arising from thermal expansion mismatch was detected with PL and confirmed with microstructural analysis that revealed damage initiation (e.g. microcracking within the TGO scale parallel to the interfaces.) Rise in luminescence near the R-line frequency for polycrystalline a-Al2O3 without any residual stress (i.e. n = 14402 cm-1 and n = 14432 cm-1) corresponded to regions where cracked TGO was adhered to YSZ and not exposed to compressive stresses from thermal expansion mismatch upon cooling.

La microscopie thermique est un outil prometteur permettant d’étudier les mesures thermiques de matériaux et les mécanismes de transfert de chaleur aux micro/nanoéchelles. La réponse thermique de la sonde a été étudiée en utilisant deux sondes résistives : Wollaston et Palladium. Un modèle en 3D réaliste a été développé pour la sonde Wollaston et l’échantillon avec leur milieu environnant. La simulation de la sonde prend en compte son support et considère que le milieu environnant est convectif. La réponse de la sonde a été évaluée lors de l'approche vers un échantillon de cuivre. La comparaison avec les résultats expérimentaux montre que la prise en compte de la convection naturelle pour le milieu environnant est une hypothèse valide. Nous présentons ensuite une méthodologie pour étudier le signal thermique de la sonde en contact avec un échantillon nanostructuré. Pour cela, nous avons utilisé un échantillon composé de marches de silicium sous une couche de SiO2. SThM s'avère être un outil puissant pour effectuer l'imagerie sub-surfacique. Nous avons montré que le signal thermique obtenu par la sonde est influencé par la présence de structures internes et correspond à un volume sondé qui tient en compte les propriétés thermiques des matériaux. Avec notre modèle, nous avons pu reconstruire le profil expérimental obtenu par SThM. Pour la sonde en Palladium, la réponse de la sonde a été étudiée expérimentalement sous conditions ambiantes en mode alternatif. L'analyse des résultats a mis en évidence la présence d’un phénomène interpréter comme une résonance d'onde thermique qui prend place au micro/nanoéchelle. Ce phénomène est lié à la longueur de diffusion thermique du milieu environnant (air) et indépendant des propriétés thermiques de l'échantillon. / Scanning thermal microscopy is a promising tool to investigate material’s thermal measurements and heat transfer mechanisms at the micro/nanoscale. The probe thermal response was explored using two different resistive probes: Wollaston and Palladium probes. A 3D realistic model was developed for the Wollaston probe-sample system with their surrounding medium. The simulation of probe takes into account its holder and considers that the surrounding medium between the probe and the sample is convective. The probe’s response was evaluated during the approach toward a sample of copper. The comparison with experimental results showed that considering natural air convection for the surrounding medium is a valid assumption. We then present a methodology to characterize the thermal signal of probe in contact with a nanostructured sample. For that, we used a sample composed of buried silicon steps under SiO2. SThM proves to be a powerful tool to perform subsurface imaging. We showed that the thermal signal obtained by the probe is influenced by the presence of internal structures and corresponds to a scanned volume which takes into account material’s thermal properties. With our modelling, we was able to rebuild the experimental profile obtained by SThM. For the Palladium probe, the probe’s response was studied experimentally under ambient conditions in the AC mode for different frequencies. The analysis of the results pointed on a phenomenon which can be described as a thermal wave resonance which takes place at micro/nanoscale. This phenomenon was shown to be related to the thermal diffusion length of the surrounding medium (air) and independent of the sample thermal properties.

Poor heat and mass transfer inside the adsorbent bed of thermal wave adsorption cooling cycles cause low system performance and is an important problem in the adsorbent bed design. In this thesis, a new adsorbent bed is designed, constructed and tested to increase the heat and mass transfer in the adsorbent bed. The adsorbent bed is constructed from a finned tube in order to enhance the heat transfer. Additionally, the finned bed geometry is theoretically modeled and the model is solved time dependently by using Comsol Multiphysics software program. The distributions of dependent variables, i.e. temperature, pressure and amount adsorbed, are simulated and plotted in Comsol Multiphysics. In the model, the dependent variables are computed by solving the energy, mass and momentum transfer equations in a coupled way and their variations are investigated two-dimensionally. The results are presented with multicolored plots in a 2-D domain. Furthermore, a parametric study is carried out for determining factors that enhance the heat and mass transfer inside the adsorbent bed. In this parametric study, the effects of several design and operational parameters on the dependent variables are investigated. In the experimental study, the finned tube is tested using natural zeolite-water and silica gel-water working pairs. Temperature, pressure and amount adsorbed variations inside the adsorbent bed at various operating conditions are investigated. After that, a second adsorbent bed with a larger size is constructed and tested. The effect of the particle diameter of the adsorbent is also investigated. The experimental and theoretical results are compared.