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<p dir="ltr">Thermal Barrier Coatings (TBC) represent the key technology enabling greater efficiency and performance in jet engines and gas turbines. In modern engines, TBCs allow gas temperatures to exceed 1700°C, well above the point at which the structural alloys lose their strength. By insulating the underlying nickel-alloy components from the extreme heat generated during combustion, TBCs support a larger temperature gradient. </p><p dir="ltr">As operating temperatures are further increased to improve performance, thermal radiation becomes a more substantial carrier of heat. However, conventional TBCs are designed to provide a single barrier against only the phonon-mediated conductive heat flux, leaving the photonic radiative heat transfer largely unmitigated. We propose a Thermal Dual Barrier Coating (TDBC) to simultaneously suppress the phononic and photonic heat transfer by integrating a reflective thermal metamaterial into an independent phonon-optimized TBC.</p><p dir="ltr">The main obstacle to achieving the TDBC is in the selection of adequate reflective materials in the metamaterial. Conventional refractory metals that demonstrate the greatest stability and functionality in thermal metamaterials show instability under harsher environments. In our work, we identified and studied the key ideas, metrics, and challenges in metamaterials based on alternating layers of refractory metals and oxides for TDBC applications.</p><p dir="ltr">Our work emphasizes oxidation as a crucial degradation factor that is unavoidable in our assessment of the metamaterials. In formulating this problem, we bring the concept of oxidation-resistance through passivation to the forefront of material selection. We emphasize the passivative and oxidative properties of the metallic layer as a critical determinant in overall stability. In our work, we assess the enhancements in stability brought via passivation through the Pilling-Bedworth Ratio. We then propose the use of metal silicides in metamaterials as an overlooked class of oxidation-resistant IR reflective materials that operate through a more complex passivation method. We demonstrate strong stability in the structural integrity as well as the infrared responses of the metamaterials at up to 1200°C in atmospheric and oxidative environments.</p><p dir="ltr">After establishing the viability of metal silicides in wide-area thin films, we explore their viability in more complex thermal structures. We fabricate metal silicide metasurfaces for directional thermal emission. We demonstrate a grating structure that exhibits enhanced structural stability and maintains directional modes in the mid-IR after annealing at 1000°C.</p>

The re-entry space vehicles encounter high temperatures when they enter the earth atmosphere and the high temperature air in the shock layer around the body undergoes partial dissociation. Also, the gas molecules injected into the shock layer from the ablative thermal protection system (TPS) undergo pyrolysis which helps in reducing the net heat flux to the vehicle surface. The chemical species due to the pyrolysis add complexity to the stagnation flow chemistry (52 chemical reactions) models which include species like NOx, CO and hydrocarbons (HCs). Although the ablative TPS is responsible for the safety of re-entry space vehicle, the induced chemical species result in variety of adverse effects on environment such as global warming, acid rain, green house effect etc. The well known three-way-catalyst (TWC) involves simultaneous removal of all the three gases (i.e, NOx, CO, Hydrocarbons) present in the shock layer. Interaction of such three-way-catalyst on the heat shield materials or on the wall of the re-entry space vehicle is to reduce the heat flux and to remove the gases in the shock layer, which is an important issue. For the re-entry vehicle the maximum aerodynamic heating occurs at an altitude ranging about 68 to 45 km during which the vehicle is surrounded by high temperature dissociated air. Then the simplest real gas model of air is the five species model which is based on N2, O2, O, NO and N. This five species model assumes no ionization and no pyrolysis gases are emitted from the heat shield materials. The experimental research work presented in this thesis is directed towards the understanding of catalytic and non-catalytic surface reactions on high temperature materials in presence of strong shock heated test gas. We have also explored the possibility of using shock tube as a high enthalpy device for synthesis of new materials. In the first Chapter, we have presented an overview of re-entry space vehicles, thermal protection system (TPS) and importance of real gas effects in the shock layer. Literature survey on TPS, ablative materials and aerothermochemistry at the stagnation point of reentry capsule, in addition to catalytic and non-catalytic surface reactions between the wall and dissociated air in the shock layer are presented. In Chapters 2 and 3, we present the experimental techniques used to study surface reactions on high temperature materials. A brief description of HST2 shock tunnel is presented and this shock tunnel is capable of generating flow stagnation enthalpies ranging from 0.7 to 5 MJ/kg and has an effective test time of ~ 800 µs. High speed data acquisition system (National Instruments and Yokogawa) used to acquire data from shock tube experiments. The experimental methods like X-ray Photoelectron Spectroscopy (XPS), Scanning Electron Microscopy (SEM), X-ray diffraction (XRD), Raman and FTIR spectroscopy have been used to characterize the shock-exposed materials. Preliminary research work on surface nitridation of pure metals with shock heated nitrogen gas is discussed in Chapter 2. Surface nitridation of pure Al thin film with shock heated N2 is presented in Chapter 3. An XPS study shows that Al 2p peak at 74.2 eV is due to the formation AlN on the surface of Al thin film due to heterogeneous non-catalytic surface reaction. SEM results show changes in surface morphology of AlN film due to shock wave interaction. Thickness of AlN film on the surface increased with the increase in temperature of the shock heated nitrogen gas. However, HST2 did not produce sufficient temperature and pressure to carry out real conditions of re-entry. Therefore design and development of a new high enthalpy shock tunnel was taken up. In Chapter 4, we present the details of design and fabrication of free piston driven shock tunnel (FPST) to generate high enthalpy test gas along with the development of platinum (Pt) and thermocouple sensors for heat transfer measurement. A free piston driven shock tunnel consists of a high pressure gas reservoir, compression tube, shock tube, nozzle, test section and dump tank connected to a vacuum pumping system. Compression tube has a provision to fill helium gas and four ports, used to mount optical sensors to monitor the piston speed and pressure transducer to record pressure at the end of the compression tube when the piston is launched. Piston can attain a maximum speed of 150 m/s and compress the gas inside the compression tube. The compressed gas bursts the metal diaphragm and generates strong shock wave in the shock tube. This tunnel produces total pressure of about 300 bar and temperature of about 6000 K and is capable of producing a stagnation enthalpy up to 45 MJ/kg. The calibration of nozzle was carried out by measuring the pitot tube pressure in the dump tank. Experimentally recorded P5 pressure at end of the shock tube is compared with Numerical codes. Calibrated pressure P5 values are used to calculate the temperature T5 of the reflected shock waves. This high pressure and high temperature shock heated test gas interacts with the surface of the high temperature test materials. For the measurement of heat transfer rate, platinum thin film sensors are developed using DC magnetron sputtering unit. Hard protective layer of aluminum nitride (AlN) on Pt thin film was deposited by reactive DC magnetron sputtering to measure heat transfer rate in high enthalpy tunnel. After the calibration studies, FPST is used to study the heat transfer rate and to investigate catalytic/non-catalytic surface reaction on high temperature materials. In Chapter 5, an experimental investigation of non-catalytic surface reactions on pure carbon material is presented. The pure carbon C60 films and conducting carbon films are deposited on Macor substrate in the laboratory to perform shock tube experiments. These carbon films were exposed to strong shock heated N2 gas in the shock tube portion of the FPST tunnel. The typical shock Mach number obtained is about 7 with the corresponding pressure and temperature jumps of about 110 bar and 5400 K after reflection at end of the shock tube. Shock exposed carbon films were examined by different experimental techniques. XPS spectra of C(1s) peak at 285.8 eV is attributed to sp2 (C=N) and 287.3 eV peak is attributed to sp3 (C-N) bond in CNx due to carbon nitride. Similarly, N(1s) core level peak at 398.6 eV and 400.1 eV observed are attributed to sp3-C-N and sp2-C=N of carbon nitride, respectively. SEM study shows the formation of carbon nitride crystals. Carbon C60 had melted and undergone non-catalytic surface reaction with N2 while forming carbon nitride. Similar observations were made with conducting carbon films but the crystals were spherical in shape. Micro Raman and FTIR study gave further evidence on the formation of carbon nitride film. This experimental investigation confirms the formation of carbon nitride in presence of shock-heated nitrogen gas by non-catalytic surface reaction. In Chapters 6 and 7, we present a novel method to understand fully catalytic surface reactions after exposure to shock heated N2, O2 and Ar test gas with high temperature materials. We have employed nano ZrO2 and nano Ce0.5Zr0.5O2 ceramic high temperature materials to investigate surface catalytic reactions in presence of shock heated test gases. These nano crystalline oxides are synthesized by a single step solution combustion method. Catalytic reaction was confirmed for both powder and film samples of ZrO2. As per the theoretical model, it is known that the catalytic recombination reaction produces maximum heating on the surface of re-entry space vehicles. This was demonstrated in this experiment when a metastable cubic ZrO2 changed to stable monoclinic ZrO2 phase after exposure to shock waves. The change of crystal structure was seen using XRD studies and needle type monoclinic crystal growth with aspect ratio (L/D) more than 15 was confirmed by SEM studies. XPS of Zr(3d) core level spectra show no change in binding energy before and after exposure to shock waves, confirming that ZrO2 does not change its chemical nature, which is the signature of catalytic surface reaction. When a shock heated argon gas interacted with Ce0.5Zr0.5O2 compound, there was a change in colour from pale yellow to black due to reduction of the compound, which is the effect of heat transfer from the shock wave to the compound in presence of argon gas. The reduction reaction shows the release of oxygen from the compound due to high temperature interaction. The XPS of Ce(3d) and Zr(3d) spectra confirm the reduction of both Ce and Zr to lower valent states. The oxygen storage and release capacity of the Ce0.5Zr0.5O2 compound was confirmed by analyzing the reduction of Ce4+ and Zr4+ with high temperature gas interaction. When Ce0.5Zr0.5O2 (which is same as Ce2Zr2O8) in cubic fluorite structure was subjected to strong shock, it changed to pyrochlore (Ce2Zr2O7) structure by releasing oxygen and on further heating it changed to Ce2Zr2O6.3 which is also crystallized in pyrochlore structure by further releasing oxygen. If this heating is carried out in presence of argon test gas, fluorite structure can easily change to pyrochlore Ce2Zr2O6.3 structure, which is a good electrical conductor. Due to its oxygen storage capability (OSC) and redox (Ce4+/Ce3+) properties, Ce0.5Zr0.5O2 had been used as oxygen storage material in three-way-catalyst. Importance of these reactions is that the O2 gas released from the compound will react with gas released from the heat shield materials, like NOx, CO and hydrocarbon (HCs) species which results in reduction of temperature in the shock layer of the re-entry space vehicle. The compound Ce0.5Zr0.5O2 changes its crystal structure from fluorite to pyrochlore phase in presence of shock heated test gas. The results presented in these two Chapters are first of their kind, which demonstrates the surface catalytic reactions. In Chapter 8, we present preliminary results of the oxygen recombination on the surface of heat shield material procured from Indian Space Research Organization (ISRO) used as TPS in re-entry space capsule (Space capsule Recovery Experiment SRE-1) and on thin film SiO2 deposited on silicon substrate. The formation of SiO between the junctions of SiO2/Si was confirmed using XPS study when shock exposed oxygen reacted on these materials. The surface morphology of the ablated SiO2 film was studied using SEM. The damage induced due to impact of shock wave in presence of oxygen gas was analyzed using Focused Ion Beam (FIB) microscope. The results reveal the damage on the surface of SiO2 film and also in the cross-section of the film. We are further investigating use of FIB, particularly related to residual stress developed on thin films due to high pressure and high temperature shock wave interaction. In Chapter 9, conclusions on the performance of FPST, synthesis of high temperature materials, catalytic and non-catalytic surface reactions on the high temperature material due to shock-heated test gases are presented. Possible scope for future studies is also addressed in this Chapter.

<p>Additive manufacturing of gun propellants is an emerging and promising field which addresses the limitations of conventional manufacturing techniques. Gun propellants are manufactured using wetted extrusion, which uses volatile solvents and dies of limited and constant geometries. On the other hand, additive techniques are faced with the challenges of maintaining the gun propellant’s energetic content as well as its structural integrity during high pressure combustion. The work presented in this thesis demonstrates the feasibility of producing functioning gun propellant grains using vibration-assisted 3D printing, a novel method which has been shown to extrude extremely viscous materials such as clays and propellant pastes. At first, the technique is compared to screw-driven additive methods which have been used in printing gun propellant pastes with slightly lower energetic content. In chapter two, diethylene glycol dinitrate (DEGDN), a highly energetic plasticizer, was investigated due to its potential to replace nitroglycerin in double base propellants with high nitroglycerin content. A novel isoconversional method was applied to analyze its decomposition kinetics. The ignition and lifetime values of diethylene glycol dinitrate were obtained using the new isoconversional method, in order to assess the safety of using the plasticizer in a modified double base propellant. In chapter three, a modified double base propellant (M8D) containing DEGDN was additively manufactured using VAP. The printed strands had little to no porosity, and their density was nearly equal to the theoretical maximum density of the mixture. The strands were burned at high pressures in a Crawford bomb and the burning was visualized using high speed cameras. The burning rate equation as a function of the M8D propellant as a function of pressure was obtained. Overall, this work shows that VAP is capable of printing highly energetic gun propellants with low solvent content, low porosity, with high printing speeds, and which have consistent burning characteristics at high pressures. </p>

<p>  </p> <p>There has been a growing interest within the aerospace industry for shifting towards a digital twin approach, for reliable assessment of individual components during the product lifecycle - across design, manufacturing, and in-service maintenance, repair & overhaul (MRO) stages. The transition towards digital twins relies on continuous updating of the product lifecycle datasets and interoperable exchange of data applicable to components, thereby permitting engineers to utilize current state information to make more-informed downstream decisions. In this thesis, we primarily develop a framework to store, track, update, and retrieve product lifecycle data applicable to a serialized component, its features, and individual locations. </p> <p>From a structural integrity standpoint, the fatigue performance of a component is inherently tied to the component geometry, its material state, and applied loading conditions. The manufacturing process controls the underlying material microstructure, which in turn governs the mechanical properties and ultimately the performance. The processing also controls the residual stress distributions within the component volume, which influences the durability and damage tolerance of the component. Hence, we have demonstrated multiple use cases for fatigue life assessment of critical aerospace components, by using the developed framework for efficiently tracking and retrieving (i) the current geometric state, (ii) the material microstructure state, and (iii) residual stress distributions.</p> <p>Model-based definitions (MBDs) present opportunities to capture both geometric and non-geometric data using 3D computer-aided design (CAD) models, with the overarching aim to disseminate product information across different stages of the lifecycle. MBDs can potentially eliminate error-prone information exchange associated with traditional paper-based drawings and improve the fidelity of component details, captured using 3D CAD models. However, current CAD capabilities limit associating the material information with the component’s shape definition. Furthermore, the material attributes of interest, viz., material microstructures and residual stress distributions, can vary across the component volume. To this end, in the first part of the thesis, we implement a CAD-based tool to store and retrieve metadata using point objects within a CAD model, thereby creating associations to spatial locations within the component. The tool is illustrated for storage and retrieval of bulk residual stresses developed during the manufacturing of a turbine disk component, acquired from process modeling and characterization. Further, variations in residual stress distribution owing to process model uncertainties have been captured as separate instances of the disk’s CAD models to represent part-to-part variability as an analogy to track individual serialized components for digital twins. The propagation of varying residual stresses from these CAD models within the damage tolerance analysis performed at critical locations in the disk has been demonstrated. The combination of geometric and non-geometric data inside the MBD, via storage of spatial and feature varying information, presents opportunities to create digital replica or digital twin(s) of actual component(s) with location-specific material state information.</p> <p>To fully realize a digital twin description of components, it is crucial to dynamically update information tied to a component as it evolves across the lifecycle, and subsequently track and retrieve current state information. Hence, in the second part of the thesis, we propose a dynamic data linking approach to include material information within the MBDs. As opposed to storing material datasets directly within the CAD model in the previous approach, we externally store and update the material datasets and create data linkages between material datasets and features within the CAD models. To this end, we develop a model-based feature information network (MFIN), a software agnostic framework for linking, updating, searching, and retrieving of relevant information across a product’s lifecycle. The use case of a damage tolerance analysis for a compressor bladed-disk (blisk) is demonstrated, wherein Ti-6Al-4V blade(s) are linear friction welded to the Ti-6Al-4V disk, comprising well-defined regions exhibiting grain refinement and high residuals stresses. By capturing the location-specific microstructural information and residual stress fields at the weld regions, this information was accessed within the MFIN and used for downstream damage tolerant analysis. The introduction of the MFIN framework facilitates access to dynamically evolving as well as location-specific data for use within physics-based models.</p> <p>In the third part of thesis, we extend the MFIN framework to enable a physics-based, microstructure sensitive and location-specific fatigue life analysis of a component. Traditionally, aerospace components are treated as monolithic structures during lifing, wherein microstructural information at individual locations are not necessarily considered. The resulting fatigue life estimates are conservative and associated with large uncertainty bounds, especially in components with gradient microstructures or distinct location-specific microstructures, thereby leading to under usage of the component’s capabilities. To improve precision in the fatigue estimates, a location-specific lifing framework is enabled via MFIN, for tracking and retrieval of microstructural information at distinct locations for subsequent use within a crystal plasticity-based fatigue life prediction model. A use case for lifing dual-microstructure heat treated LSHR turbine disk component is demonstrated at two locations, near the bore (fine grains) and near the rim (coarse grains) regions. We employ the framework to access (a) the grain size statistics and (b) the macroscopic strain fields to inform precise boundary conditions for the crystal plasticity finite-element analysis. The illustrated approach to conduct a location-specific predictive analysis of components presents opportunities for tailoring the manufacturing process and resulting microstructures to meet the component’s targeted requirements.</p> <p>For reliably conducting structural integrity analysis of a component, it is crucial to utilize their precise geometric description. The component geometries encounter variations from nominal design geometries, post manufacturing or after service. However, traditionally, stress analyses are based on nominal part geometries during assessment of these components. In the last part of the thesis, we expand the MFIN framework to dynamically capture deviations in the part geometry via physical measurements, to create a new instance of the CAD model and the associated structural analysis. This automated workflow enables engineers for improved decision-making by assessing (i) as-manufactured part geometries that fall outside of specification requirements during the materials review board or (ii) in-service damages in parts during the MRO stages of the lifecycle. We demonstrate a use case to assess the structural integrity of a turbofan blade that had experienced foreign object damage (FOD) during service. The as-designed geometry was updated based on coordinate measurements of the damaged blade surfaces, by applying a NURBS surface fit, and subsequently utilized for downstream finite-element stress analysis. The ramifications of the FOD on the local stresses within the part are illustrated, providing critical information to the engineers for their MRO decisions. The automated flow of information from geometric inspection within structural analysis, enabled by MFIN, presents opportunities for effectively assessing products by utilizing their current geometries and improving decision-making during the product lifecycle.</p>

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<p>This work focuses on the collection and analysis of Lithium-ion battery operational and temperature data during nail penetration testing through two different experimental approaches. Raman spectroscopy, machine learning, and internal temperature sensors are used to collect and analyze data to further investigate the effects on cell operation during and after nail penetrations, and the feasibility of using this data to predict future performance.</p> <p><br></p> <p>The first section of this work analyzes the effects on continued operation of a small Lithium-ion prismatic cell after nail penetration. Raman spectroscopy is used to examine the effects on the anode and cathode materials of cells that are cycled for different amounts of time after a nail puncture. Incremental capacity analysis is then used to corroborate the findings from the Raman analysis. The study finds that the operational capacity and lifetime of cells is greatly reduced due to the accelerated degradation caused by loss of material, uneven current distribution, and exposure to atmosphere. This leads into the study of using the magnitude and corresponding voltage of incremental capacity peaks after nail puncture to forecast the operation of damaged cells. A Gaussian process regression is used to predict discharge capacity of different cells that experience the same type of nail puncture. The results from this study show that the method is capable of making accurate predictions of cell discharge capacity even with the higher rate of variance in operation after nail puncture, showing the method of prediction has the potential to be implemented in devices such as battery management systems.</p> <p><br></p> <p>The second section of this work proposes a method of inserting temperature sensors into commercially-available cylindrical cells to directly obtain internal temperature readings. Characterization tests are used to determine the effect on the operability of the modified cells after the sensors are inserted, and lifetime cycle testing is implemented to determine the long-term effects on cell performance. The results show the sensor insertion causes a small reduction in operational performance, and lifetime cycle testing shows the cells can operate near their optimal output for approximately 100-150 cycles. Modified cells are then used to monitor internal temperatures during nail penetration tests and how the amount of aging affects the temperature response. The results show that more aging in a cell causes higher temperatures during nail puncture, as well as a larger difference between internal and external temperatures, due mostly to the larger contribution of Joule heating caused by increased internal resistance.</p>

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