Doctor of Philosophy / Food Science Institute -- Animal Science & Industry / J. Scott Smith / A rapid direct solvent extraction method for the extraction of 2-dodecylcyclobutanone (2-DCB) in irradiated beef using acetonirile was developed and evaluated. The 2-DCB in commercially irradiated ground beef patties was extracted with n-hexane by using a Soxhlet apparatus or with acetonitrile via direct solvent extraction. The hexane and the acetonitrile extracts were evaporated to dryness. Then, the fat in the hexane extract was removed with filtration by standing at -20 °C after the addition of a mixture of ethylacetate and acetonitrile. The defatted extract as well as the acetonitrile extract were purified with a 1 g silica cartridge and was injected into a gas chromatography-mass spectrometry (GC-MS). The 2-DCB concentration in irradiated patties was 0.031 ± 0.0026 ppm (n = 5) for the Soxhlet method and 0.031 ± 0.0025 ppm (n = 10) for direct solvent extraction. The effect of low-energy X-rays on the formation of 2-DCB was investigated in frozen ground beef. Beef patties (85/15) were irradiated by low-energy X-rays and gamma rays at 3 targeted doses of 1.5, 3.0, and 5.0 kGy. The 2-DCB was extracted with n-hexane by using a Soxhlet apparatus and analyzed by GC-MS. There was no significant difference in 2-DCB concentration between gamma-ray- and low-energy X-ray-irradiated patties at all targeted doses. The metabolism of 2-DCB was investigated in vitro and in vivo. The incubation mixture from the in vitro study was extracted with n-hexane by using a Soxhlet apparatus and injected into a GC-MS). The hexane extract from the in vitro study and of rat feces was also derivatized with a silylation reagent and injected into a GC-MS. The average percentage of 2-DCB recovered from the test incubations (2-DCB with S9 and NADPH) was 23%, compared with 50% from the controls (2-DCB in buffer). The GC-MS chromatograms of the derivatized samples showed that 2-DCB was metabolized to 2-dodecylcyclobutanol.

This research work has contributed in various ways to help develop a better understanding of textile composites and materials with complex microstructures in general. An instrumental part of this work was the development of an object-oriented framework that made it convenient to perform multiscale/multiphysics analyses of advanced materials with complex microstructures such as textile composites. In addition to the studies conducted in this work, this framework lays the groundwork for continued research of these materials. This framework enabled a detailed multiscale stress analysis of a woven DCB specimen that revealed the effect of the complex microstructure on the stress and strain energy release rate distribution along the crack front. In addition to implementing an oxidation model, the framework was also used to implement strategies that expedited the simulation of oxidation in textile composites so that it would take only a few hours. The simulation showed that the tow architecture played a significant role in the oxidation behavior in textile composites. Finally, a coupled diffusion/oxidation and damage progression analysis was implemented that was used to study the mechanical behavior of textile composites under mechanical loading as well as oxidation. A parametric study was performed to determine the effect of material properties and the number of plies in the laminate on its mechanical behavior. The analyses indicated a significant effect of the tow architecture and other parameters on the damage progression in the laminates.

Cette thèse porte sur l'étude de la durée de vie de composants et modules de puissance dans des environnements thermiques sévères, lorsque les modules de puissance sont amenés à travailler à haute température ou sous des cycles de température de forte amplitude. Les domaines visés par cette étude concernent plus particulièrement des applications extrêmement contraignantes telles que les applications aéronautiques. Un module de puissance est un assemblage de plusieurs matériaux (semi-conducteurs, brasures, céramiques, conducteurs) présentant des propriétés mécaniques, notamment de coefficient de dilatation thermiques (CTE) différentes. Les pertes dans les puces actives et les variations de température ambiante (profils de mission) sont responsables de contraintes mécaniques liées aux différences de CTE entre les différents matériaux. Les modes de défaillance étant principalement d'origine mécanique, ces travaux ont été effectués entre le SATIE et le LMT (Institut Farman). L'étude mécanique a complété des travaux expérimentaux de caractérisation et de vieillissement accéléré de modules de puissance à semi-conducteur. Ces études ont nécessité la mise en place d'essais de vieillissement spécifiques, passifs (utilisation d'une étuve permettant de contraindre les assemblages de puissance sous des cycles thermiques de grande amplitude) et actifs (utilisation de régimes extrêmes de fonctionnement tels que le court-circuit pour accélérer le vieillissement de certaines parties de l'assemblage).La première partie de ce manuscrit présente les principes physiques mis en jeu. Nous présenterons succinctement les concepts de mécanique de la rupture ainsi que les couplages physiques.La deuxième partie porte sur la rupture de la céramique des substrats DCB. Cette rupture peut provenir de défauts répartis aléatoirement dans le matériau. Nous aborderons le problème par une approche statistique où nous introduirons la "Théorie du maillon faible". L'autre cause de rupture est la présence de défauts géométriques que l'on appelle singularité où il existe une concentration des contraintes nécessitant une approche déterministe. A cette occasion nous introduirons le facteur d'intensité des contraintes qui permet d'étudier les problèmes de rupture liés à des zones singulières.La dernière partie portera sur la dégradation de la métallisation du transistor. La recherche d'indicateurs de vieillissement a demandé la mise au point de différents bancs de caractérisation électrique pour la mesure fine de différentes grandeurs électriques (courants de fuite, tensions de seuil, chute de tension à l'état passant...) dans un environnement thermique contrôlé. De plus ces caractérisations électriques sont corrélées à des observations de la métallisation effectuées par un microscope électronique à balayage de manière régulière. Nous chercherons à montrer comment la modification de la morphologie de la métallisation peut modifier les caractéristiques électriques des transistors de puissance testés.

This thesis is intended to identify the mode I and mode II fracture toughness to characterize the thin laminate interface by using the Double Cantilever Beam test (DCB) and End Notched Flexure test (ENF). This study’s thin laminate was Polyethylene Terephthalate and Low-Density Polyethylene (PET-LDPE), which is mostly used by packaging industries in the manufacturing of packages to store liquid food. As PET-LDPE film is very flexible and difficult to handle, DCB and ENF tests cannot be performed directly so, sheet metal (Aluminium) was used as carrier material. PET-LDPE film is placed between two aluminum plates to reduce the flexibility and perform the tests. Therefore, the Aluminium plate was also studied to find the constitutive parameters (young’s modulus (E) and mixed hardening parameters (Plastic properties)) under the tensile test and three-point bending test. From the test response, energy release rate calculation has been done for different Pre-crack lengths to validate the DCB and ENF experimental setup, study the different Pre-crack lengths, and characterize the laminate interface. Finite Element simulation (FE simulation) for those tests were carried out in AbaqusTM2020. When needed, the force versus displacement response from FE simulation was optimized against experimental response to find the required constitutive parameters (Young’s modulus, Hardening parameters, and PET-LDPE material properties). Implementing of optimization algorithm and automated simulation has been done with the help of MATLAB code. In contrast, MATLAB works as a server, and Abaqus works as a client and connected two interfaces to run the optimization. The results obtained from experiments and FE simulations were compared to the results found in the literature.

In dieser Arbeit werden Postprocessing-Verfahren zum Steigern der Genauigkeit und Verfügbarkeit satellitengestützer Positionierungsverfahren, die ohne Inertialsensorik auskommen, untersucht. Ziel ist es, auch unter schwierigen Empfangsbedingungen, wie sie in urbanen Gebieten herrschen, eine Trajektorie zu erzeugen, deren Genauigkeit sie als Referenz für andere Verfahren qualifiziert. Zwei Ansätze werdenverfolgt: Die Verwendung von IGS-Daten sowie das Smoothing unter Einbeziehung von Sensoren aus der Fahrzeugodometrie. Es wird gezeigt, dass durch die Verwendung von IGS-Daten eine Verringerung des Fehlers um 50% bis 70% erreicht werden kann. Weiterhin demonstrierten die Smoothing-Verfahren, dass sie in der Lage sind, auch unter schlechten Empfangsbedingungen immer eine Genauigkeit im Dezimeterbereich zu erzielen.

Structural adhesives are widely used with great success, and yet occasional failures can occur, often resulting from improper bonding procedures or joint design, overload or other detrimental service situations, or in response to a variety of environmental challenges. In these situations, cracks can start within the adhesive layer or debonds can initiate near an interface. The paths taken by propagating cracks can affect the resistance to failure and the subsequent service lives of the bonded structures. The behavior of propagating cracks in adhesive joints remains of interest, including when some critical environments, complicated loading modes, or uncertainties in material/interfacial properties are involved. From a mechanics perspective, areas of current interest include understanding the growth of damage and cracks, loading rate dependency of crack propagation, and the effect of mixed mode fracture loading scenarios on crack path selection. This dissertation involves analytical, numerical, and experimental evaluations of crack propagation in several adhesive joint configurations. The main objective is an investigation of crack path selection in adhesively bonded joints, focusing on in-plane fracture behavior (mode I, mode II, and their combination) of bonded joints with uniform bonding, and those with locally weakened interfaces. When removing cured components from molds, interfacial debonds can sometimes initiate and propagate along both mold surfaces, resulting in the molded product partially bridging between the two molds and potentially being damaged or torn. Debonds from both adherends can sometimes occur in weak adhesive bonds as well, potentially altering the apparent fracture behavior. To avoid or control these multiple interfacial debonding, more understanding of these processes is required. An analytical model of 2D parallel bridging was developed and the interactions of interfacial debonds were investigated using Euler-Bernoulli beam theory. The numerical solutions to the analytical results described the propagation processes with multiple debonds, and demonstrated some common phenomena in several different joints corresponding to double cantilever beam configurations. The analytical approach and results obtained could prove useful in extensions to understanding and controlling debonding in such situations and optimization of loading scenarios. Numerical capabilities for predicting crack propagation, confirmed by experimental results, were initially evaluated for crack behavior in monolithic materials, which is also of interest in engineering design. Several test cases were devised for modified forms of monolithic compact tension specimens (CT) were developed. An asymmetric variant of the CT configuration, in which the initial crack was shifted to two thirds of the total height, was tested experimentally and numerically simulated in ABAQUS®, with good agreement. Similar studies of elongated CT specimens with different specimen lengths also revealed good agreement, using the same material properties and cohesive zone model (CZM) parameters. The critical specimen length when the crack propagation pattern abruptly switches was experimentally measured and accurately predicted, building confidence in the subsequent studies where the numerical method was applied to bonded joints. In adhesively bonded joints, crack propagation and joint failure can potentially result from or involve interactions of a growing crack with a partially weakened interface, so numerical simulations were initiated to investigate such scenarios using ABAQUS®. Two different cohesive zone models (CZMs) are applied in these simulations: cohesive elements for strong and weak interfaces, and the extended finite element method (XFEM) for cracks propagating within the adhesive layer. When the main crack approaches a locally weakened interface, interfacial damage can occur, allowing for additional interfacial compliance and inducing shear stresses within the adhesive layer that direct the growing crack toward the weak interface. The maximum traction of the interfacial CZM appears to be the controlling parameter. Fracture energy of the weakened interface is shown to be of secondary importance, though can affect the results when particularly small (e.g. 1% that of the bulk adhesive). The length of the weakened interface also has some influence on the crack path. Under globally mixed mode loadings, the competition between the loading and the weakened interface affects the shear stress distribution and thus changes the crack path. Mixed mode loading in the opposite direction of the weakened interface is able to drive the crack away from the weakened interface, suggesting potential means to avoid failure within these regions or to design joints that fail in a particular manner. In addition to the analytical and numerical studies of crack path selection in adhesively bonded joints, experimental investigations are also performed. A dual actuator load frame (DALF) is used to test beam-like bonded joints in various mode mixity angles. Constant mode mixity angle tracking, as well as other versatile loading functions, are developed in LabVIEW® for use with a new controller system. The DALF is calibrated to minimize errors when calculating the compliance of beam-like bonded joints. After the corrections, the resulting fracture energies ( ) values are considered to be more accurate in representing the energy released in the crack propagation processes. Double cantilever beam (DCB) bonded joints consisting of 6061-T6 aluminum adherends bonded with commercial epoxy adhesives (J-B Weld, or LORD 320/322) are tested on the DALF. Profiles of the values for different constant mode mixity angles, as well as for continuously increasing mode mixity angle, are plotted to illustrate the behavior of the crack in these bonded joints. Finally, crack path selection in DCB specimens with one of the bonding surfaces weakened was studied experimentally, and rate-dependency of the crack path selection was found. Several contamination schemes are attempted, involving of graphite flakes, silicone tapes, or silane treatments on the aluminum oxide interfaces. In all these cases, tests involving more rapid crack propagation resulted in interfacial failures at the weakened areas, while slower tests showed cohesive failure throughout. One possible explanation of this phenomenon is presented using the rate-dependency of the yield stress (commonly considered to be corresponding to the maximum traction) of the epoxy adhesives. These experimental observations may have some potential applications tailoring adhesive joint configurations and interface variability to achieve or avoid particular failure modes. / Ph. D.

With continued feature size reduction in microelectronics and with more than a billion transistors on a single integrated circuit (IC), on-chip interconnection has become a challenge in terms of processing-, electrical-, thermal-, and mechanical perspective. Today’s high-performance ICs have on-chip back-end-of-line (BEOL) layers that consist of copper traces and vias interspersed with low-k dielectric materials. These layers have thicknesses in the range of 100 nm near the transistors and 1000 nm away from the transistors close to the solder bumps. In such BEOL layered stacks, cracking and/or delamination is a common failure mode due to the low mechanical and adhesive strength of the dielectric materials as well as due to high thermally-induced stresses. However, there are no available cohesive zone models and parameters to study such interfacial cracks in sub-micron thick microelectronic layers. This work focuses on developing framework based on cohesive zone modeling approach to study interfacial delamination in sub-micron thick layers. Such a framework is then successfully applied to predict microelectronic device reliability. As intentionally creating pre-fabricated cracks in such interfaces is difficult, this work examines a combination of four-point bend and double-cantilever beam tests to create initial cracks and to develop cohesive zone parameters over a range of mode-mixity. Similarly, a combination of four-point bend and end-notch flexure tests is used to cover additional range of mode-mixity. In these tests, silicon wafers obtained from wafer foundry are used for experimental characterization. The developed parameters are then used in actual microelectronic device to predict the onset and propagation of crack, and the results from such predictions are successfully validated with experimental data. In addition, nanoindenter-based shear test technique designed specifically for this study is demonstrated. The new test technique can address different mode mixities compared to the other interfacial fracture characterization tests, is sensitive to capture the change in fracture parameter due to changes in local trace pattern variations around the vicinity of bump and the test mimics the forces experienced by the bump during flip-chip assembly reflow process. Through this experimental and theoretical modeling research, guidelines are also developed for the reliable design of BEOL stacks for current and next-generation microelectronic devices.

In response to serious environmental and economic concerns, the design and production of aircrafts have been changing profoundly over the past decades with the nose-to-tail switch from metallic materials to lightweight composite materials such as carbon fibre reinforced plastic (CFRP). In this context, the present doctoral research work aimed to contribute to the development of a CFRP booster casing, a real innovation in the field initiated and conducted by Safran Aero Boosters. More specifically, this thesis addresses the matter of joining metal/CFRP hybrid structures, which are prone to possibly detrimental residual stresses.The issue is treated with an approach combining experimental characterisation and finite element (FE) simulations. The multi-layered system’s state of damage was systematically examined on hundreds of micrographs, and the outcome of this study is presented under the form of a statistical analysis. Further, the defects’ 3D morphology is investigated by incremental polishing. A number of thermal and mechanical properties are measured by diverse physical tests on part of the constituent materials, i.e. the aerospace grade RTM6 epoxy resin, the structural Redux 322 epoxy film adhesive, and AISI 316L stainless steel. They are used as input data in a FE model of the multilayer that is developed and progressively refined to obtain detailed residual stress fields after thermal loading. These results are compared to experimental data acquired by X-ray diffraction stress analysis and with the curvature-based Stoney formula. Cohesive elements are placed at specific locations within the FE model to allow simulating progressive damage. Peel tests, mode I, mode II and mixed mode I/II fracture tests are thus performed in view of measuring the joint toughness. The results of these tests are discussed and the presence of residual stress in the fracture specimens is highlighted. Key information for the calibration of the cohesive law is finally identified via inverse FE analysis of the mode I test, this being a significant step in the process of building a damage predictive FE model of the multi-layered system. / Doctorat en Sciences de l'ingénieur et technologie / info:eu-repo/semantics/nonPublished