Cette thèse a été motivée par l’étude d’un procédé innovant de production de substrats ultra-minces (d’épaisseur variant de 15 μm à 70 μm), basé sur l’implantation d’hydrogène à haute énergie, dans notre cas comprise entre 1MeV et 2.5MeV. Une telle implantation suivie d’un traitement thermique approprié, conduit au détachement d’un film mince autoporté, appelé « substrat ultra-mince ». L’intérêt de ce procédé de détachement est purement économique, car il ne génère presque aucune perte de matière première. Nous l’avons particulièrement utilisé pour produire des substrats ultra-minces de silicium (100), pour la production des cellules PV bas-coûts. Dans le but d’élargir les champs d’applications du procédé, le détachement de substrats ultra-minces de deux autres matériaux (le Ge et le SiC) très utilisés en électronique a aussi été étudié. Ainsi, dans cette étude, les paramètres optimaux d’implantation (énergie et fluence) et de recuits conduisant au détachement de grandes surfaces de Si(100) ont tout d’abord été investigués. Ensuite, l’application technologique du procédé proposé a été validée par la réalisation des cellules solaires au moyen des substrats ultrafins de Si détachés (50 μm et 70 μm d’épaisseur). Les performances PV obtenues ont été assez proches de celles obtenues avec une cellule référence réalisée sur un substrat standard. Par la suite, une étude détaillée faite par TEM et par FTIR sur les défauts étendus à différents stades de recuits a permis de mettre en lumière la nature et la distribution spatiale des défauts précurseurs de la fracture dans le Si après implantation à haute énergie. Enfin, des essais de détachements réalisés avec le Ge et le SiC, lesquels ont été comparés au cas du Si, ont permis d’en savoir plus sur les critères de détachement. En effet, plus le matériau sera rigide, i.e. plus il aura un module d’Young élevé, plus la fluence et la température de recuit nécessaires pour le détachement seront élevées. / The motivation of this thesis was the study of an innovative process for the production of ultra-thin substrates (with thicknesses between 15 μm and 70 μm), based on the high energy hydrogen implantation, in our case in the range of 1 MeV to 2.5 MeV. Such an implantation followed by an appropriate thermal annealing, lead to the delamination of a freestanding thin layer, that we call “ultra-thin substrate”. The benefit of this delamination process is purely economic, since almost no raw material is lost. We have particularly used this process to produce ultra-thin (100) Si substrates, for the production of low-cost PV solar cells. In order to extend the process application fields, the delamination of ultra-thin substrates of two other materials (Ge and SiC) widely used in electronics has been also studied. In our work, the optimal implantation parameters (energy and fluence) and thermal annealing, leading to the delamination of large areas of Si (100) were first investigated. Subsequently, in order to validate the technological application of our process, solar cells have been performed with ultra-thin silicon substrates delaminated, with thicknesses of 50 μm and 70 μm. Results of PV performances obtained were quite close to those obtained with a reference solar cell achieved on a standard substrate. After that, in order to highlight the nature and the spatial distribution of fracture precursor defects after high energy hydrogen implantation in silicon, which had not yet done so far the subject of specific studies, characterizations have been carried out at different annealing stages, by means of TEM and FTIR. Finally, delamination results obtained with Ge and SiC, which were compared to the case of Si, helped us to learn more about delamination criteria. Indeed, we observed that, as the material rigidity increase, i.e. as the Young modulus is higher, the fluence and temperature require for the delamination will be also high.

A functional nanometer-scale hybrid coating layer with multi-walled carbon nanotubes (MWCNTs) and/or nanoclays, as mechanical enhancement to ‘heal’ surface microcracks and environmental barrier layer is applied to alkaliresistant glass (ARG) fibres. The nanostructured and functionalised traditional glass fibres show both significantly improved mechanical properties and environmental corrosion resistance. Early warning material damage can be achieved by carbon nanotubes concentrated interphases in the composites. / Eine funktionale nanometerskalige Hybridbeschichtung mit multi-walled carbon nanotubes (MWCNTs) und/oder Nanoclay wurde als mechanische Verbesserung des „Ausheilens“ von Oberflächen-Mikrorissen und Barriereschicht gegenüber Umwelteinflüssen auf alkaliresistente Glasfasern (ARG) appliziert. Die nanostrukturierten und funktionalisierten traditionellen Glasfasern zeigen signifikant verbesserte mechanische Eigenschaften und Korrosionsbeständigkeit. Die Frühwarnung des Materialversagens kann durch Carbon Nanotubes, konzentriert in der Grenzschicht der Composites, erreicht werden.

This thesis deals with deterioration observed in cement-concrete cover (CBK) for three selected road sections of highways in the Czech Republic. The main objective was to determine whether concrete failure arose due to alkali-silica reaction, or other mechanism. The deterioration of concrete failure was observed in the macroscopic and microscopic scale. The mostly macroscopically observed deterioration of the concrete were cracks breaking the surface and inner parts of concrete. In micro- scale the microcracks and alcali-silica gels were observed. The CBK deterioration was quantitatively determined by three main parameters: specific length of microcracks on the CBK surface, specific length of microcracks in the drill cores and volume of alcali-silica gels and microcracks in thin sections. According to these indicators it was possible to distinguish two different types of CBK deteriorations. (1) Degradation mainly associated by alkali-silica reaction (observed on highways D11 - Vrbová Lhota and D1) and (2) degradation connected with another mechanism (cycles of freezing and thawing, mechanical degradation) was observed on the highway D5.

The main focus of this research is the transformation induced fatigue behavior of shape memory alloy (SMA) actuators undergoing thermally induced martensitic phase transformation. The recent development of aerospace applications employing shape memory alloys (SMAs) has expanded the need for fatigue life characterization and modeling. Lightweight, compact and with a great work output, SMAs are ideal materials for actuated structural components. However, fatigue life becomes a key factor in applications such as commercial airplanes. Therefore, it is necessary to not only perform fatigue testing but also to investigate the causes of fatigue failure. As a new class of materials, SMAs have unique characteristics and require novel test methodologies to conduct repeatable and reliable fatigue testing. For this research, two materials are being investigated: TiNiCu and Ni-rich NiTi. The experiments performed on the first selected alloy, i.e. TiNiCu SMA, explore three major parameters: the applied stress level, the amount of actuation, and the corrosive nature of the environment. Experimental results show that SMAs undergoing transformation induced fatigue exhibit a low-cycle fatigue behavior and the measurement of the accumulated plastic strain at failure is associated to a Manson-Coffin type failure criterion. Investigations conducted on the post-mortem microstructure showed evidence of a multiphysical coupling between corrosion and cyclic phase transformation, from which a novel cyclic damage mechanism is proposed and explained using the micromechanical shear lag model accounting for actuation and accumulated plastic strains. Thereafter, based upon the identified failure mechanism and considering damage accumulation through crack formation, a stress renormalization procedure is proposed in combination with the Miner’s rule to predict the reduction of number of cycles to failure due to cyclic phase transformation and corrosion. A direct method is first presented and the predictions show good agreement with experimental results. However, both corrosion and corrosion-free fatigue data are required. Therefore, a new approach is proposed: the inverse Miner’s rule, which requires corrosion fatigue data only to predict corrosion-free life. The new and attractive properties of the selected second alloy, i.e. Ni-rich NiTi SMA, have revived the motivation of the aerospace industry to design SMA actuators. One particular property is cyclic stability generated by precipitation hardening mechanism using precipitates. However, are also precipitates due to high Nickel content (60 wt.% or 55 at.%). Parameters such as processing, heat treatments, size effects, surface quality and environment are investigated. Thermomechanical response and fatigue life are discussed and the greatest impact is found to come from specimen surface quality. Finally, a detailed fractography presents the different microstructural aspects of the fatigue damage and concludes to a precipitation driven fatigue failure mechanism cause by precipitates.

La motivation de cette thèse est la production innovante de germes ultra-minces de silicium cristallin. L’utilisation de tels germes dans un procédé de fabrication de cellules solaires permettrait une réduction importante de la consommation de silicium, qui compte déjà pour 60% du coût de production des panneaux solaires de première génération. Dans le cadre de cette thèse, une méthode pionnière de détachement de germes minces a été mise en oeuvre. Dans cette méthode, une contrainte induite mécaniquement est guidée par des défauts étendus induits par l’implantation d’hydrogène. Par cette méthode, le détachement de germes minces d’environ 710nm d’épaisseurs a été obtenu. Le but est ensuite d’utiliser ces germes pour faire croitre du silicium cristallin avec des épaisseurs variables à souhait, soit une technique kerf-free : sans pertes. Cette étude présente ainsi les étapes menant à la mise en oeuvre de ce procédé : en premier lieu, un état de l’art des méthodes de détachement de films ultra-minces existants est réalisé. Celui-ci nous a ainsi guidés vers l’implantation d’hydrogène en tant que méthode viable du guidage de la fracture. Par la suite, différents tentatives de détachement de germes ultra-minces ont été réalisés puis caractérisés, notamment par MEB, MET, AFM et DRX. Dans de bonnes conditions de collage et de croissance de défauts, le détachement de germes ultra-minces de silicium cristallin a été réalisé. Par la suite, la croissance et la cristallisation de couches de silicium amorphe a été réalisée sur les germes détachés. Pour finir, certaines couches détachées ont été utilisées pour la production de cellules solaires prototypes. / The goal of this thesis is to find an innovative way to produce ultra-thin crystalline silicon seeds. The use of such seeds in a solar cell production process could lead to a significant reduction of the silicon consumption, which cost alone is worth 60% of the total cost of a first generation solar panel. Within the context of this PhD thesis, a pioneer seed exfoliation method was implemented. This method use the defects induced by hydrogen implantation to guide a stress-induced spalling process. This method has allowed the exfoliation of 710nm-thick crystalline silicon seeds. These seeds will then be used for the growth of crystalline silicon layers of any desired thickness, hence a totally kerf-free method. This thesis work presents the steps leading to the implementation of this process: firstly, the state of the art of ultra-thin films exfoliation methods is reviewed, which guided us towards the use of hydrogen implantation as a crack guide. Then, different ultra-thin seeds exfoliation processes were tried and characterized, specifically by SEM, TEM, AFM and XRD. In the right conditions of bonding and defects growth, ultra-thin silicon seeds were successfully exfoliated. The growth and crystallization of amorphous silicon layers on these seeds were then studied. Finally, several exfoliated layers were used for the production of prototype solar cells.

The integrity of nearly all engineering structures are threatened by the presence of cracks. Structural failure occurs if a crack larger than a critical size exists. Although most well designed structures initially contain no critical cracks, subcritical cracks can grow to failure under fatigue loading, called fatigue crack growth (FCG). Because it is impossible or impractical to prevent subcritical crack growth in most applications, a damage tolerant design philosophy was developed for crack sensitive structures. Design engineers have taken advantage of the FCG threshold concept to design for long fatigue lives. FCG threshold (DKth) is a value of DK (crack-tip loading), below which no significant FCG occurs. Cracks are tolerated if DK is less than DKth. However, FCG threshold is not constant. Many variables influence DKth including microstructure, environment, and load ratio. The current research focuses on load ratio effects on DKth and threshold FCG. Two categories of load ratio effects are studied here: extrinsic and intrinsic. Extrinsic load ratio effects operate in the crack wake and include fatigue crack closure mechanisms. Intrinsic load ratio effects operate in the crack-tip process zone and include microcracking and void production. To gain a better understanding of threshold FCG load ratio effects (1) a fatigue crack closure model is developed to consider the most likely closure mechanisms at threshold, simultaneously, and (2) intrinsic load ratio mechanisms are identified and modeled. An analytical fatigue crack closure model is developed that includes the three closure mechanisms considered most important at threshold (PICC, RICC, and OICC). Crack meandering and a limited amount of mixed-mode loading are also considered. The rough crack geometry, approximated as a two-dimensional sawtooth wave, results in a mixed-mode crack-tip stress state. Dislocation and continuum mechanics concepts are used to determine mixed-mode crack face displacements. Plasticity induced crack closure is included by modifying an existing analytical model, and an oxide layer in the crack mouth is modeled as a uniform layer. Finite element results were used to verify the analytical solutions for crack-tip stress intensity factor and crack face displacements. These results indicate that closure for rough cracks can occur at two locations: (1) at the crack-tip, and (2) at the asperity nearest the crack-tip. Both tip contact and asperity contact must be considered for rough cracks. Tip contact is more likely for high Kmax levels, thick oxide layers, and shallow asperity angles, a. Model results indicate that closure mechanisms combine in a synergistic manner. That is, when multiple closure mechanisms are active, the total closure level is greater than the sum of individual mechanisms acting alone. To better understand fatigue crack closure where multiple closure mechanisms are active (i.e. FCG threshold), these interactions must be considered. Model results are well supported by experimental data over a wide range of DK, including FCG threshold. Closure-free load ratio effects were studied for aluminum alloys 2024, 7050, and 8009. Alloys 7050 and 8009 were selected because load ratio effects at FCG threshold are not entirely explained by fatigue crack closure. It is believed that closure-free load ratio mechanisms occur in these alloys. Aluminum alloy 2024 was selected for study because it is relatively well behaved, meandering most load ratio effects are explained by fatigue crack closure. A series of constant Kmax threshold tests on aluminum alloys were conducted to eliminate fatigue crack closure at threshold. Even in the absence of fatigue crack closure load ratio (Kmax) effects persist, and are correlated with increased crack-tip damage (i.e. voids) seen on the fatigue crack surfaces. Accelerated FCG was observed during constant Kmax threshold testing of 8009 aluminum. A distinct transition is seen the FCG data and is correlated with a dramatic increase in void production seen along the crack faces. Void production in 8009 aluminum is limited to the specimen interior (plane-strain conditions), promoting crack tunneling. At higher values of Kmax (+_ 22.0 MPaà m), where plane-stress conditions dominate, a transition to slant cracking occurs at threshold. The transition to slant cracking produces an apparent increase in FCG rate with decreasing DK. This unstable threshold behavior is related to constraint conditions. Finally, a model is developed to predict the accelerated FCG rates, at higher Kmax levels, in terms of crack-tip damage. The effect of humidity (in laboratory air) on threshold FCG was studied to ensure that environmental effects at threshold were separated from load ratio effects. Although changes in humidity were shown to strongly affect threshold FCG rates, this influence was small for ambient humidity levels (relative humidity between 30% and 70%). Transient FCG behavior, following an abrupt change in humidity level, indicated environmental damage accumulated in the crack-tip monotonic plastic zone. Previous research implies that hydrogen (a component of water vapor) is the likely cause of this environmental damage. Analysis suggests that bulk diffusion is not a likely hydrogen transport mechanism in the crack-tip monotonic plastic zone. Rather, dislocation-assisted diffusion is presented as the likely hydrogen transport mechanism. Finally, the (extrinsic) fatigue crack closure model and the (intrinsic) crack-tip damage model are put in the context of a comprehensive threshold model. The ultimate goal of the comprehensive threshold model is to predict fatigue lives of cyclically loaded engineering components from (small) crack nucleation, through FCG, and including failure. The models developed in this dissertation provide a basis for a more complete evaluation of threshold FCG and fatigue life prediction. The research described in this dissertation was performed at NASA-Langley Research Center in Hampton, Virginia. Funding was provided through the NASA GSRP program (Graduate Student Researcher Program, grant number NGT-1-52174). / Ph. D.

Self-consolidating concrete (SCC) has wide use for placement in congested reinforced concrete structures in recent years. SCC represents one of the most outstanding advances in concrete technology during the last two decades. In the current work a great deal of cognizance pertaining to mechanical properties of SCC and comparison of fracture characteristics of notched and unnotched beams of plain concrete as well as using acoustic emission to understand the localization of crack patterns at different stages has been done. An artificial neural network (ANN) is proposed to predict the 28day compressive strength of a normal and high strength of SCC and HPC with high volume fly ash. The ANN is trained by the data available in literature on normal volume fly ash because data on SCC with high volume fly ash is not available in sufficient quantity. Fracture characteristics of notched and unnotched beams of plain self consolidating concrete using acoustic emission to understand the localization of crack patterns at different stages has been done. Considering this as a platform, further analysis has been done using moment tensor analysis as a new notion to evaluate fracture characteristics in terms of crack orientation, direction of crack propagation at nano and micro levels. Analysis of B-value (b-value based on energy) is also carried out, and this has introduced to a new idea of carrying out the analysis on the basis of energy which gives a clear picture of results when compared with the analysis carried out using amplitudes. Further a new concept is introduced to analyze crack smaller than micro (could be hepto cracks) in solid materials. Each crack formation corresponds to an AE event and is processed and analyzed for crack orientation, crack volume at hepto and micro levels using moment tensor analysis based on energy. Cracks which are tinier than microcracks (could be hepto), are formed in large numbers at very early stages of loading prior to peak load. The volume of hepto and micro cracks is difficult to measure physically, but could be characterized using AE data in moment tensor analysis based on energy. It is conjectured that the ratio of the volume of hepto to that of micro could reach a critical value which could be an indicator of onset of microcracks after the formation of hepto cracks.

The main objective of the presented thesis is to contribute to the development of diagnostic methods for piezoelectric sensor testing. The thesis describes the methods for piezoelectric sensors microcracks identification and diagnostics. The core of the thesis presents the development of a knock sensor prototype, design of suitable methods for the knock sensors diagnosis and evaluation of developed methods with focus on detection of microcracks in the sensor piezoceramic. The last part of the thesis deals with the influence of cracks and splits on the measured data from the piezoelectric transducer. The presented methods are focusing on impedance measurements and sensors frequency response measurements. Known properties of used piezoelectric material as an information source for measurement and diagnosis are provided. The main result of the work is the evaluation of the methods developed for the piezoelectric sensors self-diagnosis.