This master thesis is the result of a collaborative work between EMBRAER and the Escola Politécnica da USP for the study of structural health monitoring (SHM) techniques using sensors applied to aircraft structures. The goal was to develop classification techniques to discriminate between different events arising in the aircraft structure during tests; in the short term, improving the current SHM system used by EMBRAER, based on acoustic emission and, in the long term, fostering the development of a fully distributed system. As a result of studying classification methods for immediate use, we developed two techniques: the Spectral Similarity and a Support Vector Machines (SVM) classifier. Both are unsupervised solutions, due to the unlabeled nature of the data provided. The two solutions were delivered as a final product to EMBRAER for prompt use in the existing SHM system. By studying distributed solutions for future implementations, we developed a detection algorithm based on adaptive techniques. The main result was a special initialization for a maximum likelihood (ML) detector that yields an exponential decay rate in the error probability to a nonzero steady state, using adaptive diffusion estimation in a distributed sensor network. The nodes that compose the network must decide, locally, between two concurrent hypotheses concerning the environment state where they are inserted, using local measurements and shared estimates coming from their neighbors. The exponential performance does not depend on the adaptation step size value, provided it is sufficiently small. The results concerning this distributed detector were published in the journal IEEE Signal Processing Letters. / Esta dissertação de mestrado é o resultado de um trabalho colaborativo entre a EMBRAER e a Escola Politécnica da USP no estudo de técnicas de monitoramento do estado de saúde de estruturas (Structural Health Monitoring - SHM) utilizando sensores em estruturas aeronáuticas. O objetivo foi desenvolver técnicas de classificação para discriminar entre diferentes eventos que surgem em estruturas aeronáuticas durante testes; para o curto prazo, aperfeiçoando o atual sistema de SHM utilizado pela EMBRAER, baseado em emissão acústica e, no longo prazo, fomentando o desenvolvimento de um sistema completamente distribuído. Como resultado do estudo de métodos de classificação para uso imediato, desenvolvemos duas técnicas: a Similaridade Espectral e um classificador que utiliza Support Vector Machines (SMV). Ambas as técnicas são soluções não-supervisionadas, devido a natureza não rotulada dos dados fornecidos. As duas soluções foram entregues como um produto final para a EMBRAER para pronta utilização em seu atual sistema de SHM. Ao estudar soluções completamente distribuídas para futuras implementações, desenvolvemos um algoritmo de detecção baseado em técnicas adaptativas. O principal resultado foi uma inicialização especial para um detector de máxima verossimilhança (maximum likelihood - ML) que possui uma taxa de decaimento exponencial na probabilidade de erro até um valor não nulo em regime estacionário, utilizando estimação adaptativa em uma rede distribuída. Os nós que compõem a rede devem decidir, localmente, entre duas hipóteses concorrentes com relação ao estado do ambiente onde eles estão inseridos, utilizando medidas locais e estimativas compartilhadas vindas de nós vizinhos. O desempenho exponencial não depende do valor do passo de adaptação, se este for suficientemente pequeno. Os resultas referentes a este detector distribuído foram publicados na revista internacional IEEE Signal Processing Letters.

Air borne or liquid-laden solid particle transport is a common phenomenon in various industrial applications. Solid particles, transported at severe operating conditions such as high flow velocity, can cause concerns for structural integrity through wear originated from particle impacts with structure. To apply Acoustic Emission (AE) in particle impact monitoring, previous researchers focused primarily on dry particle impacts on dry target plate and/or wet particle impacts on wet or dry target plate. For dry particle impacts on dry target plate, AE events energy, calculated from the recorded free falling or air borne particle impact AE signals, were correlated with particle size, concentration, height, target material and thickness. For a given system, once calibrated for a specific particle type and operating condition, this technique might be sufficient to serve the purpose. However, if more than one particle type present in the system, particularly with similar size, density and impact velocity, calculated AE event energy is not unique for a specific particle type. For wet particle impacts on dry or wet target plate (either submerged or in a flow loop), AE event energy was related to the particle size, concentration, target material, impact velocity and angle between the nozzle and the target plate. In these studies, the experimental arrangements and the operating conditions considered either did not allow any bubble formation in the system or even if there is any at least an order of magnitude lower in amplitude than the sand particle impact and so easily identifiable. In reality, bubble formation can be comparable with particle impacts in terms of AE amplitude in process industries, for example, sand production during oil and gas transportation from reservoir. Current practice is to calibrate an installed AE monitoring system against a range of sand free flow conditions. In real time monitoring, for a specific calibrated flow, the flow generated AE amplitude/energy is deducted from the recorded AE amplitude/energy and the difference is attributed to the sand particle impacts. However, if the flow condition changes, which often does in the process industry, the calibration is not valid anymore and AE events from bubble can be misinterpreted as sand particle impacts and vice versa. In this research, sand particles and glass beads with similar size, density and impact velocity have been studied dropping from 200 mm on a small cylindrical stepped mild steel coupon as a target plate. For signal recording purposes, two identical broadband AE sensors are installed, one at the centre and one 30 mm off centred, on the opposite of the impacting surface. Signal analysis have been carried out by evaluating 7 standard AE parameters (amplitude, energy, rise time, duration, power spectral density(PSD), peak frequency at PSD and spectral centroid) in the time and frequency domain and time-frequency domain analysis have been performed applying Gabor Wavelet Transform. The signal interpretation becomes difficult due to reflections, dispersions and mode conversions caused by close proximity of the boundaries. So, a new signal analysis parameter - frequency band energy ratio - has been proposed. This technique is able to distinguish between population of two very similar groups (in terms of size and mass and energy) of sand particles and glass beads, impacting on mild steel based on the coefficient of variation (Cv) of the frequency band AE energy ratios. To facilitate individual particle impact identification, further analysis has been performed using Support Vector Machine (SVM) based classification algorithm using 7 standard AE parameters, evaluated in both the time and frequency domain. Available data set has been segmented into two parts of training set (80%) and test set (20%). The developed model has been applied on the test data for model performance evaluation purpose. The overall success rate of individually identifying each category (PLB, Glass bead and Sand particle impacts) at S1 has been found as 86% and at S2 as 92%. To study wet particle impacts on wet target surface, in presence of bubbles, the target plate has been sealed to a cylindrical perspex tube. Single and multiple sand particles have been introduced in the system using a constant speed blower to impact the target surface under water loading. Two sensor locations, used in the previous sets of experiments, have been monitored. From frequency domain analysis it has been observed that characteristic frequency for particle impacts are centred at 300-350 kHz and for bubble formations are centred at 135 – 150 kHz. Based upon this, two frequency bands 100 – 200 kHz (E1) and 300 – 400 kHz (E3) and the frequency band energy ratio (E3E1,) have been identified as optimal for identification particle impacts for the given system. E3E1, > 1 has been associated with particle impacts and E3E1, < 1 has been associated with bubble formations. Applying these frequency band energy ratios and setting an amplitude threshold, an automatic event identification technique has been developed for identification of sand particle impacts in presence of bubbles. The method developed can be used to optimize the identification of sand particle impacts. The optimal setting of an amplitude threshold is sensitive to number of particles and noise levels. A high threshold of say 10% will clearly identify sand particle impacts but for multiparticle tests is likely to not detect about 20% of lower (impact) energy particles. A threshold lower than 3% is likely to result in detection of AE events with poor frequency content and wrong classification of the weakest events. Optimal setting of the parameters used in the framework such as thresholds, frequency bands and ratios of AE energy is likely to make identification of sand particle impacts in the laboratory environment within 10% possible. For this technique, once the optimal frequency bands and ratios have been identified, then an added advantage is that calibration of the signal levels is not required.

Le contrôle non destructif (CND) par émission acoustique (EA) est utilisé dans un grand nombre de domaines tels l’énergie nucléaire, le secteur pétrolier et gazier, le génie civil ou l’industrie mécanique afin de vérifier l’intégrité des structures sous contrainte. Selon le rapport entre la longueur d’onde et l’épaisseur de la structure, l’énergie libérée par un défaut sous contrainte peut se propager sous forme d’ondes guidées (cas des structures minces) ou sous forme d’onde de Rayleigh (cas des structures épaisses). L’analyse des signaux issus de cette méthode ultrasonore « passive » présente des difficultés liées principalement à la complexité des signaux typiquement mesurés. L’objectif de la thèse est de développer des modèles permettant la simulation d’expériences de CND par EA dans le cas des structures épaisses ou minces. Les modèles développés sont basés sur un couplage entre un modèle de source d’EA, un modèle de propagation des ondes et un modèle de capteur d’EA. Dans le cas des structures épaisses, deux modèles 2D (concernant le contrôle de pièces de surface plane et cylindrique) et un modèle 3D (surface plane) ont été développés afin de prédire le signal correspondant à l’onde de Rayleigh émise par un défaut sous contraintes. Concernant les structures minces, un modèle 2D a été développée permettant de prédire le signal correspondant aux modes guidés émis par une fissure sous contrainte. Plusieurs études paramétriques ont été menées afin de définir l’influence des différentes données d’entrée des modèles sur les signaux d’EA et ainsi aider à l’interprétation des contrôles par EA. / AE Non-destructive testing is used in many fields such as nuclear energy, oil and gas, civil engineering or mechanical engineering to check the integrity of structures under stress. Depending on the ratio of structure thickness to wavelength, the energy released by a crack under stress can propagate either as guided waves (in thin structures) or as Rayleigh wave (in thick structures). The analysis of signals resulting from this ultrasonic "passive" method is particularly difficult due to the complexity of typically measured signals. The objective of this thesis is to develop models to enable the simulation of AE testing experiments in the case of thick or thin structure. The developed models rely on the coupling between an AE source model, wave propagation models and an AE Sensor model. In the case of thick structures two 2D models (for plane and cylindrical surfaces) and a 3D model (for plane surface) have been developed to predict the signal corresponding to the Rayleigh wave emitted by a crack under stress. In the case of thin structures, a 2D model has been developed to predict the signal corresponding to the guided modes emitted by a crack under stress. Several parametric studies have been conducted to determine the influence of the different model input data on the AE signals and thus help to interpret AE testing results.

Considerando as dimensões reduzidas das ferramentas de microfresamento, a seleção não otimizada dos parâmetros de corte tende a maximizar o desgaste e a quebra da ferramenta durante operações de microusinagem. Isto posto, o desenvolvimento de um sistema de monitoramento para explorar as condições da microfresa durante a usinagem é fundamental. Portanto, o objetivo desta pesquisa é monitorar via sinais de potência e emissão acústica (EA) o desgaste da ferramenta e a estabilidade de corte em operações de microfresamento do aço COS AR60 e COS AR60 de grãos ultrafinos (GUF). Os testes de microfresamento foram realizados com ferramentas de diâmetro de 1 mm e duas arestas, com substrato de metal duro e revestimento (Ti, Al, Cr) N, em um centro de usinagem CNC Romi D800 High Performance adaptado com um cabeçote de alta rotação. O microfresamento ocorreu nos dois materiais sem aplicação de fluido de corte e com velocidade de corte de 62,5 m/min e 125 m/min, mantendo constante a velocidade de avanço de 240 mm/min (fz = 6 &#956;m/aresta e 3 &#956;m/aresta), profundidade de usinagem de 100 m e comprimento de usinagem de 104 mm em corte em cheio. O sinal de potência e EA foram adquiridos à taxa de 5 kHz e 1,25 MHz, respectivamente. Os dados foram adquiridos em LabVIEW® e processados em LabVIEW® e MATLAB®. Os resultados de caracterização dos desgastes apontaram um desgaste de flanco mais expressivo e a formação de Aresta Postiça de Corte (APC) no GUF para vc = 125 m/min, e a presença de desgaste de cratera em todas as condições de corte. O aumento da potência de corte média representou a predominância do desgaste de flanco, e desgaste de cratera em sua redução. De forma semelhante, a ANOVA dos valores de EA RMS indicaram com significância (95% de confiança) uma correlação diretamente proporcional entre EA RMS e evolução do desgaste de flanco na microfresa. Quanto à estabilidade de corte, ambos os sinais apresentaram um aumento expressivo de amplitude quando o corte foi instável. Com isso, os métodos de monitoramento utilizados foram capazes de indicar a evolução do desgaste da microfresa e a ocorrência de chatter em operações de microfresamento. / Regarding the reduced dimensions of micro-milling tools, a non-optimised selection of cutting parameters tends to maximise tool wear and breakage during cutting operations. Hereupon the development of a monitoring system for exploring microtool conditions during machining is imperative. Therefore, the aim of this research is to monitor tool wear and cutting stability via cutting power and acoustic emission (AE) signals in micro-milling operations of steel COS AR60 and ultra fine-grained steel COS AR 60 (GUF). Cutting tests were performed by carbide endmill tools with (Ti, Al, Cr) N coating, two flutes and 1 mm diameter in a CNC machining centre Romi D800 High Performance adapted with a high spindle speed head. Micro-milling operations were carried out in both materials without cutting fluid application at 62.5 m/min and 125 m/min, and constant parameters of feed, set at 240 mm/min (fz = 6 &#956;m/tooth and 3 &#956;m/tooth), depth of cut of 100 m and cutting length of 104 mm performed in sloth cutting strategy. Cutting power and AE signals were acquired at the rate of 5 kHz and 1.25 MHz, respectively. The data were acquired in LabVIEW® and processed in both LabVIEW® and MATLAB®. The results on wear characterisation revealed a major flank wear and the formation of Built Up-Edge (BUE) in GUF at vc = 125 m/min, along with the occurrence of crater wear in all cutting conditions set. An increase in the average cutting power levels is linked to the predominancy of flank wear, while crater wear to its decrease. Likewise, the Analysis of Variance (ANOVA) of EA RMS values indicated with significancy (95% confidence) a direct proportion between AE RMS and flank wear in the microtool. In terms of cutting stability both EA and cutting power signals have shown an expressive rise when performing instable cutting. Thus, the methods of monitoring were feasible for recognising tool wear evolution and chatter in micro-milling operations.

L’objectif principal de cette thèse est d’étudier l’efficacité d’un inhibiteur à base de phosphate, Na3PO4, sur l’amorçage de la corrosion des armatures du béton. L’étude a été réalisée moyennant des méthodes électrochimiques et d’analyse de surface associées à l’émission acoustique et à la technique de la cellule de diffusion. L’évaluation de l’efficacité de l’inhibiteur en milieu simulant le béton a été réalisée en utilisant une nouvelle méthode de prétraitement de l’armature et de suivi de la corrosion. Il apparaît qu’en présence de Na3PO4 le rapport critique [Cl-] / [OH-] d’amorçage de la corrosion par piqûre atteint une valeur (R=15) nettement supérieure à celle sans utilisation de Na3PO4 (R ~ 0,6). L’inhibition est due à la formation d’un film renfermant des composés phosphatés (FePO4, (PO4)2Fe3,8H2O) qui bloque les sites anodiques actifs de l’acier, et augmente de façon significative sa résistance à la corrosion localisée. Pour un rapport R > 15, la dépassivation est liée à la présence d’une forte teneur en chlorure dans le milieu et conduit à terme, à la destruction quasi générale du film formé au préalable sur la surface de l’acier.La technique de cellule de diffusion a permis d’étudier, principalement, la cinétique de diffusion des ions Cl- dans un mortier confectionné sans et avec Na3PO4. La présence du phosphate dans le mortier entraîne une réduction du coefficient de diffusion des ions chlorures, et un accroissement important de la période d’amorçage du processus de corrosion. Enfin, l’inhibiteur adjuvant engendre la formation de nouveaux produits à base de phosphate dans le mortier (principalement : Ca3H2(P2O7)2, H2O et CaHPO4, 2H20). La disparition des hydrates usuels du ciment entraine une légère diminution de la résistance à la compression du béton, et de son module d’élasticité. Néanmoins, la présence de ces composés phosphatés bloque les pores du mortier et freine la diffusion des chlorures. Il s’ensuit une amélioration de la résistance de la corrosion du mortier armé en milieu 3 % NaCl. L’ensemble de ces résultats a montré clairement que cet adjuvant demeure recommandé pour la protection des armatures contre la corrosion en milieu chloruré. / The main aim of this thesis is to study the effectiveness of a phosphate based inhibitor, Na3PO4, against steel reinforcement corrosion initiation. The study was carried out by means of electrochemical methods and surface analysis associated with the acoustic emission and the diffusion cell technique. The effectiveness evaluation of this inhibitor in medium simulating the concrete pore solution has been studied using new method for reinforcement pretreatment and the corrosion monitoring. It appears that in the presence of Na3PO4, the critical ratio [Cl-] / [OH-] which prevents the pitting corrosion initiation reaches 15. This value is significantly higher than that found in the case of the steel without Na3PO4 (R ~ 0. 6). The inhibition is due to the layer formation containing phosphate compounds (FePO4, (PO4)2Fe3.8H2O), resulting in a considerable reduction of the anode active sites in contact with the electrolyte. This reinforces the steel passivation and greatly increases its resistance to localized corrosion. For R > 15 ratio, the depassivation has been associated with the presence of a high chloride content in the medium and with the destruction of the film formed beforehand on the steel surface. The diffusion cell technique was used to study mainly the Cl- ion diffusion kinetics in a mortar without and with Na3PO4. The presence of phosphate in the mortar, leads to the chloride ions diffusion coefficient reduction and an important increase of the corrosion process initiation period. Finally, the adjuvant inhibitor causes the formation of new phosphate-based products in the mortar (principally: Ca3H2(P2O7)2.H2O et CaHPO4.2H20). The disappearance of usual cement hydrates induces a slight decrease of compressive strength of the concrete and its elasticity modulus. Nevertheless, the presence of these phosphate compounds blocks the mortar pores and restricts the chloride diffusion. It follows an improvement of the corrosion resistance of the reinforced mortar in 3% NaCl medium. All these results clearly show that this adjuvant is recommended for the reinforcement protection against corrosion in chloride medium.

La compréhension du comportement d'un composite à matrice céramique (CMC) lorsqu'il est sollicité en fatigue est l'un des points clés pour permettre son utilisation dans un cadre industriel. Il est en effet nécessaire de déterminer la chronologie des différents mécanismes d'endommagement ainsi que d'estimer la durée de vie en conditions d'utilisation. Il est alors nécessaire de réaliser une caractérisation mécanique mais aussi de définir des indicateurs d'endommagement permettant la prévision de durée de vie. Dans ce but, il est intéressant de coupler l'analyse des paramètres mécaniques et les observations microstructurales à des techniques de suivi en temps réel de l'endommagement. L'émission acoustique (EA) est une méthode de suivi non destructive qui permet de répondre à cette problématique. Elle permet notamment de quantifier et de localiser l'endommagement. Dans ce travail, de nouveaux indicateurs d'endommagement sont mis en place tels la "Sévérité" des signaux définie à partir de l'énergie acoustique ainsi que la "Sentry function" définie à partir de l'énergie acoustique et de l'énergie mécanique. Ce travail s'articule autour de deux principaux axes. Dans un premier temps il s'agit de caractériser les effets de la sollicitation cyclique sur ce type de matériau, ceci notamment en comparant l'évolution des paramètres mécaniques, les observations microstructurales ainsi que l’analyse de l'évolution globale de l'émission acoustique (EA) lorsque le matériau est soumis à un chargement statique et à un chargement cyclique. La seconde partie consiste à déterminer un scenario d'endommagement. Dans un premier temps, les signaux d’EA sont analysés en fonction de leur détection dans le cycle (charge/décharge). Ensuite la détermination de la signature acoustique des différents mécanismes d'endommagement par application de techniques de reconnaissance de formes supervisées a permis d'évaluer leur chronologie d'activation durant les essais de fatigue cyclique. Cette étude a permis de mettre en évidence un ensemble de mécanismes propres à la sollicitation cyclique, composé principalement de décohésion et de frottement aux interfaces fibre/matrice et matrice/matrice. De plus, l'utilisation de l'émission acoustique a permis de définir des temps caractéristiques ou critiques pouvant être utilisés dans un objectif de prévision de la durée de vie. En effet, par exemple la sévérité des signaux a permis de mettre en évidence un temps caractéristique situé entre 25 et 45% de la durée de vie du matériau. La détection en temps réel de ce temps caractéristique permet d'estimer la durée de vie restante. / The full understanding of a ceramic matrix composite under fatigue loading is needed in view of industrial applications. It is necessary to determine the damage mechanisms chronology and to be able to forecast the lifetime of the material in the conditions of use. To reach these purposes, a mechanical characterisation has to be done as well as the definition of damage indicators. It is then interesting to link the analysis of mechanical parameters and microscope observations with a non-destructive monitoring technique. Acoustic emission (AE) appears to be a good candidate to monitor material damage under loading. It makes the quantification and the material damage localisation possible. In this study, indicators based on released acoustic energy are used as "Severity" of signals or "Sentry function" which depends on both acoustic and mechanical energies. This work is organised in two parts. First, the analysis of mechanical parameters behaviour, material microstructure and global evolution of acoustic emission under static and cyclic loading makes the characterisation of the effects of cyclic fatigue on the material possible. The second part consists in determining a damage scenario. First acoustic emission signals are analysed depending on their acquisition during a cycle (loading or unloading). Then the connection between the acoustic emission signals and the different damage mechanisms, using a supervised clustering method, facilitated the estimation of the activation of these different damage mechanisms during cyclic fatigue tests. This study pointed out different damage mechanisms generated by cyclic loading, which are mainly debonding and friction at matrix/fibre and matrix/matrix interfaces. In addition, damage indicators based on acoustic emission enabled to determine characteristic times which can be used for lifetime forecast. For example, signal severity shows a characteristic time between 25% and 45% of the time to ultimate failure. Detection of this time in real-time during a test can be used to estimate the time of the ultimate failure of the material.

Afin d’augmenter la densité d’énergie des batteries Li-ion, en particulier pour le marché des véhicules électriques, il est nécessaire de développer des matériaux d’électrode plus performants. Le silicium, dont la capacité spécifique (3579mAh/g) est dix fois supérieure à celle du graphite, est un matériau particulièrement prometteur. Néanmoins, lors de sa lithiation, il subit une forte expansion volumique (280% contre 10% pour le graphite) conduisant à la décrépitation des particules de Si et à la fissuration/décohésion de l’électrode. Il en résulte une diminution notable de la durée de vie de l’anode. Pour améliorer la tenue au cyclage des électrodes, il est nécessaire de bien comprendre/quantifier leur dégradation morphologique, ce que permettent difficilement des analyses post mortem conventionnelles. Notre objectif est d’utiliser et de développer des outils permettant d'étudier in operando la dégradation de ces électrodes. Nous avons mis en œuvre des protocoles de caractérisation in operando couplant des mesures électrochimiques à l’émission acoustique d’une part et à la dilatométrie d’autre part. Le suivi de l’activité acoustique au cours du cyclage de l’électrode a montré que les particules de Si micrométrique constituant cette électrode se fracturent dès le début de la lithiation, et que la fissuration de l’électrode se produit progressivement tout au long de la 1ère lithiation. Peu d’activité acoustique est détectée par la suite. Par l’analyse des signaux acoustiques, trois types de signaux ont été identifiés, se différenciant principalement selon leur fréquence de pic. Les signaux de hautes fréquences sont associés principalement aux micro-fractures des particules en début de lithiation, et les signaux à moyennes et basses fréquences sont respectivement attribuées à la fissuration de l’électrode et aux macro-fractures des particules de Si en fin de lithiation. L’étude dilatométrique a montré une expansion volumique maximale de ~170% avec une encre tamponnée à pH3 versus 300% si l’électrode est préparée à pH7. Cette différence s’explique par la formation de liaisons cohésives entre le liant CMC et les particules de Si lorsque l’électrode est préparée à pH 3, améliorant sa résistance mécanique. Ce qui a été confirmé par des mesures d’indentation. Ainsi, l’électrode formulée à pH 3 montre une meilleure cyclabilité. Enfin, nous avons démontré qu’une diminution notable de la durée de vie de l’électrode est observée lorsque la taille initiale des particules de Si est réduite de 230 à 85nm. Nous expliquons ce résultat inattendu par une quantité insuffisante de CMC par rapport à la surface spécifique plus élevée des particules de taille plus faible. De fait, sa résistance mécanique est insuffisante et conduit à une fissuration et une exfoliation importantes de l’électrode. Ceci est appuyé par les mesures de dilatométrie, d’émission acoustique et des observations MEB. / To increase the energy density of Li-ion batteries, especially for the electric vehicle market, the development of new electrode materials is required. Silicon is a particularly interesting material, thanks to its high specific capacity (3579mAh/g, ten times higher than the capacity of graphite). Nevertheless, upon lithiation, silicon undergoes an important expansion (300% vs 10% for graphite). This leads to the cracking of the Si particles and fracturing of the electrode film. These induces electrical disconnections upon cycling, resulting in a poor cycle life. To improve the cyclability of the Si based electrodes, it is important to better understand/quantify their mechanical degradation. Conventional post mortem analyses are insufficient for that purpose. The objective of this work is to develop and use in operando analyses techniques. Therefore, we established protocols to characterize composite electrodes by electrochemical measurements coupled with either acoustic emission (AE) or dilatometry measurements. The evolution of the acoustic activity upon cycling showed that the cracking of the micrometric Si particles and of the composite film mainly occurs during the first cycle and is initiated in the early stage of the lithiation. Very few AE signals are detected in the following cycles. The signal analysis leads to the identification of three types of signals depending to their peak frequency. High frequency signals were associated with surface micro-cracking of the Si particles at the beginning of lithiation. Medium and low frequency signals were respectively attributed to the fracturing of the electrode film and bulk macro-cracking of the Si particles at the end of lithiation. An electrode thickness expansion of 170% was measured by electrochemical dilatometry for our electrodes prepared at pH3 versus 300% for electrodes prepared at pH7. The different mechanical behavior is explained by the formation of covalent bonds between the CMC binder and Si particles at pH3, which increases the mechanical stability of electrodes. This was confirmed by the measurement of their hardness and Young’s modulus. Therefore, pH3 electrodes display a higher capacity retention. It was also demonstrated that a decrease of the Si particle size does not necessarily lead to an improvement of the electrode cycle life. Indeed, we observed a significant decrease of the electrode cycle life when the Si particle size is decreased from 230 to 85 nm. This can be explained by a lack of CMC binder in relation with the higher surface area of the smaller Si particles, leading to a lower mechanical resistance of the electrode film. Within the first cycles, Si 85 nm based electrodes suffer from important cracking and exfoliation. This was confirmed by in operando dilatometry and acoustic measurements, and post mortem SEM observations.

La corrosion dans le béton précontraint est considérée parmi les pathologies les plus dangereuses dans le secteur du génie civil. En effet ce phénomène se caractérise par la gravité de ses conséquences économiques et sécuritaires. L’objectif de ce travail consiste à évaluer l’efficacité d’un inhibiteur à base de phosphates Na3PO4.12H2O contre la corrosion des aciers de précontrainte. L’étude a été d’abord menée en milieu synthétique simulant le béton chloruré sur des armatures tendues à 80% Rm, puis d’une part sur des éprouvettes en mortier précontraint conçues à l’échelle laboratoire, et d’autre part en utilisant la technique de cellule de diffusion pour tester l’efficacité de l’inhibiteur à long terme. Les résultats issus de l’étude réalisée dans le milieu simulant ont révélé que la présence des phosphates entraine l’augmentation du seuil critique d’amorçage de corrosion localisée R=[Cl-]/[OH-] jusqu’à la valeur de 5 au lieu de 0,4. Ceci semble être dû à deux actions inhibitrices des phosphates à savoir : la stabilisation de la couche protectrice à base d’oxyde de fer et la formation de composés phosphatés très peu solubles qui bloquent les sites anodiques actifs, augmentant ainsi la résistance de l’acier à la corrosion localisée. L’emploi de Na3PO4.12H2O en tant qu’adjuvant diminue légèrement la résistance à la compression du mortier. Cependant les composés phosphatés provenant de la réaction de l’inhibiteur avec les hydrates de ciment colmatent les pores du mortier et freinent la diffusion des chlorures. Ceci améliore le comportement à la corrosion des armatures enrobées de mortier précontraint. Enfin, lorsque le triphosphate de sodium est utilisé comme inhibiteur migrateur ou comme moyen de prétraitement des armatures, la technique de la cellule de diffusion a montré son efficacité à long terme, grâce à l’augmentation de la période précédant l’amorçage d’une corrosion localisée, où l’armature est en état passif. / Corrosion in prestressed concrete is considered among the most dangerous pathologies in the civil engineering sector. Indeed, this phenomenon is characterized by the seriousness of its economic and security consequences. The objective of this work is to evaluate the efficiency of a phosphate based inhibitor Na3PO4.12H2O against the corrosion of prestressing steels. The study was first conducted on wires tensioned at 80% Rm and immersed in simulating concrete pore solution. Then it concerned, on one hand, prestressed mortar specimens designed on a laboratory scale and, on the other hand, the long term efficiency of the inhibitor using diffusion cell technique. The results obtained from the study carried out in the concrete simulating medium revealed that the presence of the phosphates causes the increase in the critical threshold of localized corrosion initiation R = [Cl -] / [OH-] up to the value of 5 instead of 0.4. This seems to be due to two phosphate inhibiting actions, namely: the stabilization of the iron oxide protective layer and the formation of very insoluble phosphate compounds which block the active anodic sites, increasing prestressing steel resistance to localized corrosion. The use of Na3PO4.12H2O as an additive slightly reduces the compressive strength of the mortar. However, phosphate compounds resulting from the reaction of the inhibitor with the cement hydrates clog the pores of the mortar and slow down the diffusion of the chlorides. This improves the corrosion behavior of prestressed mortar reinforcement. Finally, when sodium triphosphate is used as a migratory inhibitor or as a means of steel reinforcement pretreatment, the diffusion cell technique has shown its long-term efficiency, thanks to the increase of the period preceding the initiation of a localized corrosion, where the reinforcement is in a passive state.

Cette thèse a pour objectif la compréhension fine du rôle de la microstructure sur les propriétés mécaniques de composites à matrice céramique oxydes, en vue de l’introduction de ce type de matériau dans les futurs moteurs d’aviation civile. L’influence des hétérogénéités induites par la mise en forme de ce matériau est particulièrement investiguée. Ces hétérogénéités semblent favoriser l’apparition et la propagation de mécanismes d’endommagement conduisant à la ruine du matériau. L’étude est réalisée sur trois nuances de composites oxydes à tissage bidimensionnel générées à partir de trois procédés de fabrication différents. Ces procédés conduisent à la mise en place de trois types de microstructures. Des caractérisations morphologiques par porosimétrie et par μ-tomographie sont réalisées afin d’estimer la répartition des hétérogénéités et ainsi d’établir les microstructures représentatives de chaque nuance. En se basant sur ces analyses, une étude du comportement mécanique des nuances d’étude est réalisée à plusieurs échelles. Dans un premier temps, une étude des propriétés mécaniques à l’échelle macroscopique, représentative du matériau est effectuée à l’aide d’essais de traction dans le plan de tissage. En parallèle, des essais in-situ sont mis en place afin d’observer l’évolution de l’endommagement des microstructures. Ces observations permettent d’améliorer la compréhension du rôle des hétérogénéités sur l’activation des mécanismes d’endommagement. Le suivi de l’EA (Emission Acoustique) des essais est utilisé pour analyser la cinétique d’endommagement des nuances de composites oxydes. En plus de l’analyse globale de l’activité acoustique, des classifications des signaux d’EA sont réalisées. Ces classifications se basent sur la détection de signaux d’EA à l’aide de deux types de capteurs présentant des caractéristiques différentes. Une labellisation des classes est proposée en confrontant les activités de ces classes aux mécanismes d’endommagement observés lors des essais in-situ. Le couplage de l’ensemble de ces informations permet de constituer le scénario d’endommagement de chaque nuance. Il est ainsi possible d’établir le rôle de chaque type d’hétérogénéités sur le comportement mécanique des composites oxydes. / The aim of this thesis is the fine understanding on the influence of the microstructure on oxide-based ceramic matrix composites mechanical properties. These materials are good candidate for new generation of civil aircraft engines. The aim of this work is to establish a relationship between the microstructural defects generated by the manufacturing process and the mechanical behavior of the composite. These heterogeneities seem to influence the appearance and the propagation of damage mechanisms. This study is realized on three kinds of bi-dimensional oxide composites generated from three different manufacturing processes. These processes create three kinds of microstructure. Porosimetric and μ-tomographic analyses allow estimating the distribution of microstructural defects and establish typical microstructure of each oxide composite. Based on these preliminary analyses, mechanical behavior of each kind of oxide composites is studied through several representative scales. On the one hand, mechanical tensile tests are carried out in order to estimate the mechanical properties of the studied materials in the weaving plane. On the other hand, the implementation of in-situ mechanical tests allows the visualization of damage mechanisms appearance and propagation. These observations improve the understanding of the role of microstructural defects on the activation of damage mechanisms. Damage kinetics of each mechanical test are inspected through AE (Acoustic emission) analysis. This monitoring helps to link mechanical behavior with microstructural damage. In parallel with global AE analysis, AE clustering is achieved. These classifications are based on two kinds of AE sensor with different properties. Data fusion from the two sensors is accomplished. This technique allows more robust AE clustering. Cluster labelling is proposed thanks to damage mechanisms observed during in-situ mechanical tests. Damage scenarios are set up owing to macroscopic mechanical test, in-situ analysis and AE labelling. Thus, it is possible to establish the influence of each kind of microstructural defect on oxide-based CMCs mechanical behavior.

The amount and morphology of the graphite phase largely controls the resulting properties of cast iron. For instance, in flake graphite cast irons the mechanical properties are low while the thermal conductivity is high. This is in contrast with spheroidal graphite cast irons where the mechanical properties are high and the thermal conductivity is low. These differences are due to the different graphite morphologies and must be accounted for in the design work and material selection of cast iron components. In this work the influence of the graphite phase on the elastic and plastic deformation behaviour of cast irons has been studied. The material grades studied originate from castings for marine diesel engine piston rings with different chemical analyses. Two groups of pearlitic cast iron materials were studied; one with differences in graphite morphology and one with grey irons that differed in graphite content. For these different material grades the mechanical properties were correlated to microstructural parameters. In addition to standard uniaxial tensile tests, acoustic emission measurements were used for the study of deformation. When studying the modulus of elasticity of the cast iron it was found that the modulus of elasticity of the inherent graphite phase depends on the roundness of the graphite particles and is due to the strong anisotropy of the graphite phase. A linear correlation between nodularity and the modulus of elasticity of the graphite phase was derived. This correlation made it possible to account for the anisotropy of the graphite phase in the model used. By applying the linear function when modelling the effective modulus of elasticity, a high accuracy between experimental and theoretical values was achieved. Another factor affecting the elastic response when subjecting a cast iron component to tensile load was found to be the plastic deformation that actually occurs at very low strains for all of the studied cast iron grades. It was observed that the plastic deformation in the low strain elastic region, quantified by using acoustic emission measurements, increased linearly with decreasing modulus of elasticity. These measurements showed that the amount of plastic deformation in the elastic region was largely controlled by the graphite morphology. It was concluded that as the roundness of the graphite particles increases, the plastic deformation activity in the elastic region decreases. The plastic deformation activity continued linearly into the pronounced plastic region of the tensile tests. A decrease in roundness or increase in graphite fraction resulted in an increase of the amount of plastic deformation and the strain hardening exponent. A dependence between strength coefficient and graphite fraction was observed. Models for the flow curves for pearlitic cast irons were developed and shown to accurately reproduce the observed experimental curves. The surveys performed and conclusions from this thesis will be helpful in the design of new cast iron materials.