La connaissance et la maîtrise de la présence d’un biofilm représentent aujourd’hui un challenge important. Dans le contexte d’étude des capacités de développement des biofilms, BioFilm Control fait figure de pionnier grâce à leur test nommé Biofilm Ring Test. Basé sur une sollicitation du biofilm via l’attraction, par un aimant, de microbilles magnétiques au centre du puits, le test évalue la présence de biofilm par l’absence de regroupement des billes au centre du puits à un instant donné. L’enjeu de ce travail est de décliner le BioFilm Ring Test® en un examen dynamique, non destructif et à l’échelle microscopique. Dans le biofilm, la matrice polymérique assure la cohésion entre cellules et confère une protection aux bactéries qui vivent au sein du biofilm. Les propriétés mécaniques de la matrice sont donc un indicateur de l’état local du biofilm. La recherche de ces paramètres permet de pouvoir prédire et contrôler la formation, l’accumulation et la dissémination de bactéries propageant les infections et/ou l’encrassement. Néanmoins, la détermination des propriétés mécaniques des biofilms nécessite des précautions et l’usage d’un vocabulaire homogénéisé et de méthodes unifiées au sein de la communauté. Pour cela, une première partie de ce travail de thèse consiste en la proposition d’un guide de bonnes pratiques quant à la caractérisation mécanique du matériau biofilm. Dans la deuxième partie de ce travail de thèse, une méthodologie pour le suivi de particules micrométriques au sein d’un matériau vivant est développée. Le recours à des techniques d’imagerie telle que la corrélation d’images numériques permet de remonter à la cinématique du mouvement de chacune des microbilles, qui servent de marqueurs au sein des images traitées, par une mesure sans contact. Cette méthode est ensuite appliquée à l’étude de la formation de biofilm. L’originalité de ce travail repose sur la caractérisation de l’évolution de la typologie du mouvement des microbilles métalliques lors de la formation des biofilms. Il s’agit là de discriminer des comportements de billes révélateurs de la genèse d’un biofilm. En tirant parti de l’observation du mouvement de microbilles inertes introduites dans le milieu bactérien, on détecte des changements de typologies de trajectoires qui semblent être reliés à l’activité de bactéries sessiles, adhésion ou formation de matériel extracellulaire. Les résultats montrent que les diverses étapes de la formation de biofilms sont caractérisées, ce qui permet notamment de discriminer la présence ou non d’antibiotiques mélangés avec les bactéries et d’apprécier leur efficacité. Dans une dernière partie, des recherches encore en phase de développement sont exposées. Elles s’intéressent au comportement du biofilm sous sollicitation volumique. Il s’agit dans ce cas d’observer le biofilm en champ lointain et de suivre le déplacement ou la déformation d’un marquage constitué d’un agglomérat de microbilles, plongées dans un champ magnétique. Ces premiers travaux pourront servir d’ébauche à des travaux futurs dans le but de caractériser quantitativement le matériau biofilm. / The control of biofilm formation constitutes an important challenge in many industrial and biomedical applications. In this context, BioFilm Control is a pioneer thanks to its test named BioFilm Ring Test. Based on the immobilisation of magnetic microbeads by adherent cells, the assay allows to detect the presence of biofilm at a given time. The aim of this phD project is to translate the BioFilm Ring Test® into a dynamic, non-destructive and microscopic examination of the biofilm state. Whithin the biofilm, the matrix provides a strong cohesion between cells and therefore increases their resistance against chemical or mechanical stress in comparison to their planktonic counterparts. The mechanical properties of the matrix are therefore an indicator of the local state of the biofilm. The search for these parameters makes it possible to predict and control the formation, accumulation and spread of bacteria that propagate infections and/or biofouling. Nevertheless, the determination of the mechanical properties of biofilms requires precautions and the use of an homogenized vocabulary and methods that are unified within the community. To this end, a first part of this thesis work consists in proposing a guide of good practices for the mechanical characterization of biofilm material. In the second part of this work, a methodology for tracking of micrometric particles within a living material is developed. The use of full field measurement method such as digital image correlation makes it possible to trace the kinematics of the motion of each particle, which is a probe of the local environment. This method is then applied to the study of the biofilm formation, by non-contact measurement. The originality of this work is based on the characterization of the change in the microbeads movement during the biofilm formation steps. The aim is to discriminate bead behaviours that reveal the genesis of a biofilm. By taking advantage of the observation of the movement of inert microbeads embedded into the bacterial environment, we detect changes of type of trajectories which seem to be correlated to the activity of sessiles bacteria, adhesion or formation of extracellular material. The results show that the various stages of the biofilm formation are characterized by a non-destructive test. Especially, It allows to appreciate the efficiency of an antibiotic. In the last part, research still in a development phase is presented. It concerns the behaviour of biofilm under mechanical solicitation. This involves observing the biofilm in the far field and following the displacement or deformation of a pattern consisting of an agglomerate of microbeads immersed in a magnetic field. This initial work can be used as a draft for future work to quantitatively characterize the biofilm material.

A roller coaster manufacturer became aware that improperly heat treated track couplings were sent to a construction site for assembly. Concerns were that suspect couplings might not meet the engineering specifications and could be vulnerable to sudden failure. A testing company in Oak Ridge, TN that specializes in in-situ and laboratory mechanical testing was contacted by the manufacturer for help in this endeavor. The construction company elected to enlist a local testing firm to perform field tests on the components instead of the company in Oak Ridge. The test methods used are incapable of providing quantitative results that could be measured to the engineering specifications, making it unlikely to identify anything but the worst material conditions. This study is an example that the need for accurate analysis is very important. The manufacturer reported that 60 couplings were replaced, but it is presently unknown how many should have been replaced.

La décrépitation (fracturation) des matériaux actifs de batteries associée à leur variation volumique lors des cycles de charge/décharge a pour effet d'accélérer leur corrosion par l'électrolyte et/ou d'induire une perte de connectivité électronique au sein de l'électrode ce qui réduit notablement leur durée de vie. C’est particulièrement le cas des hydrures métalliques utilisés dans les batteries Ni-MH. À ce jour, l'évaluation de leur fracturation se limite généralement à une observation post mortem des électrodes par microscopie ce qui ne permet pas une analyse détaillée du processus de décrépitation. À ce titre, un de nos principaux objectifs dans le cadre de ce travail de recherche a été de développer une méthode d'analyse novatrice et performante basée sur l'émission acoustique (EA) afin d'étudier in situ la fracturation d'électrodes négatives pour batteries Ni-MH. Dans une première étape, nous avons analysé en détail les signaux acoustiques produits lors de la charge (hydruration) d'un alliage commerciale à base de LaNi5 et d'un alliage MgNi obtenu par broyage mécanique. Nous avons ainsi pu séparer les signaux générés par la fracturation des particules d’hydrures métalliques de ceux associés à la formation de bulles de H2, ce qui a permis d’établir les mécanismes qui régissent leur fracturation. Par la suite, un montage expérimental, constitué d’une cellule électrochimique connectée à un capteur de force en compression et d’un équipement d’EA, a été mis point pour suivre in-situ la fracturation et la force générée par l’expansion/contraction lors du cyclage des électrodes MgNi et LaNi5. Nous avons ainsi pu confirmer que l’expansion/contraction volumique de l’alliage MgNi est plus progressif que pour l’alliage à base de LaNi5. Par la suite, l’étude comparée par EA des alliages MgNi, Mg0.9Ti0.1Ni et Mg0.9Ti0.1NiAl0.05 a permis de mettre en évidence l'influence de leur composition sur leur résistance à la pulvérisation. Finalement, nous avons étudié en détail l’influence de l’addition de palladium dans l’alliage Mg0.9Ti0.1NiAl0.05 sur son comportement électrochimique et sa résistance à la fracturation. / The pulverization (cracking) of active materials in batteries, induced by their volume change during charge/discharge cycles, accentuates their corrosion by the electrolyte and/or leads to a loss of electronic connectivity within the electrode, which notably reduces their cycle life. This particularly occurs for metallic hydrides used in Ni-MH batteries. To date, the evaluation of their cracking is generally limited to post mortem observations of the electrodes by microscopy, which does not allow for a detailed analysis of the decrepitation process. In this respect, one of our main research objectives was to develop an innovative and efficient analysis method based on acoustic emission (AE) for in situ monitoring of the cracking of negative electrodes for Ni-MH batteries. As a first step, a detailed analysis of the acoustic signals generated during the charge (hydriding) of a commercial LaNi5-based alloy and a MgNi alloy obtained by mechanical alloying was performed. This allowed separating the signals generated by the cracking of the metallic hydride particles from those induced by the formation of H2 bubbles. We have shown that the mechanism which governs the pulverization of the MgNi alloy remarkably differs from that of the LaNi5-based alloy. In a second step, an experimental set-up made of an electrochemical cell linked to a compression force cell and an AE equipment was elaborated, in order to monitor concomitantly the cracking and the force generated by the expansion/contraction of the MgNi and LaNi5 during cycling. We have thereby been able to confirm that the volume expansion/contraction of the MgNi alloy is more progressive than that of the LaNi5 alloy. The AE-based comparative study of MgNi, Mg0.9Ti0.1NiAl5 and Mg0.9Ti0.1NiAl0.05 alloys then allowed demonstrating the positive effect of the partial Mg substitution by Ti and adding of Al on the alloy decrepitation resistance. As a final step, we have studied the impact of palladium addition in the Mg0.9Ti0.1NiAl0.05 alloy on its electrochemical behaviour and cracking resistance.

Non-destructive testing has become necessary to ensure the quality of materials and components either in-service or at the production stage. This requires the use of a rapid, robust and reliable testing technique. As a main testing technique, the ultrasound technology has unique abilities to assess the discontinuity location, size and shape. Such information play a vital role in the acceptance criteria which are based on safety and quality requirements of manufactured components. Consequently, an extensive usage of the ultrasound technique is perceived especially in the inspection of large scale composites manufactured in the aerospace industry. Significant technical advances have contributed into optimizing the ultrasound acquisition techniques such as the sampling phased array technique. However, acquisition systems need to be complemented with an automated data analysis procedure to avoid the time consuming manual interpretation of all produced data. Such a complement would accelerate the inspection process and improve its reliability. The objective of this thesis is to propose an analysis chain dedicated to automatically process the 3D ultrasound volumes obtained using the sampling phased array technique. First, a detailed study of the speckle noise affecting the ultrasound data was conducted, as speckle reduces the quality of ultrasound data. Afterward, an analysis chain was developed, composed of a segmentation procedure followed by a classification procedure. The proposed segmentation methodology is adapted for ultrasound 3D data and has the objective to detect all potential defects inside the input volume. While the detection of defects is vital, one main difficulty is the high amount of false alarms which are detected by the segmentation procedure. The correct distinction of false alarms is necessary to reduce the rejection ratio of safe parts. This has to be done without risking missing true defects. Therefore, there is a need for a powerful classifier which can efficiently distinguish true defects from false alarms. This is achieved using a specific classification approach based on data fusion theory. The chain was tested on several ultrasound volumetric measures of Carbon Fiber Reinforced Polymers components. Experimental results of the chain revealed high accuracy, reliability in detecting, characterizing and classifying defects.

According to the 2019 Canadian infrastructure report card, a concerning amount of municipal infrastructure is in poor or very poor condition. The infrastructure in this condition requires immediate action for rehabilitation or replacement. For concrete infrastructure, an effective repair can extend its service life and ensure that the services it provides continue to meet the community expectations. However, unfavorable environmental factors such as repeated/cyclic loads and freezing and thawing cycles adversely affect the bond between substrate concrete and repair materials, which lowers the structural capacity of repaired structures. So far, researchers have found that bond strength of repair can be affected by surface roughness, surface moisture, chemical adhesion or cohesion, curing regime, properties of substrate and repair materials, use of bond agent, and curing regimes. These findings are mostly based on the studies that focused on cold-jointed cylinders or beams, but in real-life repair situations, repairs of beams or slabs are located at either tension or compression side of the structure. Currently, there is no comprehensive study that investigates the bond of concrete repair under a combination of freezing and thawing and repeated/cyclic loading conditions. In addition, it is challenging to provide a rapid and non-destructive evaluation of the bond deterioration of repair materials. To address these issues systematically, this dissertation breaks the task into four phases. Phase (I) focuses on the development of an engineered “crack-free” repair mix that contains polypropylene (PP) fiber. A novel method is used to surface treat the PP fibers with supplementary cementitious materials. The effectiveness of surface-treating fibers for improved bond strength and reduced cracking is investigated. The compressive, tensile, and flexural strength of this engineered repair mix are determined and compared with two commercially available repair materials. The results from Phase I show that by adding 0.2% (by weight) Metakaolin-treated fibers into concrete mix, the compressive strength improves by up to 15.7% compared to mixes with untreated fibers. This study achieved a strength increase of 13.5% as compared to the reported 3.3% in other studies that use 25 times the amount of metakaolin used in this study. The experimental results confirm that at 0.2% dosage level, the use of novel surface treating technique is a cost-effective way to improve the strength of repair materials. Phase (II) focuses on characterizing the bond strength of various repair systems after freezing-thawing (FT) damage using both non-destructive and destructive methods. Two innovative sounding methods, which overcome the subjectivity of the traditional chain drag method, are used to evaluate FT damage non-destructively. In the experimental study, beams with a U-shaped cut are made to simulate conditions experienced by a concrete structure during a typical repair project. Three types of repair materials are used including cementitious repair concrete, cementitious repair mortar, and polymer-modified cementitious mortar. After up to 300 cycles of freeze-thaw exposure, resonant frequency and bond flexural strength of the prismatic specimens are determined. The empirical equations relating Non-destructive test (NDT) measurements and flexural bond strength of the repaired structures after freeze-thaw (FT) exposure are proposed. The results from Phase II show that the change in dynamic modulus of elasticity determined from NDTs agrees well with the change in other measurements including flexural bond strength, interfacial crack width, and mass loss after freeze-thaw exposure. In this study, linear relationships are established between dynamic modulus of elasticity and flexural bond strength for both cementitious and polymer-modified cementitious repair mortar with a coefficient of determination ranging between 0.87 and 0.95. The proposed empirical models can be used to predict bond flexural strength of repaired structures based on NDT measurement. Also, it was found that the samples repaired with polymer-modified cementitious mortar (Mix P) have superior FT resistance compared to other repaired samples. Phase (III) focuses on investigating the structural capacity and bond performance of repaired beams after cyclic/repeated loading. To accelerate the test process, a novel modified loading regime consisting of cycle groups of increasing cyclic/repeated stress amplitude is proposed. The models proposed by literature and current codes and standards are used to validate the results. Phase (IV) focuses on the development of the damage models for both individual and combined FT and cyclic loading exposure on repaired concrete structures. The results in phase III show the feasibility of using the Palmgren-Miner rule and Goodman linear model to estimate the fatigue life of repaired structures. This was confirmed within the context of this study. This study established the usefulness of using groups of increasing cyclic stress amplitude to accelerate the fatigue test process. The two-million cycle fatigue endurance limit estimated using cycle groups of Mix S (70.8%) was very similar to what was reported in the literature (71%) using the traditional time-consuming cyclic loading method. This study found that the formulas proposed by CSA 23.3 can effectively predict the moment resistance of both intact (control) and repaired RC beams. The ratio of experimental moment resistance values to its predictions ranges from 0.91 to 1.04. Based on the experimental results of previous three phases, an empirical model that predicted the fatigue service life of FT-damaged concrete structures is proposed. Future research requires a more comprehensive study on the FT performance of various polymer-modified cementitious mortars of different mix designs in repairing concrete structures. By increasing the number of tested specimens, a better relationship could be established between destructive and NDT methods. Future research is also required to explore the combined effect of FT and cyclic loading on repaired RC structures experimentally. / Graduate / 2023-03-22

Le contrôle non destructif est devenu nécessaire pour assurer la qualité des matériaux et des composants soit en service ou à l'étape de la production. Ceci nécessite l'utilisation d'une technique d’inspection rapide, robuste et fiable. En tant que technique de contrôle principale, la technologie des ultrasons a des capacités uniques pour évaluer la position, la taille et la forme des discontinuités. Ces informations ont un rôle essentiel dans les critères d'acceptation qui sont fondés sur la sécurité et les exigences de qualité des composants fabriqués. Par conséquent, un usage intensif de la technique des ultrasons apparaît notamment dans l'inspection des composites fabriqués à grande échelle dans l'industrie aérospatiale. D'importants progrès techniques ont contribué à l'optimisation des techniques d'acquisition par ultrasons telles que la technique de "Sampling Phased Array". Cependant, les systèmes d'acquisition doivent être complétés par une procédure d'analyse automatisée de données afin d'éviter l'interprétation manuelle fastidieuse de toutes les données produites. Un tel complément permet d'accélérer le processus d'inspection et d'améliorer sa fiabilité. L'objectif de cette thèse est de proposer une chaîne d’analyse dédiée au traitement automatique des volumes échographiques 3D obtenus en utilisant la technique Sampling Phased Array. Tout d'abord, une étude détaillée du bruit de speckle affectant les données échographiques a été effectuée, puisque ce type de bruit réduit la qualité des données échographiques. Ensuite, une chaîne d’analyse complète a été développée, constituée d'une procédure de segmentation suivie d'un processus de classification. La méthodologie de segmentation proposée est adaptée aux données ultrasonores 3D et a pour objectif de détecter tous les défauts potentiels à l'intérieur du volume d'entrée 3D. La procédure de segmentation étant en priorité dédiée à la détection des défauts qui est vitale, une difficulté principale est le taux élevé de fausses alarmes qui peuvent être détectées également. La classification correcte des fausses alarmes est nécessaire afin de réduire le taux de rejet des pièces saines. Cela doit être fait sans risquer la perte des vrais défauts. Par conséquent, la segmentation doit être suivie d'un processus de classification efficace qui doit distinguer les défauts réels des fausses alarmes. Ceci a été réalisé en utilisant une approche de classification spécifique basée sur une approche de fusion de données. La chaîne complète d'analyse a été testée sur plusieurs mesures ultrasonores volumiques de composites plastiques à renfort fibre de carbone. Les résultats expérimentaux de la chaîne ont révélé une grande précision ainsi qu'une très bonne fiabilité de détection, de caractérisation et de classification des défauts avec un taux très faible de fausses alarmes. / Non-destructive testing has become necessary to ensure the quality of materials and components either in-service or at the production stage. This requires the use of a rapid, robust and reliable testing technique. As a main testing technique, the ultrasound technology has unique abilities to assess the discontinuity location, size and shape. Such information play a vital role in the acceptance criteria which are based on safety and quality requirements of manufactured components. Consequently, an extensive usage of the ultrasound technique is perceived especially in the inspection of large scale composites manufactured in the aerospace industry. Significant technical advances have contributed into optimizing the ultrasound acquisition techniques such as the sampling phased array technique. However, acquisition systems need to be complemented with an automated data analysis procedure to avoid the time consuming manual interpretation of all produced data. Such a complement would accelerate the inspection process and improve its reliability. The objective of this thesis is to propose an analysis chain dedicated to automatically process the 3D ultrasound volumes obtained using the sampling phased array technique. First, a detailed study of the speckle noise affecting the ultrasound data was conducted, as speckle reduces the quality of ultrasound data. Afterward, an analysis chain was developed, composed of a segmentation procedure followed by a classification procedure. The proposed segmentation methodology is adapted for ultrasound 3D data and has the objective to detect all potential defects inside the input volume. While the detection of defects is vital, one main difficulty is the high amount of false alarms which are detected by the segmentation procedure. The correct distinction of false alarms is necessary to reduce the rejection ratio of safe parts. This has to be done without risking missing true defects. Therefore, there is a need for a powerful classifier which can efficiently distinguish true defects from false alarms. This is achieved using a specific classification approach based on data fusion theory. The chain was tested on several ultrasound volumetric measures of Carbon Fiber Reinforced Polymers components. Experimental results of the chain revealed high accuracy, reliability in detecting, characterizing and classifying defects.

L’évaluation des performances des procédures de Contrôle Non Destructifs (CND) en aéronautique est une étape clé dans l’établissement du dossier de certification de l’avion. Une telle démonstration de performances est faite à travers l’établissement de probabilités de détection (Probability Of Detection – POD), qui intègrent l’ensemble des facteurs influents et sources d’incertitudes inhérents à la mise en œuvre de la procédure. Ces études, basées sur des estimations statistiques faites sur un ensemble représentatif d’échantillons, reposent sur la réalisation d’un grand nombre d’essais expérimentaux (un minimum de 60 échantillons contenant des défauts de différentes tailles, qui doivent être inspectés par au moins 3 opérateurs [1]), afin de recueillir un échantillon suffisant pour une estimation statistique pertinente. Le coût financier associé est élevé, parfois prohibitif, et correspond majoritairement à la mise en œuvre des maquettes servant aux essais. Des travaux récents [2-5] ont fait émerger une approche de détermination de courbes POD utilisant la simulation des CND, notamment avec le logiciel CIVA. L’approche, dite de propagation d’incertitudes, consiste à : - Définir une configuration nominale d’inspection, - Identifier l’ensemble des paramètres influents susceptibles de varier dans l’application de la procédure, - Caractériser les incertitudes liées à ces paramètres par des lois de probabilités, - Réaliser un grand nombre de simulations par tirage aléatoire des valeurs prises par les paramètres variables selon les lois de probabilités définies. Le résultat de cet ensemble de simulations constitue enfin la base de données utilisée pour l’estimation des POD. Cette approche réduit de façon très importante les coûts d’obtention des POD mais est encore aujourd’hui sujette à discussions sur sa robustesse vis-à-vis des données d’entrée (les lois de probabilité des paramètres incertains) et sur la prise en compte des facteurs humains. L’objectif de cette thèse est de valider cette approche sur des cas d’application AIRBUS et d’en améliorer la robustesse afin de la rendre couramment utilisable au niveau industriel, notamment en la faisant accepter par les autorités de vol (FAA et EASA). Pour ce faire le thésard devra mener des campagnes de validations des codes de simulation des CND, mettre en œuvre la méthodologie décrite plus haut sur les cas d’application AIRBUS, puis proposer et mettre en œuvre des stratégies d’amélioration de la robustesse de la méthode vis-à-vis des données d’entrée et des facteurs liés à l’humain. / The performance assessment of non-destructive testing (NDT) procedures in aeronautics is a key step in the preparation of the aircraft's certification document. Such a demonstration of performance is done through the establishment of Probability of Detection (POD) laws integrating all sources of uncertainty inherent in the implementation of the procedure. These uncertainties are due to human and environmental factors in In-Service maintenance tasks. To establish experimentally these POD curves, it is necessary to have data from a wide range of operator skills, defect types and locations, material types, test protocols, etc. Obtaining these data evidences high costs and significant delays for the aircraft manufacturer. The scope of this thesis is to define a robust methodology of building POD from numerical modeling. The POD robustness is ensured by the integration of the uncertainties through statistical distributions issued from experimental data or engineering judgments. Applications are provided on titanium beta using high frequency eddy currents NDT technique. First, an experimental database will be created from three environments: laboratory, A321 aircraft and A400M aicraft. A representative sample of operators, with different certification levels in NDT technique, will be employed. Multiple inspection scenarios will be carried out to analyze these human and environmental factors. In addition, this study will take into account the impact of using different equipments in the HFEC test. This database is used, subsequently, to build statistical distributions. These distributions are the input data of the simulation models of the inspection. These simulations are implemented with the CIVA software. A POD module, based on the Monte Carlo method, is integrated into this software. This module will be applied to address human and ergonomic influences on POD. Additionally this module will help us to understand in a better way the equipment impact in POD curves. Finally, the POD model will be compared and validated with the experimental results developed.