Les films minces sont abondamment utilisés pour protéger ou fonctionnaliser les surfaces. Les contraintes mécaniques peuvent cependant entraîner la ruine de ces structures par la propagation de fissures ou leur décollement. Nous présentons deux systèmes expérimentaux qui amènent à s'interroger sur les limites de validité des critères de stabilité communément admis. Pour une couche de sol- gel présentant une énergie d'adhésion modérée avec son substrat de silicium, nous observons la propagation de fissures dans des films réputés stables. Les motifs de propagation sont étonnement réguliers (en forme de spirales ou d'allées de croissants). Nous caractérisons expérimentalement cette propagation. Nous mettons en évidence un nouveau mode de propagation de fissure où la délamination et la fissure transverse collaborent. Nous montrons l'existence d'une taille d'interaction robuste entre fissures indépendantes du chargement et des énergies de rupture. Nous proposons un modèle simple permettant de prédire les conditions de propagation et la sélection des motifs. Nous caractérisons enfin la dynamique de propagation de telles fissures. Dans un second système expérimental motivé par les applications en électronique flexible, nous nous intéressons à des films nanométriques d'oxyde de zinc déposés sur des substrats de polymère. La rigidité du substrat est alors faible devant celle de la couche. Nous décrivons la fragmentation du film et proposons une extension d'un modèle de couche élastique sur fondation élasto-plastique. Enfin, nous nous intéressons à la compression et à la fragmentation d'un multicouche comportant une fine épaisseur d'argent. / Nanometer to micrometer thin film coatings are extensively used in material science to protect and functionalize surfaces. Coating processes however generally result into residual strains and may induce the propagation of cracks with dramatic consequences on film reliability. We present two experimental models which challenges the usual stability criteria for thin films. For a thin sol-gel layer moderatly adherent to a silicon substrate, we observe fracture propagation in coatings considered stable. Moreover, intriguing cracks of regular geometry are found to self-replicate an initial triggering pattern independently from the local material properties. We present a novel mode of fracture which involves the simultaneous progression of both, a crack and a front of delamination. We describe the fracture mechanism with universal energy arguments and provide a simple model describing the crack path. We eventually characterize the dynamics of the propagation. In a second model experiment, we study the fragmentation of coating deposited on a compliant substrate (motivated by flexible electronics application). We describe the fragmentation and propose an extension to an elastic layer deposited on an elastic foundation to an elasto-plastic case. Eventually, we study the compression and fragmentation of a zinc oxyde and silver multilayer

Multilayered materials and structures are of special interest to both academic researchers and industrial engineers as they have been used in an increasing number of applications, such as micro- electromechanical system (MEMS) on polymer substrate, protective coating on metal structure for anti-corrosion, ceramic coating on metal substrate for abrasion resistance, thermal barrier coatings, metal or metal oxide coating on metal-coated polymer for reflectance tuning and protection, as well as laminated composites and structures, etc. However, the surface layer and joint interface are commonly prone to premature failures because of cracking and delamination due to their different thermal and mechanical properties. In return, the premature failures will affect the performance and structural integrity of the device and eventually cause the failure of the multilayered structures to perform their functions. Therefore, it is essential to understand the mechanical behavior and corresponding failure mechanisms of the multilayered systems. This Ph.D. dissertation focuses on the study of opening-mode fracture (OMF) behavior and interfacial delamination in different types of multilayered structures, such as the aluminum plate or wire with alumina protective coating, multilayered advanced polymeric reflectors, and asphalt pavements. In addition, another failure mechanism, i.e. the material degradation and aging, is also studied. Firstly, a two-dimensional (2D) elasoplastic fracture model in Cartesian coordinates is developed to study the OMF in the thin alumina film fully bonded to an aluminum plate undergoing large- scale yielding. The stress field in the coating layer is described by one section between two adjacent cracks. The 2D plane strain formulations are employed to analyze the elastic field in the thin film, while a one-dimensional (1D) linear hardening plastic model is applied to account for the large plastic deformations in the substrate under substantial yielding. An elastoplastic shear lag model is established to transfer the tensile stress in the substrate to the thin film. General formulations and explicit expressions of the elastic/elastoplastic solutions of the thin film/substrate system under different loading stages have been presented. The elastic field in the thin film is then verified with the finite element (FE) results. The fracture energy release rate (ERR) is calculated and corresponding elastoplastic fracture analysis is conducted. Experimental characterization is further conducted to validate the present model; the results show that this fracture modle can capture the fracture initiation, infilling, and saturation in the thin film successfully. This model has been extended to cylindrical coordinates, where the alumina coating is fully bonded to an aluminum wire/rod. Due to the axial symmetry, the proposed 2D elasoplastic fracture model has been reproduced in polar coordinates and be used to study the OMF behavior of alumina coating fully bonded to an aluminum wire. For the case where thermal loading is applied on coating/substrate structures, neither the plane strain nor plane stress assumption can be applied because the thermal loading would introduce multi axial normal stress, therefore, a three-dimensional (3D) elastic fracture model is then developed to study the OMF in the coating fully bonded to the elastic substrate. When the temperature change reaches a certain level, block cracking will initiate in the surface layer to release the accumulated thermal stress. For simplicity, we assume the top surface of the coating would keep flat and in a rectangular shape after deformation. Then the elastic field in both coating and substrate is analyzed and verified with the FE results. The fracture ERR is then obtained based on the solved elastic field and used to analyze the fracture initiation, infilling, and saturation. In order to verify the fracture analysis, the theoretical fracture analysis results are compared with FE simulation results based on the cohesive zone model (CZM) and experimental data from the literature. The good agreement demonstrates the accuracy of the proposed 3D fracture model. In addition, this model for coating/substrate system is extended to study multilayered structures with arbitrary number of layers. In order to verify this extended model, the predicted elastic field in an advanced polymeric solar reflector is compared with FE simulation results and parametric studies are conducted to investigate the effect of geometry on the accuracy of this model. Furthermore, the fracture behavior of the surface layer in the advanced polymeric solar reflector is studied using the calculated fracture ERR. Additionally, the delamination behavior, as another common failure mode of the coating/substrate structures, is then studied. The delamination fracture energy of a multilayered glass solar reflec- tor is tested by employing the width-tapered beam method. The testing results indicate that the weakest interface of the multilayered solar reflector would be the glass-copper interface with a de- lamination fracture energy 4.4 J/m2. Using the tested fracture energy as an input, an FE model is built based on the CZM and the returned peeling force from simulation is then compared with the test results to verify the accuracy of the test method. The good agreement between the simulation and test results demonstrates that the width-tapered beam method is accurate enough to measure the delamination fracture energy of this multilayered solar reflector. Additionally, the effect of aging on the delamination fracture energy is investigated by measuring the delamination fracture energy after 50 hrs’ accelerated aging test. The results show that the aging has minor effect of delamination fracture energy for samples with alumina (Al2O3) protective coating, while it reduces the delamination fracture energy for samples with titania (TiO2) protective coating. As another failure mechanism, the material degradation or aging behavior is studied in this dissertation. The weight percentage of oxygen (WPO) in three types of asphalt binders extracted from reclaimed asphalt pavements (RAPs) and one extracted from fresh Hot Mix Asphalt (HMA), that have been aged under continuous ultraviolet (UV) or UV/moisture/condensation exposure for different period, is measured using a energy-dispersive X-ray spectroscopy (EDX). Then the tested data are fitted based on two classic aging models, namely the fast-rate constant-rate (FRCR) and nonlinear differential dynamic (NDD) models. The good fitted results show that both FRCR and NDD models can capture the aging behavior of asphalt binders extracted from both RAPs and fresh HMA under continuous UV or UV/moisture/condensation exposure. Meanwhile, although exposed under UV for the same time, the WPO in samples after UV/moisture/condensation aging are lower than those in samples after continuous UV aging, which indicates that condensation and moisture reduce the UV-induced photo-oxidative aging rate.

The employment of composite materials in the aerospace industry has been gradually considered due to the fundamental lightweight and strength characteristics that these type of materials offer. The science material and technological progress that has been reached, matches perfectly with the requirements for high-performance materials in aircraft and aerospace structures, thus, the development of primary structure elements applying composite materials became something very convenient. It is extremely important to pay attention to the failure modes that influence composite materials performances, since, these failures lead to a loss of stiffness and strength of the laminate. Delamination is a failure mode present in most of the damaged structures and can be ruinous, considering that, the evolution of interlaminar defects can carry the structure to a total failure followed by its collapse. Different techniques are usually adopted to accurately predict the behavior of damaged structures but, due to the complex nature of failure phenomena, there is not an established pattern. The present research project aims to develop a delamination propagation model to estimate a progressive interlaminar delamination failure in laminated composite materials and to allow the prediction of material\'s degradation due to the delamination phenomenon. Experimental tests assisted by ASTM Standards were performed to determine material\'s parameter, like the strain energy release rate, using GFRPs laminated composites. The delamination propagation model proposed was implemented as subroutines in FORTRAN language (UMAT-User Material Subroutine) with formulations based on the Fracture Mechanics. Finally, the model was compiled beside with the commercial Finite Element program ABAQUSTM. / O emprego de materiais compósitos na indústria aeroespacial tem sido gradualmente utilizado devido às suas características fundamentais, como peso leve e alta rigidez, que este tipo de material oferece. Tanto a ciência do material como o desenvolvimento tecnológico que se tem logrado, possibilitaram que estes materiais cumprissem com os requisitos de desempenho para aplicações em estruturas aeronáuticas e aeroespaciais, por tanto, o desenvolvimento de elementos de estruturas primárias usando materiais compósitos, passou a ser muito conveniente. É de extrema importância prestar atenção aos modos de falha que comprometem a performance dos materiais compósitos, uma vez que, estas falhas levam a uma perda de resistência e rigidez do laminado. A delaminação é um modo de falha presente na maioria de estruturas danificadas e pode ser desastroso, considerando que, a evolução dos defeitos interlaminares podem levar a estrutura a falhar seguido pelo colapso estructural. Diferentes técnicas são geralmente adotadas para prever, de maneira correta, o comportamento de estruturas danificadas, porém, devido à natureza complexa do fenômeno de falha, não existe um padrão estabelecido. O presente trabalho de pesquisa visa desenvolver um modelo de delaminação e de propagação da delaminação para estimar a evolução da falha interlaminar em materiais compósitos laminados e permitir a predição do comportamento do material com a evolução da delaminação. Ensaios experimentais auxiliados por normas ASTM foram realizados para determinar parâmetros do material, tais como, as taxas de liberação de energia de deformação, usando materiais compósitos laminados de matriz polimérica reforçada com fibra de vidro. O modelo de propagação da delaminação proposto, foi implementado como uma sub-rotina em linguagem FORTRAN (UMAT – User Material) com formulações baseadas na Mecânica da Fratura. Finalmente, o modelo foi compilado com o software comercial de Elementos Finitos, ABAQUSTM.

Infrastructure deterioration is an international problem requiring significant attention. One particular manifestation of this deterioration is the occurrence of sub-surface cracking (delaminations) in reinforced concrete bridge decks. Of many techniques available for inspection, air-coupled impact-echo testing, or sounding, is a non-destructive evaluation technique to determine the presence and location of delaminations based upon the acoustic response of a bridge deck when struck by an impactor. In this work, two automated air-coupled impact echo sounding devices were designed and constructed. Each device included fast and repeatable impactors, moving platforms for traveling across a bridge deck, microphones for air-coupled sensing, distance measurement instruments for keeping track of impact locations, and signal processing modules. First, a single-channel automated sounding device was constructed, followed by a multi channel system that was designed and built from the findings of the single-channel apparatus. The multi channel device performed a delamination inspection in the same manner as the single-channel device but could complete an inspection of an entire traffic lane in one pass. Each device was tested on at least one concrete bridge deck and the delamination maps produced by the devices were compared with maps generated from a traditional chain-drag sounding inspection. The comparison between the two inspection approaches yielded high correlations for bridge deck delamination percentages. Testing with the two devices was more than seven and thirty times faster, respectively, than typical manual sounding procedures. This work demonstrates a technological advance in which sounding can be performed in a manner that makes complete bridge deck scanning for delaminations rapid, safe, and practical.

Delaminations in concrete bridge decks result primarily from corrosion of the reinforcing bars (or rebar). This corrosion leads to volumetric expansion of the rebar. When the rebar expands, concrete cracks, and there is a localized separation of the concrete cover from the underlying concrete. Impact-echo testing is an effective technique to map delaminations on concrete bridge decks. However, mapping speed is limited by necessary retrieval of the impactor for traditional tests. To achieve higher scanning speeds, it is advantageous to use both a non-contact measurement (air-coupled impact-echo) and disposable-impactor excitation. Disposable impactors have the potential advantage of achieving greater deck scanning speeds because they do not need to be retrieved, and they can also be used with air-coupled measurement systems. This thesis reports impact excitation of concrete using disposable impactors such as water droplets and ice balls. The impact characteristics of these impactors are compared with those of steel balls and chain links. Comparing the acoustic recordings on intact and delaminated concrete surface shows that water droplets and ice balls are able to excite flexural resonant modes associated with delamination defects. The use of water droplets and ice balls for shallow delamination detection in concrete is thus demonstrated.

The high stiffness to weight ratio and fatigue resistance make carbon fibre composites suitable for both military and large civil aircraft. The limited ability of current numerical methods to capture the complex growth of damage in laminated composites leads to a conservative design approach applied in today??s composite aircraft structures. The aim of the presented research was to develop an improved methodology for the failure prediction of laminated composites containing delaminations located between arbitrary layers in the laminate, and to extend the investigations to composite structures subjected to barely visible impact damage (BVID). The advantages of fracture mechanics-based methodologies to predict interlaminar failure in composite structures were identified, from which the crack tip element (CTE) approach and the virtual crack closure technique (VCCT) were selected for assessment. Extensive validation of these fracture mechanics methods is presented on a number of composite structures ranging from coupons to large stiffened panels. It was shown that the VCCT was relatively insensitive to the crack front mesh size, whilst predictions using the CTE methodology were significantly influenced by the element size. Based on the obtained results modelling guidelines for the VCCT and CTE were established. Significant contribution of this research to the field of the analysis of composite structures was the development of a novel test method for the evaluation of embedded single and multi-level delaminations. The test procedure of the single delamination specimen was proposed as an analogous test to conventional compression experiments. The transverse test overcame the inherent problems of in-plane compression testing and produced less scatter of experimental measurements. Quantitative analysis of numerical results employing the validated finite element modelling approaches showed that the failure load and location were in agreement with experiments. Furthermore, new modelling techniques for composite structures containing BVID proposed in this research produced good correlation with test data from the compression after impact (CAI) test. The study of BVID provided a significant contribution toward the knowledge of the applicability of implicit FE solvers to predict failure of CAI specimens as well as the criticality of centrally impacted specimens.

The use of composite structures in engineering applications has proliferated over the past few decades due to its distinct advantages namely: high structural performance, corrosion resistance, and high strength/weight ratio. However, they also come with a set of disadvantages, i.e. they are prone to fibre breakage, matrix cracking and delaminations. These types of damage are often invisible and if undetected, could lead to catastrophic failures of structures. Although there are systems to detect such damage, the criticality assessment and prognosis of the damage is often much more difficult to achieve. The research study conducted here resulted in the development of a Structural Health Monitoring (SHM) system for a 2D polymeric composite T-joint, used in maritime structures. The SHM system was found to be capable of not only detecting the presence of multiple delaminations in a composite structure, but also capable of determining the location and extent of all t he delaminations present in the T-joint structure, regardless of the load (angle and magnitude) acting on the structure. The system developed relies on the examination of the strain distribution of the structure under operational loading. This SHM system necessitated the development of a novel pre-processing algorithm - Damage Relativity Assessment Technique (DRAT) along with a pattern recognition tool, Artificial Neural Network (ANN), to predict and estimate the damage. Another program developed - the Global Neural network Algorithm for Sequential Processing of Internal sub Networks (GNAISPIN) uses multiple ANNs to render the SHM system independent to variations in structural loading and capable of estimating multiple delaminations in composite T-joint structures. Upto 82% improvement in detection accuracy was observed when GNAISPIN was invoked. The Finite Element Analysis (FEA) was also conducted by placing delaminations of different sizes at various locations in two structures, a composite beam and a T-joint. Glass Fibre Reinforced Polymer T-joints were then manufactured and tested, thereby verifying the accuracy of the FEA results experimentally. The resulting strain distribution from the FEA was pre-processed by the DRAT and used to trai n the ANN to predict and estimate damage in the structures. Finally, on testing the SHM system developed with strain signatures of composite T-joint structures, subjected to variable loading, embedded with all possible damage configurations (including multiple damage scenarios), an overall damage (location & extent) prediction accuracy of 94.1% was achieved. These results are presented and discussed in detail in this study.

Impulse technology is a process in which water is removedfrom a wet paper web by the combined action of mechanicalpressure and intense heat. This results in increased dewateringrates, increased smoothness on the roll side of the sheet, andincreased density. Although the potential benefits of impulsepressing have been debated over the past thirty years, itsindustrial acceptance has been prevented by web delamination,which is defined as a reduction in the z-directional strengthof paper. This thesis deals with the mechanism of heat transfer withphase change during impulse pressing of wet paper. The resultsof four complementary experimental studies suggest that littleor no steam is formed in an impulse nip prior to the point ofmaximum applied load. As the nip is unloaded and the hydraulicpressure decreases, hot liquid water flashes to steam. Weadvance the argument that the force expressed upon flashing canbe used to displace liquid water, in a mechanism similar tothat originally proposed by Wahren. Additionally, modelexperiments performed in a novel experimental facility suggestthat the strength of flashing-assisted displacement dewateringcan be maximized by controlling the direction of steam venting.If this solution could be exploited in a commercially viableimpulse press, delamination would cease to be an issue ofconcern. The thesis includes a study of the web structure ofdelaminated paper. Here, we characterized delaminated paper bythe changes in transverse permeability and cross-sectionalsolidity profiles measured as a function of pressingtemperature. We found no evidence that wet pressing and impulsepressing induced stratification in non-delaminated sheets andconcluded that the parabolic solidity profiles observed weredue to capillary forces present during drying. Further, thepermeability of mechanically compressed never-dried samples wasfound to be essentially constant for pressing temperatureslower than the atmospheric boiling point of water and toincrease significantly at higher pressing temperatures. Wepropose this to be a result of damage to the cell wall materialdue to flashing of hot liquid water in the fiber walls andlumina. Finally, we present a method and an apparatus formeasurement of the thermal properties of water-saturated paperwebs at temperatures and pressures of interest for commercialhigh-intensity processes. After validation, the method wassuccessfully applied to measure the thermal conductivity,thermal diffusivity and volumetric heat capacity ofwater-saturated blotter paper as functions of temperature andsolids content. Here, we found that the thermal conductivityincreased with solids content in the range from 30%\ to 55%,which is in conflict with the commonly stated assumptions of adecreasing trend. We propose that this discrepancy could be dueto the thermal conductivity of air-free fibers wetted byunpressable water only, being significantly different from thatof dry cellulose.

Within the framework of this thesis, three innovative electrochemical devices have been studied. A part of the work is devoted to an already existing device, laminates which are debonded by the application of a voltage. This type of material can potentially be used in a wide range of applications, including adhesive joints in vehicles to both reduce the total weight and to simplify the disassembly after end-of-life, enabling an inexpensive recycling process. Although already a functioning device, the development and tailoring of this process was slowed by a lack of knowledge concerning the actual electrochemical processes responsible for the debonding. The laminate studied consisted of an epoxy adhesive, mixed with an ionic liquid, bonding two aluminium foils. The results showed that the electrochemical reaction taking place at the releasing anode interface caused a very large increase in potential during galvanostatic polarization. Scanning electron microscopy images showed reaction products growing out from the electrode surface into the adhesive. These reaction products were believed to cause the debonding through swelling of the anodic interface so rupturing the adhesive bond. The other part of the work in this thesis was aimed at innovative lithium ion (Li‑ion) battery concepts. Commercial Li-ion batteries are two-dimensional thin film constructions utilized in most often mechanically rigid products. Two routes were followed in this thesis. In the first, the aim was flexible batteries that could be used in applications such as bendable reading devices. For this purpose, nano-fibrillated cellulose was used as binder material to make flexible battery components. This was achieved through a water-based filtration process, creating flexible and strong papers. These paper-based battery components showed good mechanical properties as well as good rate capabilities during cycling. The drawback using this method was relatively low coulombic efficiencies believed to originate from side-reactions caused by water remnants in the cellulose structure. The second Li-ion battery route comprised an electrochemical process to coat carbon fibers, shown to perform well as negative electrode in Li-ion batteries, from a monomer solution. The resulting polymer coatings were ~500 nm thick and contained lithium ions. This process could be controlled by mainly salt content in the monomer solution and polarization time, yielding thin and apparently pin-hole free coatings. By utilizing the carbon fiber/polymer composite as integrated electrode and electrolyte, a variety of battery designs could possibly be created, such as three-dimensional batteries and structural batteries. / <p>QC 20130403</p>

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