Orientador: Fernando Galembeck / Tese (doutorado) - Universidade Estadual de Campinas, Instituto de Quimica / Made available in DSpace on 2018-08-11T02:26:13Z (GMT). No. of bitstreams: 1 Braganca_FabiodoCarmo_D.pdf: 5432342 bytes, checksum: bed10dd45e0418cfb0468e2a4a0df2ae (MD5) Previous issue date: 2008 / Resumo: Este trabalho mostra a influência das interações eletrostáticas nas propriedades físicas e morfológicas de nanocompósitos poliméricos com argila preparados a partir de dispersões aquosas, e as características estruturais de laminados nanoestruturados autoadesivos preparados com borracha natural e argila. A preparação dos nanocompósitos envolveu a utilização de argilas produzidas através da troca do sódio por potássio, lítio e cálcio e a mistura destas com um látex estireno-acrílico sintetizado em laboratório. O tipo e o grau de hidratação dos cátions influenciaram de maneira significativa as propriedades mecânicas dos nanocompósitos. Mapas elementares baseados em espectroscopia por perda de energia de elétrons mostraram que os contra-íons estão presentes nas regiões onde se sobrepõem polímero e argila. Este resultado forneceu subsídios para a proposição de um modelo, onde os contra-íons atuam como uma ponte iônica entre as lâminas de argila e a matriz polimérica, ambas contendo excesso de cargas negativas. O modelo de adesão eletrostática mediada por contra-íons foi aplicado com sucesso na preparação de nanocompósitos com polietileno de baixa densidade e argila em meio aquoso. Os nanocompósitos preparados apresentaram aumento de aproximadamente 40% no módulo elástico frente ao polímero puro, quando 4% em massa de argila foi incorporado à matriz. Para a preparação dos laminados auto-adesivos, filmes nanocompósitos com propriedades mecânicas diferentes, em função da quantidade de argila incorporada à matriz, mas altamente compatíveis por possuírem a mesma matriz polimérica, foram unidos sem a utilização de adesivos ou tratamentos superficiais para aumentar a compatibilidade entre eles. Microtomografias de raios X, ensaios mecânicos e microscopia eletrônica de varredura acoplada a um feixe iônico focalizado (SEM/FIB) permitiram verificar que, sob estresse mecânico e de intumescimento, os filmes rompem no interior permanecendo a interface entre eles fortemente conectada / Abstract: This Thesis demonstrates the influence of electrostatic interactions on the physical and morphological properties of polymer clay nanocomposites prepared in aqueous medium and the characteristics of self-adhesive natural rubber/clay laminate nanocomposites. Na-montmorillonite (Na-MMT) and its ion-exchanged derivatives (K-, Li-, Ca- MMT) were used to make nanocomposites by mixing with a low-Tg styrene-acrylic latex; these materials were used to verify the effects of counterions on nanocomposite morphology and mechanical properties. The monovalent cation clays form exfoliated/intercalated nanocomposites with more than 10-fold increase in modulus, as compared to the pristine polymer, and ~ 200 % increase in tensile strength. Li-MMT nanocomposites mechanical properties are strongly dependent on the extent of drying, as expected considering that these ions are strongly hydrated. Analytical electron micrographs show that the counterions are always accumulated in the domains containing clay and polymer, both carrying excess negative charges. The electrostatic interaction model was applied to making low density polyethylene and clay nanocomposites, in aqueous medium. The nanocomposite elastic modulus increases about 40% as compared to the pure polymer, thus verifying again the model. This result was attained adding 4% of Na-MMT to the polymer matrix. The assemblage of the self-adhesive laminates was made by joining natural rubber/clay nanocomposite films with different mechanical properties without using any adhesive or surface treatment. The joined nanocomposite films showed different properties due to their different clay contents but they show high compatibility since both use the same rubber matrix. X-ray microtomography, mechanical tests and electron microscopy with a focused ion beam showed that, under mechanical and swelling stress, the laminates undergo bulk fracture while keeping the interfaces strongly connected / Doutorado / Físico-Química / Doutor em Ciências

Afin de mieux comprendre et de mieux quantifier la formation des dommages d'impact et leurs conséquences sur la tenue de la structure composite, le recours à la simulation numérique semble être un complément indispensable pour enrichir les campagnes expérimentales. Cette thèse a pour objectif la mise au point d'un modèle d'impact pour la simulation numérique par éléments finis dynamique implicite, capable de prévoir les dommages induits.La première étape du travail a consisté à élaborer un modèle s'appuyant sur le modèle de comportement du pli « Onera Progressive Failure Model » (OPFM) et sur le modèle bilinéaire de zones cohésives proposé par Alfano et Crisfield, puis d'évaluer la sensibilité aux différentes composantes des lois de comportement de la réponse à un impact et des dommages prévus. Des essais d'impact et d'indentation sur des plaques stratifiées en carbone/époxy ont ensuite été réalisés, analysés et enfin confrontés aux résultats numériques, afin d'évaluer les performances à l'impact du modèle OPFM et ses limites.Ces travaux permettent d'aboutir à trois principales conclusions. Premièrement, l'usage de modèles de zones cohésives semble nécessaire pour prévoir la chute de force caractéristique de l'impact sur stratifiés. Deuxièmement, la prise en compte des contraintes hors plan, notamment les cisaillements, est indispensable pour prévoir correctement l'endommagement d'impact. Enfin, si le modèle OPFM est capable de prévoir qualitativement les dommages d'impact, l'absence de caractère adoucissant ou de viscoplasticité semble cependant limiter leur prévision quantitative. / In order to improve the understanding and the quantification of the impact damage formation and of their consequences on the composite structure behavior, numerical simulation seems to be a necessary complement to experiments. This thesis aims at designing an impact model suited for a dynamic implicit finite element numerical simulation, able to predict the induced damages.The first step of the work consisted in building an impact model using the ply behavior law “Onera Progressive Failure Model” (OPFM) and the bilinear cohesive law defined by Alfano and Crisfield, then in evaluating the impact response and the predicted damage sensitivity to the different parameters of the behavior laws. Impact and indentation tests on carbon/epoxy laminate plates have then been performed, analyzed and compared with the numerical results, in order to evaluate the impact performance of OPFM and its limits.This work points out three key results. First, the use of cohesive zone models seems necessary to predict the typical load drop. Secondly, the out-of-plane constraints, especially the shearing, must be taken into account to correctly predict impact damages. Finally, even if the OPFM model is able to qualitatively predict impact damages, the lack of softening or viscoplasticity seems to limit their quantitative prediction.

Man-made materials such as fiber-reinforced composites (FRCs) can be tailored for optimum performance in product design applications in terms of strength and weight. The current work is aimed at studying the behaviors of composite laminates based on E-glass CSM (Chopped Strand Mat) or WRM (Woven Roving Mat) plies with a polyester resin for impact protection applications. Detailed mechanical characterization of CSM and WRM laminates till failure is carried out for tensile, compressive and shear loads by varying manufacturing process, number of plies, and laminate thickness. The effect of fiber volume fraction on mechanical properties is shown. The efficacy of CSM and WRM laminates as energy- absorbing countermeasures is studied by performing quasi-static and axial impact tests on cylindrical tubes made of the stated FRCs. In addition to load-displacement and specific energy absorption attributes, failure modes are of interest in such studies. The potential of FRC laminates for protection against projectile impact is investigated by performing low velocity impact perforation tests with a falling tup fitted with an indentor, and medium to high velocity projectile impact tests in a gas gun-based device. The valuable results generated are used for the validation of nonlinear finite element-based CAE (Computer-Aided Engineering) procedures including application of a multi-modal failure criterion for explicit dynamic analysis. The present study not only throws light on complex mechanical behavior of an important class of lightweight materials under static and dynamic loads, but also simulation tools for the design of impact safety countermeasures such as bullet-proof laminates and energy–absorbing components for automotive body structures.

L’étude réalisée dans le cadre de cette thèse représente une recherche sur la durabilité de la réparation par collage de patchs externes de structures composites endommagées. Le comportement des réparations sollicitées en traction a été étudié. Les approches expérimentale et numérique ont été réalisées. La qualité et la répétitivité des réparations dépendent fortement du savoir-faire employé durant leur mise en œuvre. A ce titre, un protocole de fabrication précis a été établi et validé. Ce protocole a ensuite été appliqué strictement dans l’ensemble de l’étude. L’effet de la géométrie des patchs sur la performance des réparations en traction a été discuté. De plus, deux séries de patchs présentant des rigidités de membranes et des séquences d’empilement différentes ont été testées. Pratiquement, plusieurs méthodes de contrôle ont été appliquées pour localiser l’initiation de l’endommagement et suivre son évolution jusqu’à la rupture final. L’observation des scénarios d’évolution de l’endommagement a conduit à proposer trois modèles phénoménologiques permettant l’élaboration et la validation d’un modèle numérique.Le modèle numérique proposé a été validé grâce à la corrélation avec les résultats expérimentaux. Ensuite, ce modèle a été appliqué pour réaliser une étude paramétrique. Les résultats obtenus ont permis de proposer un modèle d’aide à la conception et à l’optimisation des structures composites réparées. Ce modèle fournit des informations intéressantes sur la meilleure combinaison des paramètres de réparation à utiliser. / The study in this thesis represents research on the durability of the repair of damaged composite structures by bonding external patches. The behaviour of the remedies sought in tension was investigated. The experimental and numerical approaches have been made.The quality and repeatability of repairs depends heavily on skills used during their installation works. As such, a specific manufacturing protocol was established and validated. This protocol was then applied strictly throughout the study. The effect of patch geometry on the performance of repair in tension has been discussed. In addition, two sets of patches with the different membrane stiffness and stacking sequences were tested. Practically, several control methods were applied to locate damage initiation and follow its evolution until the final rupture. Observing damage evolution scenarios has led to propose three phenomenological models for the development and validation of a numerical model.The proposed numerical model has been validated through correlation with experimental results. Then, this model was applied to perform a parametric study. The results obtained allowed to propose a model to help design and optimization of repaired composite structures. This model provides interesting information on the best combination of repair settings.

No description available.

Laminados compósitos com matrizes poliméricas, respectivamente termorrígida e termoplástica, reforçadas com fibras contínuas de carbono foram submetidos a impacto único transversal com diferentes níveis de energia. Os danos imprimidos aos materiais estruturais foram avaliados por termografia ativa infravermelha na modalidade transmissão. Em geral, os termogramas do laminado termoplástico apresentaram indicações mais claras e bem definidas dos danos causados por impacto, se comparados aos do compósito termorrígido. O aquecimento convectivo das amostras por fluxo controlado de ar se mostrou mais eficaz que o realizado por irradiação, empregando-se lâmpadas incadecentes. Observou-se também que tempos mais longos de aquecimento favoreceram a visualização dos danos. O posicionamento da face impactada do espécime, relativamente à câmera infravermelha e à fonte de calor, não afetou a qualidade dos termogramas no caso do laminado termorrígido, enquanto que influenciou significativamente os termogramas do compósito termoplástico. Os resultados permitiram concluir que a termografia infravermelha é um método de ensaio não-destrutivo simples, robusto e confiável para a detecção de danos por impacto inferior à 5 Joules em laminados compósitos poliméricos reforçados com fibras de carbono. / Continuous carbon fiber-reinforced thermosetting and thermoplastic composite laminates were exposed to single transversal impact with different energy levels. The damages marked to the structural materials were evaluated by active infrared thermography in transmission mode. In general, the thermoplastic laminate thermograms showed more clear and delineated damage indications when compared to the ones from thermosetting composite. The convective heating of the samples by controlled hot air flow was more efficient than via irradiation using lamp. It was also observed that longer heating times improved the damage visualization. The positioning of the specimen´s impacted face regarding the infrared camera and the heating source did not affect the thermo-imaging of thermosetting specimens, whereas it substantially influenced the thermograms of thermoplastic laminates. The results allow concluding that infrared thermography is a simple, robust and trustworthy methodology for detecting impact damages as light as 5 Joules in carbon fiber composite laminates.

Z důvodu rozdílných koeficientů délkové teplotní roztažnosti jednotlivých vrstev vzniká ve vrstvách keramického vrstevnatého kompozitního materiálů reziduální napětí. V průběhu chladnutí vrstevnatého kompozitu ze slinovací teploty jednotlivé vrstvy smršťují různými rychlostmi v závislosti na velikosti koeficientu délkové teplotní roztažnosti. Jestliže jsou tyto vrstvy spolu pevně spojeny vzniká v jednotlivých vrstvách různě velké trvalé zbytkové napětí. Velikost residuálního napětí je dána objemovým podílem obou složek v kompozitu. Tato práce byla zaměřena na přípravu a popis 7-mi a 9-ti vrstevných keramických laminátů složených ze střídajících se vrstev dvou rozdílných materiálů. Keramické lamináty byly připraveny pomocí metody suspenzního lití a elektroforetické depozice. U připravených laminátu byl sledován vznik tzv. hranových trhlin (edge cracks) ve vrstvách obsahujících tlaková zbytková pnutí. Výsledky pozorování přítomnosti hranových trhlin pro různou konfiguraci velikosti zbytkových napětí a tloušťky vrstev byly srovnány s teoretickou předpovědí vytvořenou pomocí parametrického 2D modelu. Vliv vzniklých hranových trhlin na průběh lomu byl studován pomocí 3D rekonstrukce lomového povrchu po ohybové zkoušce připravených vrstevnatých kompozitů.

The thesis aimed to identify fracture strain for multiaxial loading for laminate material of Al and LDPE that is mostly used in the food packing technology specially in liquid packaging industry. These materials are thin and flexible which make it difficult to handle and test it. The investigation was through applying new Nakajima test setup on such a material by designing a custom setup and 3D printing the Nakajima setup prototype to be able to use it in this study. DIC technique was used to get the results from the Nakajima test and the software used to apply the DIC technique is GOM correlate. As a validation for measurement from such a technique, a tensile test has been done and measured strains were compared with those from the specimen from the Nakajima that has smallest width as it was close to a uniaxial loading. One more validation technique was by creating a FE-model using (Abaqus software) for the biaxial loading and comparing it to the biaxial loading results that obtained from the DIC analysis.

A polymer laminate consisting of multiple layers of proprietary blends of Ethylene Vinyl Alcohol (EVOH) and Thermoplastic Polyurethane (TPU) and used in the construction of air bladders was evaluated for hygroscopic effects driving delamination and multiple layer fragmentation. These air bladders are observed to suffer delamination during a manufacturing process that involves immersion in an alcohol/water solution. A plausible underlying mechanism is differential swelling and absorption by the laminate constituents. Both room and elevated temperature swelling tests were carried out to find the absorption and swelling coefficients of the constituents. These coefficients served as input into a Finite Element Analysis (FEA) model used to predict laminate failure. The diffusion coefficient for EVOH could not be obtained because the material did not reach saturation within the available timeframe of the experiment. The diffusion coefficient of the TPU was found to be 4.09E-12 [m^2/s] at room temperature and 1.26E-11 [m^2/s] at 40°C. The diffusion coefficient for TPU was an order of magnitude larger at elevated temperature and the TPU reached saturation much quicker than the EVOH, suggesting that the diffusion coefficient for the TPU was significantly greater than that of the EVOH. The swelling coefficients were 1.03E-3 m^3/kg and 9.97E-4 m^3/kg for the EVOH at room temperature and 40°C respectively, and 1.16E-3 m^3/kg and 1.09E-3 m^3/kg for the TPU at room temperature and 40°C respectively. The swelling coefficient was very close across materials and within the margin of error across temperatures. These results are required for future FEA simulations to confirm that differential swelling is the driving mechanism behind debonding and laminate failure. Tensile testing was done on laminated sheets used in production to identify cracking and layer separation at strains of 20%, 40%, and 100%. Scanning Electron Microscope (SEM) imaging was used to understand damage initiation and accumulation in the layers.

Transverse ply cracking often leads to the loss of stiffness and reduction in thermal expansion coefficients. This paper presents the thermoelastic degradation of general cross-ply laminates, containing transverse ply cracks, subjected to biaxial extension, bending and thermal loading. The stress and displacement fields are calculated by using the state space equation method [Zhang D, Ye JQ, Sheng HY. Free-edge and ply cracking effect in cross-ply laminated composites under uniform extension and thermal loading. Compos Struct [in press].]. By this approach, a laminated plate may be composed of an arbitrary number of orthotropic layers, each of which may have different material properties and thickness. The method takes into account all independent material constants and guarantees continuous fields of all interlaminar stresses across interfaces between material layers. After introducing the concept of the effective thermoelastic properties of a laminate, the degradations of axial elastic moduli, Poisson¿s ratios, thermal expansion coefficients and flexural moduli are predicted and compared with numerical results from other methods or available test results. It is found that the theory provides good predictions of the stiffness degradation in both symmetric and antisymmetric cross-ply laminates. The predictions of stiffness reduction in nonsymmetric cross-ply laminates can be used as benchmark test for other methods.