This investigation concerns the validity and feasibility of using moduli reduction to monitor the effect of fatigue damage in graphite epoxy composites. Five laminate orientations were considered, [O]₄, [90]₄, [±45]_s, [0,90]_s, [0,90,±45]_s, and four inplane-stiffness properties were monitored for each. The stiffness parameters were E_xx, E_yy, G_xy, and v_xy, and were measured using a longitudinal tension test, a rail shear test and a transverse bend test. Nondestructive testing techniques such as C-scan and edge replication were also performed to aid in the observation of damage development. Results describe the response of each laminate orientation in tension-tension fatigue, including a record of changes in the stiffness properties at intervals during fatigue. Longitudinal stiffness (E_xx) and shear stiffness (G_xy) were shown to significantly decrease for the [0,90,±45]_s, laminate following fatigue loading. The inplane stiffness properties for the other four laminates remain essentially unchanged following fatigue loading. Matrix cracking and delamination appears to contribute to the stiffness reductions that occur in the [0,90,±45]_s laminate. / Master of Science

This study consisted of two main parts, the thermoviscoelastic characterization of Kevlar 49/Fiberite 7714A epoxy composite lamina and the development of a numerical procedure to predict the viscoelastic response of any general laminate constructed from the same material. The four orthotropic material properties, S₁₁, S₁₂, S₂₂, and S₆₆, were characterized by 20 minute static creep tests on unidirectional ([0]₈, [10]₈, and [90]₁₆) lamina specimens. The Time-Temperature-Superposition-Principle (TTSP) was used successfully to accelerate the characterization process. A nonlinear constitutive model was developed to describe the stress dependent viscoelastic response for each of the material properties. A new numerical procedure to predict long term laminate properties from lamina properties (obtained experimentally) was developed. Numerical instabilities and time constraints associated with viscoelastic numerical techniques were discussed and solved. The numerical procedure was incorporated into a user friendly microcomputer program called Viscoelastic Composite Analysis Program (VCAP), which is available for IBM ‘PC’ type computers. The program was designed for ease of use and includes graphics, menus, help messages, etc. The final phase of the study involved testing actual laminates constructed from the characterized material, Kevlar/epoxy, at various temperature and load levels for 4 to 5 weeks. These results were then compared with the VCAP program predictions to verify the testing procedure (i.e., the applicability of TTSP in characterizing composite materials) and to check the numerical procedure used in the program. The actual tests and predictions agreed, within experimental error and scatter, for all test cases which included 1, 2, 3, and 4 fiber direction laminates. The end result of the study was the development and validation of a user friendly microcomputer program that can be used by design engineers in industry to predict thermoviscoelastic properties of orthotropic composite materials. / Ph. D.

The viscoelastic response of polymer-based composite laminates, which may take years to develop in service, must be anticipated and accommodated at the design stage. Accelerated testing is therefore required to allow long-term compliance predictions for composite laminates of arbitrary layup, based solely upon short-term tests. In this study, an accelerated viscoelastic characterization scheme is applied to T300/5208 graphiteepoxy laminates. The viscoelastic response of unidirectional specimens is modeled using the theory developed by Schapery. The transient component of the viscoelastic creep compliance is assumed to follow a power law approximation. A recursive relationship is developed, based upon the Schapery single-integral equation, which allows approximation of a continuous time-varying uniaxial load using discrete steps in stress. The viscoelastic response of T300/5208 graphite-epoxy at 149C to transverse normal and shear stresses is determined using 90-deg and 10-deg off-axis tensile specimens, respectively. parameters In each case the seven viscoelastic material required in the analysis are determined experimentally, using a short-term creep/creep recovery testing cycle. A sensitivity analysis is used to select the appropriate short-term test cycle. It is shown that an accurate measure of the power law exponent is crucial for accurate long-term predictions, and that the calculated value of the power law exponent is very sensitive to slight experimental error in recovery data. Based upon this analysis, a 480/120 minute creep/creep recovery test cycle is selected, and the power law exponent is calculated using creep data. A short-term test cycle selection procedure is proposed, which should provide useful guidelines when other viscoelastic materials are being evaluated. Results from the short-term tests on unidirectional specimens are combined using classical lamination theory to provide long-term predictions for symmetric composite laminates. Experimental measurement of the long-term creep compliance at 149C of two distinct T300/5208 laminates is obtained. A reasonable comparison between theory and experiment is observed at time up to 10 5 minutes. Discrepancies which do exist are believed to be due to an insufficient modeling of biaxial stress interactions, to the accumulation of damage in the form of matrix cracks or voids, and/or to interlaminar shear deformations which may occur due to viscoelastic effects or damage accumulation. / Doctor of Philosophy

An epoxy resin (Epon 828) was chemically modified with two different elastomers, poly(dimethyl-co-diphenyl) siloxane (PSX) and carboxyl-terminated butadiene-acrylonitrile (CTBN), to enhance its fracture toughness. The friction and wear of specimens modified with different amounts of elastomer were investigated in a pin-on-disk wear machine. An attempt was made to correlate the fracture toughness of the epoxy material to its fatigue wear rate for experiments in which a steel ball was sliding on a modified epoxy disk. A different type of experiment, modified epoxy pin sliding on an abrasive disk, was performed to detect whether abrasive wear of modified epoxies responds differently than fatigue wear to the fracture toughness. Other experiments were performed in which the wear debris produced during sliding was blown out of the interface to study its influence on friction and wear behavior. The effect of surface morphology on friction and wear was also studied. The results indicated that a marked improvement in fracture toughness was achieved for samples with higher elastomer content. Regardless of the type of the experiment, epoxy pin-on-abrasive disk or steel ball-on-epoxy disk, wear rates correlated positively with inverse of fracture toughness. Both friction coefficient and wear rate were found to be influenced by the removal of the wear debris, especially for samples with higher elastomer content. The friction coefficient was reduced for samples with higher elastomer content and this was attributed to the low surface energy of the elastomer. CTBN-modified epoxies exhibited lower friction coefficients than epoxies modified with polysiloxane. It was found that sample morphology had a significant effect on both friction coefficient and wear rate; the sample with approximately the same domain size but the least number of elastomeric domains exhibited the highest friction coefficient and the highest wear rate. / Ph. D.

Metal implants are a type of hard tissue replacement currently used. Metals used for implants include: stainless steel, titanium, chrome, and cobalt alloys. Such implants often fail at the interface with bone. Metal implants fail when the surface of the implant is coated with an osteoconductive material. An osteoconductive material provides scaffolding for cellular migration, cellular attachment, and cellular distribution. A reason for metal implant failure could be the vastly different material properties than bone. Motivation for the research was to find a suitable bone substitute other than metal. Materials considered were: zirconia toughened alumina, carbon fiber reinforced epoxy, and glass fiber reinforced epoxy. Those materials have been used in previous biological applications and can be cast into complex configurations. Objectives of the study were to compare material properties of the composites to bone. A method to create porosity was then tested in the material that was similar to bone in critical material property. Some of the materials were statistically similar to bone in yield strength. Method to create interconnected porosity in those materials resulted in 49% void space.

Les développements récents en électronique de puissance visent à augmenter la densité de puissance totale dans les systèmes de conversion d'énergie. Cela contraint alors de plus en plus les matériaux isolants, tels que l'encapsulation dans les modules de puissance. Si les renforcements de champ électrique au sein des polymères isolants atteignent des valeurs critiques, cela peut entraîner une activité de décharges partielles, des arborescences voire la rupture totale de l'isolation. L'objectif de cette thèse est d'étudier l'adaptation des propriétés diélectriques d'un polymère composite isolant afin de réduire les contraintes autour des zones de renforcements de champ électrique. Nous proposons une nouvelle approche de gradation de potentiel pour minimiser les renforcements de champ à travers une structuration locale du matériau composite sous forme d'un gradient de permittivité auto-adaptatif localisé là où les contraintes sont les plus intenses. Cette structuration est réalisée via l'application d'un champ électrique DC lors du procédé d'élaboration du matériau composite, permettant le déplacement par électrophorèse des particules. Le composite à gradient de permittivité est composé d'une matrice époxy chargée en particules à forte permittivité (titanate de strontium SrTiO3 ou titanate de baryum BaTiO3). L'action d'un champ électrique DC sur la résine liquide chargée en particules engendre leur accumulation vers l'électrode de plus fort potentiel, formant ainsi une couche fortement chargée, qui confère à cette région une permittivité plus élevée. Chaque région du composite structuré (zone de la couche accumulée et zone faiblement chargée en particules) a été caractérisée en termes de propriétés diélectriques (permittivité et pertes). Alors que la région des composites faiblement chargée en particules conserve une permittivité voisine de celle des composites homogènes, la couche accumulée présente une augmentation importante liée à l'augmentation de la densité de particules. Les concentrations en particules de chaque région du matériau structuré ont été déterminées précisément, et les valeurs de permittivités associées se corrèlent bien avec les valeurs de permittivité des matériaux composites homogènes de taux de chargement équivalent. Cela montre que la couche accumulée ne s'est pas organisée d'une façon particulière. Concernant la rigidité diélectrique de la couche accumulée, elle présente des valeurs suffisantes pour tenir les contraintes rencontrées et ses valeurs suivent la loi de puissance classique en fonction de l'épaisseur. Des simulations par éléments finis confirment l'intérêt de ces matériaux pour la minimisation des renforcements de champ électrique au niveau du point triple dans les modules de puissance. Ces résultats montrent tout le potentiel applicatif de ces nouveaux matériaux à gradient de champ. Ils pourraient permettre l'amélioration de la fiabilité et de la robustesse des modules de puissance et autres systèmes électriques travaillant sous fort champ. / New developments in power electronics allow increasing the power density of the conversion systems. This means that the insulating materials, such as the encapsulation in power modules, are more are more stressed. If the electric field reinforcements in insulating polymers reach critical values, this can lead to a partial discharge activity, electrical treeing and eventually a complete breakdown of the insulation. The objective of this thesis is to study the appropriate matching of the dielectric properties of insulating polymer composites in order to reduce the electrical stress in the regions of field reinforcement. A new approach to minimize the reinforcements is proposed through a local structuration of the composite material allowing an auto-adaptive permittivity gradient where the largest stresses are present. This structuration is achieved thanks to the application of a DC electric field during the elaboration process of the composite material, leading to the displacement of the particles by electrophoresis. The field grading material is an epoxy matrix filled with high permittivity particles (strontium titanate SrTiO3 or barium titanate BaTiO3). Applying a DC electric field on the liquid resin containing the particles induces their accumulation on the high voltage electrode, building an accumulated layer highly concentrated in particles, conferring to this region a higher permittivity. Each region of the structured composite (accumulated layer and low concentrated region) was characterized in terms of dielectric properties (permittivity and losses). While the low concentrated region of particles keeps a permittivity close to that of homogeneous composites one, the accumulated layer exhibits a significant increase due to the increase in the local particle content. The particle concentration in each region of the structured material were precisely determined, and the related permittivity values are in good agreement with the permittivity values of the homogeneous composite materials of the same filler content. This shows that the accumulated layer was not organized in a particular way. Regarding the dielectric strength of the accumulated layer, its values are large enough for the applications and these values follow the typical power law versus thickness. Finite element methods prove that these materials are appropriate for minimizing the electric field reinforcements at the triple point, between the metal, the ceramic and the encapsulation. These results highlight the interests of these new kind of field grading materials. They could allow improving the reliability and the robustness of power modules or other electrical systems working at high field.

Submitted by Ronildo Prado (ronisp@ufscar.br) on 2017-03-02T12:48:47Z No. of bitstreams: 1 DissEHB.pdf: 15859692 bytes, checksum: c4538902f4ec95de542bf12edadd5749 (MD5) / Approved for entry into archive by Ronildo Prado (ronisp@ufscar.br) on 2017-03-02T12:49:08Z (GMT) No. of bitstreams: 1 DissEHB.pdf: 15859692 bytes, checksum: c4538902f4ec95de542bf12edadd5749 (MD5) / Approved for entry into archive by Ronildo Prado (ronisp@ufscar.br) on 2017-03-02T12:49:29Z (GMT) No. of bitstreams: 1 DissEHB.pdf: 15859692 bytes, checksum: c4538902f4ec95de542bf12edadd5749 (MD5) / Made available in DSpace on 2017-03-02T12:49:51Z (GMT). No. of bitstreams: 1 DissEHB.pdf: 15859692 bytes, checksum: c4538902f4ec95de542bf12edadd5749 (MD5) Previous issue date: 2016-07-11 / Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / In the present work epoxy/ MWCNT/ mineral fillers nanocomposites were obtained using ultrasonication and calendering. The effect of addition of mineral filler (calcium carbonate, montmorillonite and sepiolite) in electrical, mechanical and thermal properties of epoxy/ MWCNT were analyzed. Two different CNT were studied, with different aspect ration and purity, however only Nanocyl CNT’s presented improvement in the nanocomposites electrical properties and for that reason was employed for hybrid epoxy/ MWCNT/ mineral nanocomposites production. The electrical percolation threshold was determined as 0.04 wt% and for 0.3 wt% the electrical conductivity reached 1.29X10-2 S/m. The addition of calcium carbonate and montmorillonite improved electrical conductivity for epoxy nanocomposites produced with 0.05 wt% CNT and the same behavior was observed for epoxy/ MWCNT / sepiolite nanocomposites at 0.1 wt% CNT. The epoxy/ MWCNT nanocomposite at 0.05% CNT when produzed via calendering presented improvement in the electrical conductivity compared to the same nanocomposite produced via ultrasonication. For epoxy/ MWCNT at 0.05 wt% of CNT, the addition of calcium carbonate in the nanocomposite led to an electrical conductivity 1 decade higher than the epoxy/ 0.05 wt% CNT nanocomposite produced via calendering. The mineral fillers also modified thermal and mechanical behavior of the nanocomposites, and improvements in flexural modulus, thermal stability and Tg were observed. / Neste trabalho produziu-se nanocompósitos híbridos de resina epóxi/ NTCPM/ cargas minerais utilizando-se sonicação de alta energia e calandragem, e estudou-se a influência da adição de diferentes cargas minerais (carbonato de cálcio, montmorilonita e sepiolita) nas propriedades elétricas, térmicas e mecânicas de nanocompósitos epóxi/NTCPM. Neste trabalho foram utilizados dois diferentes tipos de nanotubos de carbono, com razões de aspecto e purezas diferentes, e verificou-se que somente um deles apresentou melhoria nas propriedades elétricas dos nanocompósitos epóxi/NTCPM, o qual foi empregado na produção de nanocompósitos híbridos epóxi/ NTCPM/ cargas minerais. A percolação elétrica dos nanotubos de carbono foi determinada em aproximadamente 0,04% em massa, e para um teor de 0,3% em massa de nanotubos de carbono, a condutividade elétrica atingiu 1,29X10-2 S/m. Nos nanocompósitos processados via sonicação de alta energia, observou-se elevação da condutividade elétrica com a adição de montmorilonita sódica e carbonato de cálcio para os teores de 0,05% em massa de NTCPM e com a adição de sepiolita somente para o teor de 0,1% em massa de NTCPM. Nos nanocompósitos processados via calandragem, o nanocompósito de resina epóxi/ 0,05% NTCPM apresentou condutividade elétrica duas vezes superior ao mesmo nanocompósito processado via sonicação de alta energia e a adição de carbonato de cálcio elevou a condutividade elétrica do nanocompósito de resina epóxi/ 0,05% NTCPM/ carbonato de cálcio em uma ordem de grandeza quando comparado ao nanocompósito epóxi/ 0,05% NTCPM processado via calandragem. A adição de NTCPM e cargas minerais também modificou os comportamentos mecânico e térmico dos nanocompósitos, elevando-se o módulo elástico em flexão, resistência térmica e Tg. / FAPESP: 2014/16299-8

La cuisson rapide de préimprégnés est une problématique d'actualité qui sous entend les nécessités de rentabilité dans l'industrie aéronautique. Cette étape est basée sur la maîtrise du degré d'avancement de réaction du système thermodurcissable au cours du cycle qui régit l'ensemble des propriétés finales des pièces composites. La caractérisation et la modélisation cinétique du préimprégné aéronautique M21/T700 sont réalisées en vue d'appliquer des dynamiques de mise en oeuvre rapides applicables sur une installation de thermocompression dotée d'un moule chaué par induction de technologie Cage System de Roctool. La construction de diagrammes Temps Température Transformation et la réalisation d'un couplage thermo-cinétique par éléments finis permettent de proposer des cycles optimisés d'une durée de moins de 2 heures (au lieu de 4h30 en cuisson autoclave), en préservant la présence de particules de thermoplastiques dans la matrice. L'étude des propriétés des plaques fabriquées montre des résultats comparables à ceux obtenus pour des pièces mises en oeuvre lors de cycles standards de fabrication à l'aide du procédé autoclave. / The increase of composite content in aerospace structures requires an improvement of profitability through high curing processes. The curing step is based on the control of the degree of cure of the thermosetting system that governs the final properties of the composite parts. The Cage System technology from the Roctool company enables high curing rates thanks to induction heating system. Thus, the characterization and the kinetic modeling of the M21/T700 aeronautical prepreg have been realized for such sollicitations (i.e. high heating rates). To provide a better temperature control, the thermal and kinetic interactions are also considered by finite element modeling of composite thickness. Time Temperature Tranformation diagrams have been set up to build short curing cycle of less than 2h (instead of 4h30 in autoclave curing), considering the presence of thermoplastic particules. Finally, the part properties are in good agreement with the autoclave cycle recommended by the material supplier.

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