This master’s thesis deals with the composite materials and especially aims on the carbon and glass fiber composites. It points out different composition types and manufacturing methods which reflect in the different mechanical properties, final quality of the manufactured part and also in the manufacturing time. The practical part includes two particular manufacturing methods using prepregs, one cured in an autoclave and one by hot compression moulding.

The doctoral thesis is aimed at preparation of glass fiber reinforced polymer composites with controlled interphase formed by plasma-polymerized tetravinylsilane and tetravinylsilane/oxygen thin films. The thin polymer films of specific physico-chemical properties and thickness were deposited to improve interfacial adhesion of glass fiber/polyester composites. The fiber surface modification was performed by using plasma enhanced chemical vapor deposition in low-temperature RF plasma operating in an various effective power range and different treatment time. Test results were examined in relation to the interlayer thickness and different treatment conditions. The prepared interlayers were analyzed to evaluate physico-chemical composition and properties (XPS, RBS, ERDA, FTIR and spectroscopic elipsometry). Selected mechanical properties were evaluated by AFM. Mechanical response of plasma interlayers was evaluated by short beam shear test and direct method of testing the interfacial shear strength using microindentation. The interphase shear failure was controlled by the shear strength at the interlayer/fiber interface as follows from experimental and model data.

Orientador: Michelli Leali Costa / Resumo: Dentre os setores de aplicações comerciais de materiais compósitos avançados, destaca-se o setor aeroespacial com larga aplicação desses materiais. Entre as técnicas de união aplicadas aos compósitos termoplásticos está a soldagem com grandes vantagens em relação aos outros processos de uniões tais como, redução de custo, agilidade de processamento, redução de elementos acumuladores de tensão, preparações mais simplórias das superfícies a serem soldadas. Mesmo com essas vantagens e, embora o processo já seja utilizado nos setores industriais, a soldagem de compósitos tem como desafio a melhoria de sua resistência, a aplicação do processo para reparos ou processamentos em campo, além da necessidade de avaliação dos efeitos das condições climáticas em juntas soldadas, as quais podem estar submetidas quando em operação em uma aeronave, por exemplo. Mediante a isso, esse trabalho visa produzir e estudar juntas soldadas por resistência elétrica e por tocha acetilênica em compósito PEI/fibra de vidro. Os compósitos obtidos foram submetidos ao condicionamento higrotérmico seguido de ensaios mecânicos de LSS (Lap Shear Strength) e ENF (End-Notched Flexure). O mecanismo de fratura das juntas soldadas foi avaliado por microscopia. A partir das análises e dos resultados obtidos, foi observado que os valores de resistência ao cisalhamento em modo II dos compósitos soldados por resistência elétrica (3270,9 J/m²) são similares aos descritos na literatura para os compósitos PEI/fibra de vid... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: Among the commercial application sectors of advanced composite materials, the aerospace sector with wide application of these materials stands out. Among the joining techniques applied to thermoplastic composites is welding with great advantages over other joining processes such as cost reduction, processing agility, reduction of stress accumulators, little or no preparation required of the surface to be processed. Even with these advantages, and although the process is already used in the industrial sectors, composite welding has the challenge of improving its resistance, the application of the process for field repairs or processing, and the need to evaluate the effects of weather conditions. welded joints, which may be subjected when operating in an aircraft, for example. Therefore, this work aims to produce and study joints welded by electric resistance and acetylene torch in PEI / fiberglass composite. The composites obtained were subjected to hygrothermal conditioning followed by mechanical tests of LSS (Lap Shear Strength) and ENF (End-Notched Flexure). The fracture mechanism of the welded joints was evaluated by microscopy. From the analyzes and results obtained, it was observed that the shear strength values in mode II of the composites welded by electric resistance (3270.9 J / m²) are similar to those described in the literature for PEI / fiberglass composites. However, for the composites welded by the oxyacetylene process, a reduction of approximately 20% in the va... (Complete abstract click electronic access below) / Mestre

[ES] En el ámbito de los materiales compuestos o composites para la construcción, el cemento reforzado con fibras de vidrio (GRC, del inglés glass fiber reinforced cement) es el más extensamente utilizado, por sus excelentes propiedades mecánicas (resistencia a flexión y tenacidad). Sin embargo, la durabilidad de estos composites se ha demostrado crítica, y es necesario proponer alternativas. Las fibras usadas, de carácter álcali-resistente (fibras AR, formadas por agrupación de filamentos), son atacadas por el medio agresivo que impone el cemento hidratado. Una alternativa interesante, desde el punto de vista tecnológico, es la incorporación de materiales cementantes suplementarios de carácter puzolánico. El objetivo del presente trabajo es estudiar la influencia de las diferentes adiciones activas en morteros de GRC, observando el comportamiento de los elementos constitutivos del material en condiciones normales de curado, y también al ser sometidos a procesos de envejecimiento controlado. Asimismo, se analiza el comportamiento de los nuevos composites sometidos a diferentes medios agresivos, evaluando la durabilidad y la mejora de los compuestos por medio de la determinación de sus propiedades mecánicas, químicas y físicas. Se han elaborado probetas de GRC a través del procedimiento de premezcla (premix) y se han determinado sus propiedades mecánicas (resistencia a flexión, tenacidad y módulo de elasticidad). Adicionalmente, se han cuantificado las ganancias de resistencia al comparar composites GRC basados en cemento Portland (especímenes control) con otros en los que se ha sustituido hasta el 60% de dicho cemento por adiciones puzolánicas. Al objeto de mejorar la reactividad de las puzolanas, en algunos casos se ha implementado un aumento de su finura a través de la molienda (cenizas volantes molidas, CVm) o de procesos de sonicación (humo de sílice sonicado, HSS). Los especímenes de GRC han sido sometidos a un proceso de envejecimiento (tratamiento en agua a 55ºC durante un período prolongado) y se ha observado un empeoramiento muy importante de la resistencia a flexión y la tenacidad de aquellos que poseen solamente cemento Pórtland como componente cementante. Los composites GRC que contienen cantidades elevadas de puzolana (60% de CVm) o mezclas de puzolanas (50%CVm / 10%HSS, 50%CVm / 10%FCC) presentan una mejora sustancial de las propiedades mecánicas con respecto a los GRC control. La mejora de estos sistemas GRC con elevados porcentajes de puzolanas reactivas se han confirmado a través de estudios físicos y físico - químicos: evaluación de densidad, absorción, estudios microscópicos (lupa y microscopía electrónica de barrido) y análisis termogravimétrico. En cuanto a la respuesta de los composites GRC frente a diferentes disoluciones agresivas, se ha demostrado el efecto beneficioso de la presencia de puzolanas. Después de la exposición de los morteros de GRC a una disolución de NH4Cl, el comportamiento mecánico de los morteros puzolánicos se mantiene por encima del mortero GRC control: esto se debe a la relación directa existente con el incremento de la densidad y la disminución de grado de absorción del composite con la sustitución puzolánica. Al evaluar las propiedades de los morteros de GRC después de su exposición a una disolución de H2SO4, se observan diferencias muy importantes en la evolución de la masa, resistencia a flexión y tenacidad: los composites control son más afectados por la acidez del medio, de modo que la pérdida de masa es muy significativa si se compara con los GRC que presentan puzolanas. La estancia en la empresa Saint Gobain Vetrotex, ha permitido confirmar una gran similitud en los resultados obtenidos mediante los procedimientos seguidos en el laboratorio de la UPV (compuestos de GRC premezclado) comparados con las prácticas desarrolladas por el laboratorio de materiales de la empresa (composites de GRC proyectado). Se han evaluado / [CAT] En l'àmbit dels materials compostos o compòsits per a la construcció, el ciment reforçat amb fibres de vidre (GRC, de l'anglès glass fiber reinforced cement) és el més extensament utilitzat, per les seves excel·lents propietats mecàniques (resistència a flexió i tenacitat). No obstant això, la durabilitat d'aquests compòsits s'ha demostrat crítica, i cal proposar alternatives. Les fibres usades, de caràcter àlcali-resistent (fibres AR, formades per agrupació de filaments), són atacades pel medi agressiu que imposa el ciment hidratat. Una alternativa interessant des del punt de vista tecnològic és la incorporació de materials cimentants suplementaris de caràcter putzolànic. L'objectiu d'aquest treball és estudiar la influència de les diferents addicions actives en morters de GRC, observant el comportament dels elements constitutius del material en condicions normals de curat, i també quan son sotmesos a processos d'envelliment controlat. Així mateix, s'analitza el comportament dels nous compòsits sotmesos a diferents mitjans agressius, avaluant la durabilitat i la millora dels compostos mitjançant la determinació de les seves propietats mecàniques, químiques i físiques. S'han elaborat provetes de GRC a través del procediment de mescla prèvia (premix) i s'ha determinat les seves propietats mecàniques (resistència a flexió, tenacitat, mòdul d'elasticitat). Addicionalment s'han quantificat els guanys de resistència al comparar compòsits GRC basats en ciment Portland (espècimens control) amb altres en què s'ha substituït fins al 60% d'aquest ciment per materials putzolànics. A l'objecte de millorar la reactivitat de les putzolanes, en alguns casos s'ha implementat un augment de la seva finor a través de la mòlta (cendres volants mòltes, CVm) o de processos de sonicació (fum de sílice sonicat, HSS). Els espècimens de GRC han estat sotmesos a un procés d'envelliment (tractament en aigua a 55ºC durant un període prolongat) i s'ha observat l'empitjorament molt significatiu de la resistència a flexió i la tenacitat d'aquells que posseeixen solament ciment Pòrtland com a component cimentant. Els compòsits GRC que contenen quantitats elevades de putzolana (60% de CVm) o mescles de putzolanes (50% CVm / 10% HSS, 50% CVm / 10% FCC) presenten una millora substancial de les propietats mecàniques respecte als GRC control. La millora d'aquests sistemes GRC amb elevats percentatges de putzolanes reactives s'han confirmat a través d'estudis físics i fisicoquímics: avaluació de densitat, absorció, estudis microscòpics (lupa i microscòpia electrònica de rastreig) i anàlisi termogravimètric. Pel que fa a la resposta dels compòsits GRC enfront de diferents dissolucions agressives, s'ha demostrat l'efecte beneficiós de la presència de putzolanes. Després de l'exposició dels morters de GRC a una dissolució de NH4Cl, el comportament mecànic dels morters putzolànics es millor que el morter GRC control: això es deu a la relació directa existent amb l'increment de la densitat i la disminució del grau d'absorció del compòsit amb la putzolana. Quan s¿ha avaluat les propietats dels morters de GRC després de la seva exposició a una dissolució H2SO4, s'observen diferències molt importants en l'evolució de la massa, resistència a flexió i tenacitat: els compòsits control són més afectats per l'acidesa del medi, de manera que la pèrdua de massa és molt significativa si es compara amb els GRC que presenten putzolanes. L'estada a l'empresa Saint Gobain Vetrotex, ha permès confirmar una gran similitud en els resultats obtinguts mitjançant els procediments seguits en el laboratori de la UPV (compostos de GRC amb premescla) comparats amb les pràctiques desenvolupades pel laboratori de materials de l'empresa (compostos de GRC projectat). S'han avaluat prototips per a la indústria de l'GRC projectat. / [EN] In the field of composite materials for construction, glass fiber reinforced cement (GRC) is the most widely used, due to its excellent mechanical properties (resistance to bending and toughness). However, the durability of these composites has been demonstrated to be critical and alternatives need to be proposed. The used fibers, alkali-resistant (AR fibers, formed by grouping of filaments), are attacked by the aggressive medium imposed by the hydrated cement. An interesting alternative, from a technological point of view, is the incorporation of supplementary cementitious materials of pozzolanic behaviour. The purpose of this research is to study the influence of the different mineral additions in GRC mortars, observing the behaviour of the constituent elements of the material under normal curing conditions and controlled aging processes. Likewise, the behaviour of new composites subjected to different aggressive environments is analyzed, evaluating the durability and improvement of the compounds by determining their mechanical, chemical and physical properties. GRC specimens have been produced through the premix procedure and their mechanical properties (flexural strength, toughness, and modulus of elasticity) have been determined. Additionally, resistance gains have been quantified when comparing GRC composites based on Portland cement (control specimens) with others in which up to 60% of that cement has been replaced by pozzolanic additions. In order to improve the reactivity of pozzolans, in some cases an increase in its fineness has been implemented through grinding (ground fly ash, CVm) or sonication processes (sonicated silica fume, HSS). The GRC specimens have been subjected to an aging process (treatment in water at 55ºC for an extended period) and worsening of the flexural strength and toughness of those who only have Portland cement as cementitious component has been observed. GRC composites containing high amounts of pozzolan (60% CVm) or mixtures of pozzolans (50% CVm / 10% HSS, 50% CVm / 10% FCC) show a substantial improvement in mechanical properties compared to the control GRC. The improvement of these GRC systems with high percentages of reactive pozzolans have been confirmed through physical and physical-chemical studies: evaluation of density, absorption, microscopic studies (magnifying glass and scanning electron microscopy), and thermogravimetric analysis. Regarding the response of GRC composites against different aggressive solutions, the beneficial effect of the presence of pozzolans has been demonstrated. After the exposure of the GRC mortars to a NH4Cl solution, the mechanical behavior of pozzolanic mortars remains above that of the control GRC mortar: this is due to the direct relationship existing with the increase in density and the decrease in the absorption of the composite with the pozzolanic replacement. When evaluating the properties of GRC mortars after exposure to an H2SO4 solution, very important differences are observed in the evolution of the mass, flexural strength and toughness: the control composites are more affected by the acidity of the medium, so that the loss of mass is very significant when compared to the GRCs that present pozzolans. The stay at the Saint Gobain Vetrotex company has confirmed a great similarity to the results obtained by the procedures followed at the UPV laboratory (premixed GRC compounds) compared to the practices developed by the company's materials laboratory (composites of projected GRC). Scalable prototypes have been assessed for the projected GRC industry. / Lalinde Castrillón, LF. (2020). Estudio de compuestos de GRC y adiciones activas: Propiedades mecánicas, envejecimiento acelerado y durabilidad [Tesis doctoral]. Universitat Politècnica de València. https://doi.org/10.4995/Thesis/10251/157637 / TESIS

Hybride Oberflächenaktivierungen von Glasfaserrovings mittels Polymer/Zement-Kompositen ermöglichen eine komplette Durchdringung des Rovings mit Beton von der Matrix bis zu den innenliegenden Einzelfilamenten. Dies erlaubt einen deutlich verbesserten Lasteintrag in den gesamten Rovingquerschnitt bei der Verwendung als Faserverstärkung in textilbewehrten Betonen. Auf Grund von ausgeprägten Domänen hydratisierter Zementsteinphasen innerhalb des Rovings ergibt sich eine komplexe, multiskalige Verbundstruktur, die sich in ihren Eigenschaften deutlich von klassischen polymerbeschichteten Rovings unterscheidet. Wir diskutieren diesen Ansatz in Bezug auf Herstellung, nano-/mikroskopische Charakterisierung, sowie der mechanischen Eigenschaften der Probenkörper unter beschleunigten Alterungsbedingungen. Die mikroskopischen Untersuchungen mittels höchstauflösender Elektronenmikroskopie und Nanoindentation zielen darauf ab, die Grenzflächenanbindung, die veränderte Struktur in Abhängigkeit des verwendeten Polymers und der Additive sowie die Korrosionsmechanismen aufzuklären. / Hybrid surface modifications of glass fiber rovings with polymer/cement-composites allow the generation of extended cement phases within the roving and an activation of the innermost filaments to the surrounding concrete matrix. This enables enhanced load transfer across the full roving cross section when used as fibrous reinforcement in textile-reinforced concrete. Due to the presence of extended concrete domains within the roving, a complex multiscale composite structure develops, displaying distinctly different properties as compared to standard polymer impregnation routes. We discuss this approach in terms of production, nano/microscopic characterization of the concrete composites and mechanical properties of the resulting specimens under accelerated aging conditions. The microscopy studies using highest resolution electron microscopy and nanoindentation aim to elucidate the interface connection, the changes in morphology of the concrete as a function of the polymer and additives used, as well as shedding light on the corrosion mechanisms.

Im Rahmen des Transferprojektes T01 „Textilbeschichtung mit hochviskosen Massen“ des Sonderforschungsbereiches 532 (SFB 532) wird die Realisierung und Bewertung eines integrierten Beschichtungskonzeptes zur nachhaltigen Verbesserung der Tragfähigkeit von textilbewehrten Betonbauteilen an der RWTH Aachen University untersucht. Dazu wird eine neue Auftragstechnik für hochviskose Beschichtungsmassen entwickelt, die eine vollständige Penetration von Multifilamentgarnen mit großen Garntitern und einer hohen Anzahl an Filamenten in textilen Gelegen erzielt. Des Weiteren werden aktive Beschichtungsmassen auf der Basis von Polyvinylalkohol-Zement-Compositen, die eine homogene Anbindung aller Einzelfilamente an die Zementmatrix ermöglichen, erforscht.

The increased use of thermoplastics in load carrying components, especially in the automotive industry, drives the needs for a better understanding of its complex mechanical properties. In this thesis work for a master degree in solid mechanics, the mechanical properties of a PA 6/66 resin with and without reinforcement of glass fibers experimentally been investigated. Topics of interest have been the dependency of fiber orientation, residual strains at unloading and compression relative tension properties. The experimental investigation was followed by simulations implementing existing and available constitutive models in the commercial finite element code LS-DYNA. The experimental findings showed that the orientation of the fibers significantly affects the mechanical properties. The ultimate tensile strength differed approximately 50% between along and cross flow direction and the cross-flow properties are closer to the ones of the unfilled resin, i.e. the matrix material. An elastic-plastic model with Hill’s yield criterion was used to capture the anisotropy in a simulation of the tensile test. Residual strains were measured during strain recovery from different load levels and the experimental findings were implemented in an elastic-plastic damage model to predict the permanent strains after unloading. Compression tests showed that a stiffer response is obtained for strains above 3% in comparison to tension. The increased stiffness in compression is although too small to significantly influence a simulation of a 3 point bend test using a material model dependent of the hydrostatic stress.

<p>Composite materials have become widely used for high-performance applications, particularly in the aerospace industry where annual production volumes are low and a higher part cost can be supported. During the last decades composite materials are beginning to see use in a broader range of applications, including the automotive and sports equipment industries. Simultaneously, there is increasing demand from consumers and regulatory bodies to make cars more fuel efficient and in the case of EV’s longer drive range, which can be accomplished by reducing vehicle weight. Composite materials have high specific stiffnesses and strengths, resulting in weight savings when they are used to replace traditionally metal components. However, in order for widespread adoption of composite parts to be viable for the automotive industry, high-rate manufacturing must be realized to reach the required production volumes and part costs.</p> <p>Toward this goal, advanced composite manufacturing techniques have been developed. These techniques typically combine high automation with careful material selection, which can include fast-curing resins and thermoplastics with adapted melt viscosities and thermomechanical properties. They also allow for complex part geometries to be produced in a single step, reducing the need for additional assembly time. Further, they can be used to easily create multi-material components, which can result in parts that benefit from the desirable mechanical properties of the constituent materials without sacrificing performance.</p> <p>This thesis develops a framework for the design and high-rate manufacture of multi-material components. First, a critical literature review is conducted to develop a clear understanding of existing research into combinations of dissimilar materials, including epoxy/polyamide, thermoplastic elastomer/polyamide, and aluminum/thermoplastic. It is shown that, for all material combinations studied, interfacial delamination and subsequent deformation are the primary energy absorption mechanisms and that manufacturing conditions may affect interfacial bond strength. Based on this foundation, adhesion testing is performed on devoted sample configurations fabricated under controlled molding conditions. For these material combinations, interfacial adhesion can be significantly improved with carefully selected processing temperatures, even to the extent that adhesive bond between dissimilar materials can be stronger than the cohesive bond in the constituent materials. Next, impact and quasi-static indentation testing were performed to determine the effects of interfacial adhesion and part design on crash performance. The materials tested all benefit from the placement of a more ductile material on the impacted side of the sample (top surface), indicating a more favorable dissipation of the contact stresses from the impactor, and a higher strength material on the bottom surface where it can withstand tensile stresses imposed by impact-induced bending. </p> <p> Finally, a complex part consisting of a unidirectional polyamide/carbon fiber preform and a thermoplastic overmold is manufactured via a hybrid overmolding process. Interfacial temperature during overmolding is varied to confirm if the same improvements in interfacial bond strength seen in the compression molding test samples are attainable under realistic high-rate manufacture conditions. Additionally, the preform volume is varied to examine the effect of the preform reinforcement on a part’s bending performance. For this system, varying the preform temperature had no effect on interfacial bond strength. A predictive technical cost model is also used to determine the effect of manufacturing changes on part costs. Increasing the tow volume three-fold increased the absorbed energy by more than 30% and requires an increased cost of only 3.8%. </p> <p>This thesis proves that a tough, multi-material part can be rapidly produced via hybrid overmolding. It was demonstrated that a complex shaped part could be produced at a complete line cycle time of approximately 90 secondsmaking it a viable method to produce high-performance, low-cost components. </p>

<div>Self-sensing materials are engineered to transduce mechanical effects like deformations and damages into detectable electrical changes. As such, they have received immense research attention in areas including aerospace, civil infrastructure, robotic skin, and biomedical devices. In structural health monitoring (SHM) and nondestructive evaluation (NDE) applications, damages in the material cause breakage in the conductive filler networks, resulting in changes in the material's conductivity. Most SHM and NDE applications of self-sensing materials have used direct current (DC) measurements. DC-based methods have shown advantages with regard to sensitivity to microscale damages compared to other SHM methods. Comparatively, alternating current (AC) measurement techniques have shown potential for improvement over existent DC methods. For example, using AC in conjunction with self-sensing materials has potential for benefits such as greater data density, higher sensitivity through electrodynamics effects (e.g., coupling the material with resonant circuitry), and lower power requirements. Despite these potential advantages, AC techniques have been vastly understudied compared to DC techniques. </div><div><br></div><div>To overcome this gap in the state of the art, this thesis presents two contributions: First, an experimental study is conducted to elucidate the effect of different damage types, numbers, and sizes on AC transport in a representative self-sensing composite. And second, experimental data is used to inform a computational study on using AC methods to improve damage detection via electrical impedance tomography (EIT) – a conductivity imaging modality commonly paired with self-sensing materials for damage localization. For the first contribution, uniaxial glass fiber specimens containing 0.75 wt.% of carbon nanofiber (CNF) are induced with five types of damage (varying the number of holes, size of holes, number of notches, size of notches, and number of impacts). Impedance magnitude and phase angle were measured after each permutation of damage to study the effect of the new damage on AC transport. It was observed that permutations of hole and notch damages show clear trends of increasing impedance magnitude with the increasing damage, particularly at low frequencies. These damages had little-to-no effect on phase angle, however. Increasing numbers of impacts on the specimens did not show any discernable trend in either impedance magnitude or phase angle, except at high frequencies. This shows that different AC frequencies can be more or less useful for finding particular damage types.</div><div><br></div><div>Regarding the second contribution, AC methods were also explored to improve damage detection in self-sensing materials via EIT. More specifically, the EIT technique could benefit from developing a baseline-free (i.e., not requiring a ‘healthy’ reference) formulations enabled by frequency-difference (fd) imaging. For this, AC conductivity measurements ranging from 100 Hz to 10 MHz were collected from various weight fractions of CNF-modified glass fiber/epoxy laminates. This experimental data was used to inform fdEIT simulations. In the fdEIT simulations, damage was simulated as a simple through-hole. Simulations used 16 electrodes with four equally spaced electrodes on each side of the domain. The EIT forward problem was used to predict voltage-current response on the damaged mesh, and a fdEIT inverse problem was formulated to reconstructs the damage state on an undamaged mesh. The reconstruction images showed the simulated damage clearly. Based on this preliminary study, this research shows that fdEIT does have potential to eliminate the need for a healthy baseline in NDE applications, which can potentially help proliferate the use of this technique in practice.</div>

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