Polymer/clay nanocomposites consisting of an epoxy resin matrix filled with organoclays have been investigated. The main objective of this study was to determine which combination of components led to the greatest enhancement in properties of the epoxy resin. Exfoliation of the clay was desired, as exfoliated nanocomposites are known to exhibit great improvements in mechanical properties [1]. The epoxy resins studied were di-functional DGEBA and tetra-functional TGDDM. The epoxy resin was cured with three different hardeners, these included: the high functionality amine hardener, TETA, and two anhydride hardeners, accelerated MTHPA and pure HHPA. The three organoclays used, contained alkylammonium cations and were also compared to the unmodified clay. Morphology was investigated by XRD and TEM, and the flexural properties of the resulting nanocomposites were studied. The effect that the addition of an organoclay has on the cure of the epoxy resin was investigated using MDSC. Both the temperatures required to cure the resin with, and without, the clay, and any changes in the total heat flow that occurred were studied. The Tg++ of the cured nanocomposites was also measured using MDSC. The heat flow results indicated that the clays added to the epoxy resins act as a physical barrier, which prevents the resin from reaching full cure. In the higher functional resin, the addition of clay resulted in a significant decrease in the total heat flow, suggesting that a large amount of epoxy remains uncured, and, as a result, there should be a reduction in the amount of cross-linking. The lower cross-link density led to a significantly lower Tg and the mechanical properties were also poorer. The reactivity of the hardener towards the resin was found to have the greatest impact on the cured nanocomposite morphology. Intragallery polymerisation occurring at a faster rate than the extragallery polymerisation causes exfoliation. In order to achieve a balance that favours intragallery polymerisation, it was found that the curing reaction was required to be catalysed by the alkylammonium cation of the organoclay, and not catalysed by other means. The DGEBA cured with HHPA provided the largest layer expansion in the clay structure due to the alkylammonium cation catalysing the anhydride ring-opening reaction. The effect was not seen with TGDDM due to the tertiary amine in its structure. The accelerator within the MTHPA assisted extragallery polymerisation of the resin and the TETA cured readily without additional catalysis.

Thesis (M. S.)--Chemical Engineering, Georgia Institute of Technology, 2009. / Committee Chair: Nair, Sankar; Committee Member: Koros, William; Committee Member: Ludovice, Peter; Committee Member: Meredith, Carson; Committee Member: Thio, Yonathan; Committee Member: Zhou, Min.

Submitted by Aelson Maciera (aelsoncm@terra.com.br) on 2017-08-28T17:47:20Z No. of bitstreams: 1 TeseJPFS.pdf: 7489825 bytes, checksum: c319cc8a992956b23bf6db8d3857c32c (MD5) / Approved for entry into archive by Ronildo Prado (bco.producao.intelectual@gmail.com) on 2018-01-17T18:50:59Z (GMT) No. of bitstreams: 1 TeseJPFS.pdf: 7489825 bytes, checksum: c319cc8a992956b23bf6db8d3857c32c (MD5) / Approved for entry into archive by Ronildo Prado (bco.producao.intelectual@gmail.com) on 2018-01-17T18:51:10Z (GMT) No. of bitstreams: 1 TeseJPFS.pdf: 7489825 bytes, checksum: c319cc8a992956b23bf6db8d3857c32c (MD5) / Made available in DSpace on 2018-01-17T19:05:30Z (GMT). No. of bitstreams: 1 TeseJPFS.pdf: 7489825 bytes, checksum: c319cc8a992956b23bf6db8d3857c32c (MD5) Previous issue date: 2017-06-23 / Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / In this work conductive polymer nanocomposites (CPNs) based on block copolymers and multi walled carbon nanotubes (MWCNT) were obtained. Two of the copolymers were commercial: polystyrene-b-polybutadiene-b-polystyrene (SBS), and polystyrene-b-poly(ethylene-butylene)-b-polystyrene (SEBS). The other copolymer was synthesized: polystyrene-b-poly(vinylidene fluoride) (PS-b-PVDF). Three systems of block copolymer/MWCNT were then obtained and studied for specific purposes. The SBS/MWCNT was produced using two routes: the solution and melt mixing. The influence of the processing conditions on the structure and on the electrical conductivity of these nanocomposites were evaluated and compared. For the second system, SEBS/MWCNT, the aim was evaluate the influence of the grafting of MWCNT with PS on the conductivity of the nanocomposites. For the third system, PS-b-PVDF/MWCNT, the aim was to evaluate the influence of the polymer matrix on the conductivity of the nanocomposites. The nanocomposites had their electrical properties evaluated by measurements of DC electrical conductivity and AC impedance spectroscopy. Their morphologies were evaluated by atomic force microscopy (AFM) and electron microscopy; and their structures were analyzed by small angle X ray scattering (SAXS). The results showed that the higher electrical conductivities and the lower percolation thresholds were obtained for the SBS/MWCNT nanocomposites obtained by the solution technique. The SEBS/MWCNT nanocomposites with PS grafted on MWCNT had higher conductivity than the non-grafted systems. The nanocomposites PS-b-PVDF/MWCNT had also better conductivities than the PVDF/MWCNT. Therefore, it was shown that both the modification of the processing, as well as the filler and the matrix are suitable approaches to control the structures and the electrical conductivity of CPNs based on MWCNT and block copolymers. / Neste trabalho de doutorado foram obtidos nanocompósitos poliméricos condutores (NPCs) baseados em copolímeros em bloco e nanotubos de carbono de paredes múltiplas (MWCNT). Dois dos copolímeros utilizados são comerciais: os triblocos poliestireno-b-polibutadieno-b-poliestireno (SBS), e o poliestireno-b-poli(etileno-butileno)-b-poliestireno (SEBS). O outro copolímero foi sintetizado: o poliestireno-b-poli(difluoreto de vinilideno) (PS-b-PVDF). Três sistemas copolímero em bloco/MWCNT foram então obtidos e estudados com objetivos específicos. Para o primeiro sistema, SBS/MWCNT, o objetivo foi o de avaliar e comparar a influência do processamento na condutividade elétrica dos nanocompósitos. Para o segundo sistema, SEBS/MWCNT, o objetivo foi o de avaliar a influência da enxertia de PS nos MWCNT nas condutividades dos nanocompósitos. Para o terceiro sistema, PS-b-PVDF/MWCNT, o objetivo foi o de avaliar a influência da matriz polimérica na condutividade elétrica. Os nanocompósitos tiverem suas propriedades elétricas avaliadas por medidas de condutividade elétrica DC e por espectroscopia de impedância AC; tiveram suas morfologias avaliadas por microscopia de força atômica (AFM) e microscopia eletrônica, e suas estruturas avaliadas por raios X de baixo ângulo (SAXS). Os resultados mostraram que as maiores condutividades elétricas e menores limites de percolação foram obtidos para os nanocompósitos SBS/MWCNT processados por mistura por solução em relação aos obtidos por mistura no estado fundido; para os nanocompósitos SEBS/MWCNT com MWCNT enxertados com PS em relação aos não enxertados; para os nanocompósitos do copolímero PS-b-PVDF/MWCNT, em relação aos do homopolímero, PVDF/ MWCNT. Desta maneira, ficou demonstrado que tanto a modificação do processo, quanto da carga, quanto da matriz podem induzir a diferentes estruturações do material e podem ser meios favoráveis para controle da condutividade elétrica de NPCs baseados em copolímeros em bloco e MWCNT. / FAPESP: 2014/17597-2 / FAPESP: 2015/09924-6 / CNPq: 141456/2013-2

Structurer les matériaux composites, pour au moins une des phases, à l’échelle nanométrique, c’est-à-dire former des matériaux nanocomposites, est une voie pour optimiser nombre de leurs propriétés. Le domaine de la propulsion et des propergols n’échappe pas à cette règle. C’est dans ce contexte que s’est déroulée cette thèse sur la synthèse de nanocomposites ‘nanoparticules métalliques/polymère’ en milieux fluides supercritiques (FSCs). Les principales étapes rencontrées dans l’élaboration de nanocomposites en milieu scCO2 ont été étudiées : i) Etude thermodynamique des systèmes polymère/scCO2, ii) Mesure de leur viscosité et iii) Synthèse de nanoparticules inorganiques dans des polymères en milieux FSCs. De plus, une partie importante de la thèse a concerné la synthèse de nanoparticules d’aluminium en milieux fluides supercritiques en vue de leur intégration dans des matrices polymères pour des applications propergols. / Structuring composite materials, at least for one phase, at the nanometer scale, that is to say synthesize nanocomposite materials, is an interesting way to optimize their properties. The field of propulsion and propellants follows this rule. This is the context of this PhD dealing with the synthesis of nanocomposites constituted of metallic nanoparticles and polymer in supercritical fluids. The main steps for the formation of nanocomposites in scCO2 have been studied: i) Thermodynamical study of polymer/scCO2 systems, ii) Viscosity measurements of polymer/scCO2 systems and iii) Synthesis of inorganic nanoparticles in polymers in supercritical fluids. Moreover, an important part of this work has concerned the synthesis of aluminum nanoparticles in supercritical fluids in order to incorporate them in polymer matrixes for applications to propellants.

Made available in DSpace on 2014-12-17T14:06:57Z (GMT). No. of bitstreams: 1 AntonioMM_DISSERT.pdf: 3167534 bytes, checksum: a8247e394e6c3656375c3f16b429e065 (MD5) Previous issue date: 2010-10-15 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Poly(methyl methacrylate)/clay nanocomposites were prepared by melt mixing using a montmorillonite-rich clay (MMT). The clay in natura was treated with acrylic acid to facilitate the dispersion in the polymer matrix. A masterbatch of PMMA/clay was prepared and combined with the pure PMMA and then subjected to extrusion process using singlescrew and twin-screw extruders followed by injection. Nanocomposites were processed with clay contents of 1, 3, 5 and 8 wt.%. The effect of shear processing on the morphology of the nanocomposites was evaluated by XRD, SEM and TEM. Thermal and mechanical properties of the nanocomposites were investigated through TGA, DSC, HDT, VICAT, tensile and impact tests, to evaluate the effect of the addition of clay to the PMMA matrix. Flammability tests were also conducted to investigate the effect of the addition of clay on the flame retardation properties. SEM images of the nanocomposites indicated the presence of clay agglomerates, which resulted in the reduction of properties such as thermal stability, mechanical strength and impact resistance, and increased the rate of burning for materials processed by both extrusion routes / Nanocomp?sitos de poli(metacrilato de metila) (PMMA) foram preparados a partir da t?cnica de mistura no estado fundido com argila rica em montmorilonita (MMT). A argila in natura foi inicialmente tratada com ?cido acr?lico para facilitar a dispers?o na matriz polim?rica. Depois, foi preparado um concentrado de PMMA e argila que foi combinado com o PMMA puro e submetido ao processo de extrus?o realizado em extrusoras monorosca e dupla rosca com posterior inje??o. Nanocomp?sitos foram processados com 1, 3, 5 e 8% em massa de argila. O efeito do cisalhamento sobre a morfologia dos nanocomp?sitos foi avaliado por DRX, MEV e MET. Para avaliar o efeito da adi??o de argila na matriz de PMMA foram investigadas propriedades t?rmicas e mec?nicas, atrav?s de an?lises de TG, DSC, HDT, VICAT, tra??o e impacto. Ensaios de inflamabilidade foram tamb?m realizados para investigar o efeito da adi??o de argila sobre as propriedades de retardo de chama. As an?lises morfol?gicas mostraram a presen?a de aglomerados de argila distribu?dos na matriz de PMMA, o que resultou na redu??o de propriedades como estabilidade t?rmica, resist?ncia mec?nica e ao impacto, e elevou a taxa de queima para os materiais processados por ambas as rotas de extrus?o

Made available in DSpace on 2014-12-17T14:07:18Z (GMT). No. of bitstreams: 1 LourdesARR_TESE.pdf: 12458480 bytes, checksum: 0efd4ff8bfb0c0bf6bcd3c18e449a690 (MD5) Previous issue date: 2013-05-17 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / Nacomposites of polymers and lamellar clayminerals, has generated high scientific and technological interest, for having mechanical properties and gas barriers differentiated of polymers and conventional composites. In this work, it was developed nanocomposites by single screw extruder and injection, utilizing commercial raw material, with the goal to investigate the quality of new developed materials. It was evaluated the influence of the content and the kind of clay in the structure and in the nanocomposites properties. It was used regular and elastomeric poly (methyl methacrylate) (Acrigel LEP 100 and Acrigel ECP800) and six montmorillonites (Cloisite 10A, 11B, 15A, 20A, 25A e 30B) at the concentration of 1% e 3% in weight. The nanocomposites were characterized by X-ray diffraction (XRD), thermal gravimetric analysis (TGA), transmission electron microscopy (TEM), colorimetric, optical transparency, flexural and tensile tests, Rockwell hardness and esclerometry. It was founded that is possible to obtain intercalated and exfoliated nanocomposites PMMA/MMT, and the top results was obtained in the materials with 1%in clay weight organophilizated with 2M2HT (Cloisite 15A and 20A) presented intercalate and hybrid morphology (exfoliated and flocullated). The ones that was produced with organophilizated clay with 2MHTL8 (Cloisite 30B) had excellent visual quality, but the majority presented hybrid morphology. In the materials processed with organophilizated clay with MT2ETOH (Cloisite 30B), there were color change and loss of transparency. It occurs improvement in a few mechanical properties, mainly in the materials produced with PMMA elastomeric (Acrigel ECP800), being more significant, the increase in the resistance to stripping in those nanocomposites / Nanocomp?sitos de pol?meros e argilominerais lamelares t?m gerado alto interesse cient?fico e tecnol?gico por possu?rem propriedades mec?nicas e de barreira ? g?s diferenciadas de pol?meros e de comp?sitos convencionais. Neste trabalho, foram desenvolvidos nanocomp?sitos por meio de extrusora monorosca e injetora, utilizando mat?rias-primas comerciais, com a finalidade de investigar a qualidade dos novos materiais desenvolvidos. Foi avaliada a influ?ncia do teor e do tipo de argila na estrutura e nas propriedades dos nanocomp?sitos. Foram usados PMMA comum e elastom?rico (Acrigel? LEP100 e Acrigel? ECP800) e seis argilas montmorilonitas (Cloisite? 10A, 11B, 15A, 20A, 25A e 30B) nas concentra??es de 1% e 3% em peso. Os nanocomp?sitos foram caracterizados por difra??o de raios X (DRX), termogravimetria (TGA), microscopia eletr?nica de transmiss?o (MET), colorimetria, transpar?ncia ?ptica, ensaios de tra??o uniaxial, flex?o, dureza Rockwell e esclerometria. Constatou-se que ? poss?vel obter nanocomp?sitos PMMA/MMT intercalados e esfoliados, sendo os melhores resultados obtidos nos materiais processados com 1% em peso de argilas organofilizadas com 2MBHT (Cloisite? 10A e 11B). Materiais produzidos com argilas organofilizadas com 2M2HT (Cloisite? 15A e 20A) apresentaram morfologia intercalada e h?brida (esfoliada e floculada). J? os produzidos com argilas organofilizadas com 2MHTL8 (Cloisite? 25A) tiveram excelente qualidade visual, por?m a maioria apresentou morfologia h?brida. Nos materiais processados com argilas organofilizadas com MT2ETOH (Cloisite? 30B) houve altera??o na cor e perda da transpar?ncia. Houve melhoria em algumas propriedades mec?nicas, principalmente nos materiais produzidos com PMMA elastom?rico (Acrigel? ECP800), sendo mais significativo, o aumento na resist?ncia ao riscamento nesses nanocomp?sitos

Orientador: Marcelo Ornaghi Orlandi / Banca: Walter Katsumi Sakamoto / Banca: Emerson Rodrigues de Camargo / Resumo: Nanocompósitos são materiais que combinam duas (ou mais) fases sólidas, uma das quais deve possuir dimensões nanométricas, que pode reunir em um único material várias propriedades melhoradas para uma dada aplicação e, portanto, podem permitir a coexistência de propriedades tradicionalmente antagônicas como, transparência e condutividade. O presente trabalho teve como objetivo a obtenção de um nanocompósito polimérico transparente e condutor de polimetilmetacrilato - PMMA com nanofitas do sistema Indium Tin Oxide - ITO. Para isto primeiramente estudou-se a influência da temperatura na síntese das nanoestruturas de ITO e depois de obtida a temperatura de síntese que proporcionou o crescimento de nanofitas de ITO com maior condutividade e maior transparência no espectro visível, estudou-se a influência da inserção destas nanofitas nas propriedades ópticas e elétricas de filmes nanocompósitos de PMMA. Como as nanofitas obtidas são emaranhadas, para a obtenção do nanocompósito foi realizada uma separação prévia das mesmas utilizando duas dispersões distintas: sendo a primeira em um ultrasom convencional e a segunda em uma ponta ultrasônica. Depois de dispersas, as nanofitas foram misturadas ao PMMA comercial dissolvido em concentrações mássicas de 1%, 2%, 5% e 10% de nanofitas. As soluções foram então depositadas sobre substrato de vidro e, depois de secos, os filmes foram destacados. As caracterizações ópticas mostraram que a transmitância no espectro visível dos filmes diminui em função do aumento da quantidade de nanofitas no compósito. Neste estudo, as caracterizações elétricas mostraram que ocorreu percolação das nanofitas no polímero após a inserção de 5% em massa de nanofitas. As imagens de MET para os filmes corroboraram os resultados previstos pelas caracterizações elétricas. Os filmes... (Resumo completo, clicar acesso eletrônico abaixo) / Abstract: Nanocomposites are materials which have two or more solid phases, and one of these phases should be in nano-sized scale range. These materials can have several properties increased for special application and it is possible to obtain composites with traditionally antagonistic combinations of properties, such as transparence in the visible range of light and good conductivity. The main goal of this work is obtain a transparent and conductive polymer-based nanocomposite using polymethylmethacrylate - PMMA and ITO (Indium Tin Oxide) nanobelts. To reach this goal it was first studied the influence of temperature on the synthesis of nanostructured ITO. Once the temperature of synthesis was optimized to ensure the growth of ITO nanobelts with both good conductivity and good transparency in the visible spectrum, we studied the influence of ITO nanobelts on the electrical and optical properties of nanocomposites of PMMA. Because the synthesized nanobelts are entangled each other, to obtain the composite it was realized a separation of them using two different ways; first using a conventional ultrasound and after an ultrasonic tip. Then, nanobelts were mixed with commercial PMMA dissolved in THF 10% in mass concentrations of 1%, 2%, 5% and 10%. So, the solution was deposited over a glass substrate by casting. The results showed that films transmittance in visible range decreases by increasing the amount of nanobelts. The electrical characterization showed that percolation occurred after 5%wt of filler. TEM images of composites corroborate the results provided by the electrical measures. The films prepared using both dispersions had the same transmittance in the visible spectrum, despite of the films obtained by dispersing the nanobelts in ultrasonic tip had a lower electrical resistance. Thus it can be concluded that the dispersion by ultrasonic... (Summary complete electronic access click below) / Mestre

No fim do século XX cresceu o interesse por materiais com potencial para aplicação na área da nanotecnologia. Um destes materiais é o grafeno (alótropo do carbono da espessura de um átomo), indicado para aplicações que exploram desde propriedades ópticas até mecânicas. Todavia, os métodos de produção estabelecidos até o momento geram normalmente um produto com alto grau de defeitos estruturais. Por isso, o objetivo deste estudo foi desenvolver um método mais brando para obtenção de grafeno, por meio do desenrolamento de nanotubos de carbono (NTC) de parede múltipla na presença de líquidos iônicos (LI) (que possuem caráter lubrificante e estabilizador) e adicioná-lo à resina epoxídica para avaliar seu efeito nas propriedades do nanocompósito. A metodologia consistiu em definir a rota a que a mistura NTC:LI (bis(trifluorometanosulfonil)imidato de 1-n-butil-3-metilimidazólio – BMImNTf2), na proporção 1:10, deveria ser submetida e depois avaliar variações para validação do método (alteração de temperatura, solventes – LI BMImCl e tolueno e nanocarga – grafite). As misturas de grafeno-NTC/LI produzidas foram adicionadas na proporção de 0,1% em massa de grafeno-NTC à resina epoxídica. A caracterização das misturas se deu pelas técnicas de microscopia eletrônica de transmissão (MET), espectroscopia Raman e microscopia de força atômica (AFM), e dos nanocompósitos, também por microscopia eletrônica de varredura (MEV), análise termogravimétrica (TGA), calorimetria diferencial exploratória (DSC), infravermelho (IV) análise dinâmico-mecânica (DMA) e ensaios mecânicos. A morfologia observada em MET e AFM evidenciou que a rota em que a mistura permaneceu 3 h em aquecimento e agitação magnética sob vácuo e 3 h sob sonificação resultou em grafeno de algumas camadas. Os resultados de Raman mostraram que foi produzido grafeno de boa qualidade, baseando-se na razão ID/IG. Nos nanocompósitos, confirmou-se que BMImNTf2 mantém as folhas de grafeno abertas. Já com BMImCl a morfologia dos NTC permanece inalterada, mas seu grau de emaranhamento é diminuído pela ação lubrificante deste LI, o que reflete em melhoria na resistência ao impacto. Os NTC sem a presença de um LI de forma geral não conferiram melhoria à matriz polimérica (ex: queda de 35% na dureza). / In the late twentieth century, the interest in materials with potential application in the nanotechnology´s field has increased. One of these materials is graphene (carbon allotrope of a single atom thickness), suitable for applications, which exploit properties such as optical or mechanical. However, the methods developed up to now to obtain graphene usually generate a product with high degree of structural defects. Therefore, the aim of this study was to produce graphene sheets through a milder route of unrolling multi-walled carbon nanotubes (CNT) in ionic liquids (IL; which have a lubricating and stabilizing character) and to add it to an epoxy resin to evaluate its effect on the nanocomposite properties. The methodology consisted of defining the route through which the 1:10 mixture of CNT:IL (1-n-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imidate - BMImNTf2) should be submitted, and then evaluate possible variations for validating the method (change in temperature, solvents - toluene and IL BMImCl and nanofiller - graphite). The produced graphene-CNT/IL mixtures were added at 0.1% by weight of graphene-CNT to epoxy resin. Characterization of the graphene/IL mixtures was done by transmission electron microscopy (TEM), Raman spectroscopy and atomic force microscopy (AFM), and the nanocomposites also by scanning electron microscopy (SEM), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), dynamical mechanical analysis (DMA) and mechanical tests. The morphology observed using TEM and AFM showed that the route based on 3 h under heating, stirring and vacuum, followed by 3 h of sonication leads to CNT unrolling. Raman spectra showed that the produced graphene was of good quality, based on the low ID/IG ratio. In the nanocomposites, CNT unrolling was confirmed when IL BMImNTf2 was used, yielding reasonable property improvements. In the case of IL BMImCl, the unrolling of the CNT did not occur, but the lubricant effect of the IL decreased the degree of entanglement, which increased its impact strength. Differently, the non-treated CNT generally reduced the properties of the polymer matrix, e.g. a 35% drop in hardness.

Un nouveau type de Senseur de déformation Résistif Quantique (QRS) à base de nanotubes de carbone (CNT) a été développé pour le suivi de santé de structures composites (SHM). Les senseurs ont été fabriqués directement par pulvérisation en couche par couche (sLBL) sur la surface de fibres de verre ou de carbone d'une formulation de nanoComposites Polymères Conducteurs (CPC). La réponse des transducteurs CPC a été étudiée sous diverses sollicitations mécaniques en mode statique et dynamique. Différentes stratégies de suivi de santé des composites à l'aide de senseurs piézo-résistifs ont été comparées en termes d'efficacité de suivi des sollicitations mécaniques dans les domaines élastique et plastique et des endommagements. Les résultats montrent que les réponses des senseurs conservent toutes les caractéristiques statiques et dynamiques d'entrée fournissant ainsi des informations utiles pour le SHM. Cela permet d'envisager leur déploiement dans des pièces composites de grandes dimensions, pour évaluer les déformations et les concentrations de contraintes locales et ainsi faciliter la simulation et la modélisation dans ces zones critiques. La réponse électrique des QRS a aussi été utilisée pour évaluer l'accumulation d'endommagement dans les composites en association avec la microscopie et l'émission acoustique (AE) afin de détecter l'initiation de fissures et leur propagation dans des composites stratifiés. Sur la base des résultats obtenus dans cette étude, les QRS étudiés peuvent être considérées comme des capteurs en temps réel peu intrusifs qui semblent être tout à fait appropriés pour effectuer des mesures dvnamioues dans des aoolications d'inoénierie structurelle. / A new type of carbon nanotubes based Quantum Resistive Strain sensor (QRS sensor) for structural health monitoring (SHM) has been developed directly on glass fibers' surface via spray layer by layer (slbl) technique. The response of similar transducers was investigated under varying static and dynamic sollicitations. Different strategies of piezo-resistive sensing in GFRP are compared in terms of efficiency to follow mechanical solicitations and damages in both elastic and plastic demains. The results demonstrate that the sensors' output retains ail static and dynamic features of the input thus providing useful information for SHM and further can be extended for composite parts with large dimensions, to probe local stress/strain concentrations and facilitate the simulation of these critical areas. The electrical responses of QRS combined with those of the acoustic emission (AE) technique and microscopy have allowed investigating damage initiation and propagation in laminated composites. Based on the results obtained in this study, the investigated QRS can be considered as real time in situ non strongly invasive sensors which appear to be suitable for performing dynamic measurements in structural engineering applications.

Submitted by Maria Medeiros (maria.dilva1@ufcg.edu.br) on 2018-06-26T13:22:14Z No. of bitstreams: 1 EDUARDO DE MELLO SILVA - TESE (PPGCEMat) 2016.pdf: 5216619 bytes, checksum: 8f7a31431fc1647b163344adf16c2291 (MD5) / Made available in DSpace on 2018-06-26T13:22:14Z (GMT). No. of bitstreams: 1 EDUARDO DE MELLO SILVA - TESE (PPGCEMat) 2016.pdf: 5216619 bytes, checksum: 8f7a31431fc1647b163344adf16c2291 (MD5) Previous issue date: 2016-02-29 / Capes / O presente trabalho trata da obtenção e caracterização de filmes planos de PEBDL/bentonita com e sem a incorporação de um agente compatibilizante (PE-gMA). Os filmes foram obtidos por extrusão plana e suas propriedades mecânicas, de permeabilidade e térmicas foram avaliadas em função do teor (0 a 5% em massa) e do tipo de carga incorporada. Duas argilas foram utilizadas: a) uma bentonita de origem local (Paraibana) e b) uma argila organofílica comercial importada. A argila paraibana foi purificada e organofilizada antes de ser incorporada à matriz polimérica. As argilas utilizadas foram caracterizadas através da sua capacidade de troca catiônica (CTC), por difração de raios-x (DRX), por espectroscopia no infravermelho por transformada de Fourier (FTIR), análise da composição química por energia dispersiva (EDX), análise granulométrica e por análise termogravimétrica (TGA). Os nanocompósitos obtidos na forma de filmes planos foram caracterizados por DRX, microscopia eletrônica de varredura (MEV), permeabilidade ao vapor de água e aos gases O2 e CO2, propriedades mecânicas, análise termogravimétrica (TGA) e análise da calorimetria exploratória diferencial (DSC). Os filmes de nanocompósitos com compatibilizante apresentaram morfologia intercalada/parcialmente esfoliada e os filmes sem a presença do compatibilizante apresentaram morfologia compatível com a de nanocompósitos intercalados/microcompósitos. Os resultados das propriedades mecânicas mostraram que os filmes preparados com o agente compatibilizante apresentaram propriedades superiores à da matriz pura e às dos outros sistemas preparados. A presença do agente compatibilizante reduziu significativamente a permeabilidade ao vapor de água e a permeabilidade ao gás O2 nos filmes, mas os filmes sem a presença do agente compatibilizante apresentaram aumento desta propriedade quando comparados ao filme de PEBDL puro. As analises térmicas mostraram um aumento discreto da estabilidade térmica para os filmes de nanocompósitos preparados com o agente compatibilizante. / The present work deals with the manufactur and characterization of flat films of LLDPE/bentonite with and without the incorporation of a compatibilizing agent (PE-g-MA). The films were obtained by flat die extrusion and its mechanical, permeability and thermal properties were evaluated in function of clay content (0 to 5% by mass) and clay identity. Two clays were used: a) a local bentonite (from Paraiba) and b) an imported commercial organoclay. The local clay was purified and organophilized before being incorporated into the polymer matrix. The clays were characterized by cation exchange capacity (CEC), x-ray diffraction (XRD), spectroscopy Fourier transform infrared (FTIR), analysis, chemical composition by dispersive energy (EDX), particle size analysis and by thermogravimetric analysis (TG). Nanocomposites obtained as flat films were characterized by XRD, scanning electron microscopy (SEM), water vapor, O2 and CO2 gas permeability, mechanical properties, thermogravimetric analysis (TG) and differential scanning calorimetry (DSC). The nanocomposite films with compatibilizer showed an intercalated/partially exfoliated morphology while the morphology of the films without compatibilizer was compatible with that of intercalated nanocomposites/microcomposites. The mechanical properties of the films prepared with the compatibilizer agent were higher than those of the neat matrix and the other systems prepared. Compatibilizing agent addition significantly reduced water vapor and O2 gas permeability in films, but the films without the presence of the compatibilizer showed an increase of this property when compared to pure LLDPE film. The influence of compatibilizer addition on CO2 permeability was small. Thermal analyzes showed a slight increase of thermal stability for the films of nanocomposites prepared with the compatibilizing agent.