M. Tech. (Civil Engineering, Faculty of Engineering and Technology), Vaal University of Technology) / Modified asphalt concrete is one of the important construction materials for flexible pavements. The addition of polymers and natural hydrocarbon modifiers to enhance the properties of asphalt concrete over a wide temperature range in paving applications has been the common practice. Currently these modified asphalt mixtures are relatively expensive. However, recycled polymers and rubber added to asphalt have also shown similar results in improving the performance of road pavements. In this study, an attempt has been made to use low density polyethylene (LDPE) obtained from plastic waste and crumb rubber obtained from worn out vehicle tyres. The aim was to optimise the proportions of LDPE in the bitumen binder using the ‘wet process’ and crumb rubber aggregates in the hot mix asphalt (HMA) using the ‘dry process’. The Marshall method of bituminous mix design was carried out for varying percentages of LDPE namely 2%, 4%, 6%, 8% and 10% by weight of bitumen binder and 1%, 2%, 3%, 4% and 5% crumb rubber by volume of the mineral aggregates. The characteristics of bitumen modified with LDPE were evaluated. The modified asphalt mix was also evaluated to determine the different mix characteristics. The results from laboratory studies in terms of the rheological properties of the LDPE modified bitumen binder showed an increase in viscosity, softening point and stiffness of the binder. The optimum Marshall stability values for HMA mixtures containing 2% crumb rubber tyre and 4% LDPE were found to be 30% higher than the conventional asphalt concrete mix. The wheel tracking test done at 50ºC was 9.81mm rut depth showing a good rutting resistance of the optimized mixture compared to the conventional asphalt mixes. The Modified Lottman test gave a Tensile Strength Ratio value of 0.979 which indicates a low degree of moisture susceptibility of the modified asphalt mix. The above results showed improved properties of the asphalt mixture. The economic assessment done using the present worth of costs indicated a reduction in maintenance cost due to the extended service life of the modified asphalt pavement.

Devido à demanda dos países em desenvolvimento, a produção de cimento e as emissões de CO2 relacionadas aumenta progressivamente, colocando esta indústria sob pressão devido às preocupações com o aquecimento global. Como diminuir a produção não é uma opção sustentável do ponto de vista social, deve-se primar pela diminuição dos impactos ambientais mantendo-se o aumento da produção. Porém, as principais estratégias de redução das emissões substituição de clínquer por adições, aumento da eficiência de fornos e uso de combustíveis alternativos não são capazes de uma redução que compense o crescimento da produção, mesmo com a disseminação dos maiores esforços industriais possíveis, devido a limites tecnológicos e de disponibilidade de materiais. A captura e sequestro de carbono, por sua vez, pode vir a aumentar significativamente o custo do cimento, prejudicando justamente os países mais necessitados. Novas alternativas são necessárias. Uma delas, ainda pouco desenvolvida, é o aumento da eficiência do uso dos ligantes em materiais cimentícios, como os concretos. Esta tese tem o objetivo de explorar o potencial desta estratégia para contribuir à mitigação das emissões de CO2 da cadeia concreto/cimento. O êxito nesta tarefa tem relação direta com o uso de ferramentas de empacotamento e dispersão de partículas para permitir comportamento reológico adequado à aplicação com uso de menor teor de água na mistura. O trabalho foi dividido em três etapas: 1) levantamento de dados para criação de benchmark da tecnologia atual de concretos com relação e eficiência no uso dos ligantes através de dois indicadores de eficiência Índice de Ligantes (IL) e Índice de CO2 (IC); 2) levantamento da teoria de empacotamento e dispersão de partículas; e 3) estudo experimental demonstrando como a eficiência do uso dos ligantes pode ser aumentada através da aplicação dos conceitos da etapa 2, do controle mais preciso do comportamento reológico e do uso de finos inertes para substituir clínquer para obtenção de parâmetros reológicos. Concluiu-se que o potencial de aumento da eficiência é superior a 50%. Porém, sua implantação em escala comercial dependeria de aumento do controle tecnológico das dosagens de concreto e de profundas modificações na cadeia produtiva e na definição de agregados, fillers, cimento e ligantes. / Due to the increasing demand of developing countries, cement production and related CO2 emissions increases steadily, putting industry under pressure due to global warming constraints. As decreasing production is not a sustainable option from social point of view, environmental loads need to be decreased even maintaining the increase of production. However, current strategies for reducing emissions clinker replacement by mineral additions, increase of kiln efficiency and the use of alternative fuels are not capable of a reduction which could compensate the increasing in production, even with the dissemination of highest industrial efforts due to technological and materials availability limits. Carbon capture and storage, by the time, could increase significantly cement cost, which could harm exactly the neediest countries. New alternatives are needed. One of them, few developed yet, is increasing the efficiency of binder use on cementitious materials, such as concretes. This thesis has the aim of exploring the potential of this strategy for contributing to the mitigation of CO2 emissions of concrete/cement chain. The success in this task is directly related to the use of tools of packing and dispersion of particles for allowing an adequate rheological behavior for the application but with a lower water content in the mixture. The thesis was divided in three main steps: 1) literature research for creating a benchmark of current concrete technology in terms of binder efficiency by two efficiency indexes Binder Intensity (BI) and CO2 Intensity (CI); 2) research of particles packing and dispersion theory; and 3) experimental planning for demonstrating how the binder use efficiency can be significantly increased by the use of concepts from step 2, a more precise rheological behavior control and the use of inert fillers for replacing clinker to obtain rheological parameters. It could be concluded that the potential of efficiency increase is higher than 50%. However, the implantation in commercial scale would depend on the increase of technological control in concrete designs, and also on deep changes in the productive chain and in the definitions of aggregates, fillers, cement and binders.

O processo de moldagem de pós injeção é utilizado para a fabricação de peças de geometrias complexas e com alto volume de produção. Em aplicações ortodônticas e médicas, nas quais são requeridas elevadas durezas e resistências à corrosão, o aço inoxidável 17-4 PH é utilizado aplicando-se aquela técnica de conformação. A atmosfera de sinterização é responsável pelo controle das reações químicas que ocorrem durante a densificação do material e são fundamentais para a qualidade final do produto. O objetivo deste trabalho foi avaliar a influência da atmosfera de sinterização na dureza e resistência à corrosão deste tipo de aço. A remoção dos ligantes primários foi realizada por meio de extração química utilizando-se um solvente com menor impacto ambiental, que se mostrou adequado a tal fim. A extração térmica posterior dos ligantes foi realizada pelo aquecimento nas temperaturas de 250°C e 450°C sendo, posteriormente, a temperatura elevada a 900°C, para o início da sinterização. Utilizou-se atmosferas de Nitrogênio, Vácuo e Hidrogênio, com temperaturas de sinterização de 1250°C e 1330°, com tempos de patamares de 30 e 60 minutos. Verificou-se que as densidades atingidas nas atmosferas de Hidrogênio e Vácuo são semelhantes e se adequaram às especificações requeridas pela norma, enquanto a atmosfera de Nitrogênio resultou em características inferiores. As durezas e as resistências à corrosão obtidas com o uso das atmosferas de Hidrogênio e Vácuo foram também superiores as das amostras sinterizadas em atmosfera de Nitrogênio. / The powder injection molding process is used to manufacture parts with complex shapes, with high production demand. In orthodontic and medical applications, in which high hardness and corrosion resistance are required, 17-4 PH stainless steel is used by applying this forming technique. The sintering atmosphere is responsible for controlling the chemical reactions that occur during material densification and is critical to the ultimate product quality. This research study aims at evaluating the influence of the sintering atmosphere on the hardness and corrosion resistance of this type of steel. The removal of the primary binder was carried out by chemical extraction applying a solvent with less environmental impact, which has proved to be suitable for this purpose. The subsequent binder thermal extraction was held by heating at temperatures of 250°C and 450°C and, therefore, at temperature of 900°C, to initiate sintering. Nitrogen, vacuum and hydrogen atmospheres were used with sintering temperatures at 1250°C and 1330°, with 30 and 60 minute-step time. It was verified that the densities achieved in hydrogen and vacuum atmospheres are similar and suitable by the regulations, whereas the nitrogen atmosphere resulted in lower performance. The hardness and corrosion resistance obtained with the use of hydrogen and vacuum atmospheres were also higher than those obtained for samples sintered in the nitrogen atmosphere.

Les chapes autonivelantes sont souvent composées de ciment alumineux et de sulfate de calcium pour assurer une prise rapide. Le ciment alumineux est généralement à base de monocalcium aluminate (CA). Récemment, un nouveau ciment alumineux riche en mayénite (C12A7) a été conçu pour optimiser l’application des chapes par l’augmentation de la quantité d’ettringite formée. Le développement de l’hydratation au jeune âge (pendant les premières 24 heures) de ce type de produit est pourtant très peu connu. L’objectif principal de cette étude est d’évaluer l’interaction entre l’hydratation au jeune âge et le séchage naturel à travers un modèle de couplage. Ce modèle est appliqué à l’étude d’une pâte pure ettringitique composée de ciment riche en C12A7 et de plâtre alpha. Tout d’abord, un modèle cinétique d’hydratation, initialement développé en système dilué, a été proposé pour étudier l’hydratation d’une pâte pure ettringitique en condition endogène. Il permet de décrire l’évolution en fonction du temps de la porosité, de la teneur en eau, des quantités de phases (réactifs et hydrates). Un modèle de distribution de rayon de pores a été aussi proposé. Ce modèle permet d’obtenir la courbe de pression capillaire au jeune âge nécessaire pour la modélisation des transferts hydriques. Ensuite, une modélisation complète des transferts hydriques a été présentée. Elle a montré que l’hypothèse d’une pression de gaz constante conduit à une surestimation de perte de masse pour des matériaux à faible perméabilité. Pourtant, pour le cas des ciments alumineux, cette hypothèse peut être retenue pour simplifier le couplage avec le modèle cinétique d’hydratation. Enfin, une modélisation des couplages entre l’hydratation et la dessiccation a été développée. L’originalité de ce modèle porte sur l’intégration de la courbe isotherme issue du modèle de distribution poreuse dans la modélisation des transferts hydriques via une fonction Matlab. Le modèle a été capable de reproduire la cinétique de perte de masse d’un échantillon de pâte pure ettringite réactive soumis au séchage précoce. La nécessité de la prise en compte de l’évolution de température a été mise en évidence. De plus, le modèle a prévu un arrêt précoce de l’hydratation à la surface séchante après 10 heures d’hydratation. L’effet de la dessiccation atteint une profondeur de 5 mm sur un échantillon de 3 cm d’épaisseur. / Self-leveling flooring compounds (SLC) are often composed of calcium aluminate cements (CAC) and calcium sulfate to ensure rapid setting. The mineral composition of calcium aluminate cements is usually designed around monocalcium aluminate (CA). Recently, a new cement with the main compound of mayenite (C12A7) has been designed to optimize the application of SLC by increasing the amount of ettringite in the hydration product. However, there is a lack of knowledge related to early-age hydration (during the first 24 hours) of this type of product. The main objective of this study is to evaluate the interaction between early-age hydration and natural drying through a coupling model. This model is applied to the study of an ettringite binder composed of cement rich in C12A7 and plaster First, a kinetic model of hydration, initially developed in a diluted system, has been proposed to study the hydration of an ettringite paste under endogenous conditions. It allows to describe the evolution as a function of time of the porosity, the water content, and the quantities of phases (reactants and hydrates). A model of pore size distribution has also been proposed. This model allows us to obtain the capillary pressure curve at early-age, which is necessary for the modeling of moisture transport. Then, a complete modeling of water transfers was presented. It has shown that the assumption of constant gas pressure leads to an overestimation of mass loss for weakly permeable materials. However, for the case of CAC, this hypothesis can be retained to simplify the coupling with the kinetic model of hydration. Finally, a modeling of the coupling between hydration and desiccation has been developed. The originality of this model concerns the integration of the isothermal curve resulting from the pore size distribution model in the modeling of water transfers via a Matlab function. The model was able to reproduce the kinetics of mass loss of a sample of ettringite binder subjected to early drying. The role of temperature was also elucidated. In addition, the model predicted an early stop of hydration on the drying surface after 10 hours of hydration. The effect of desiccation reaches a depth of 5 mm on a sample with a thickness of 3 cm.

O copolímero SBS é o aditivo mais empregado mundialmente na modificação de ligantes asfálticos, por melhorar diversas de suas características. Um dos principais problemas deste tipo de formulação é a separação de fases, que pode ser minimizada com a incorporação de aditivos. Um novo polietileno de alta densidade e baixo peso molecular oxidado (com denominação comercial TITAN 9686) foi utilizado nesta pesquisa, com o objetivo de testar a hipótese de que a adição de proporções adequadas deste aditivo possa melhorar as características reológicas do asfalto+SBS. O experimento laboratorial foi delineado com base na técnica de experimentos com misturas, englobando um total de nove formulações compostas com asfalto, SBS e TITAN. O teor de SBS variou entre 0 e 5% em peso e o de polietileno variou entre 0 e 2% em peso. Foi utilizado óleo aromático no teor de 4% em peso para todas as nove misturas. As misturas foram analisadas em três condições de envelhecimento: virgem, curto prazo (na estufa RTFO) e longo prazo (na estufa PAV). Foram realizados os seguintes ensaios reológicos: (i) de cisalhamento em regime oscilatório em diferentes condições de temperatura e frequência (para medida do módulo complexo e do ângulo de fase, usados na determinação do grau de desempenho, no cálculo dos parâmetros G*/sen(δ) e G*.sen(δ) e na construção de curvas-mestre), (ii) de viscosidade Brookfield, (iii) de fluência e recuperação sob múltiplas tensões (para medida do percentual de recuperação e da compliância não-recuperável), (iv) de varredura de amplitude linear (para cálculo do parâmetro a f e para ajuste do modelo de fadiga) e (v) de estabilidade à estocagem. Acerca das características escolhidas para mensurar a melhora ou piora das propriedades das misturas asfalto+SBS com a adição de TITAN, podem ser feitas as seguintes observações: (i) a estabilidade à estocagem é melhorada com a adição de TITAN, em particular no teores entre 1 e 2%; (ii) a sensibilidade ao envelhecimento tanto a curto quanto a longo prazos diminui com a adição de TITAN; (iii) a adição de TITAN aumenta a resistência à deformação permanente, à luz dos parâmetros Jnr e R e aumenta a sensibilidade dos ligantes asfálticos modificados com SBS a mudanças bruscas nos níveis de tensão aplicados; e (iv) a adição de TITAN contribui com o aumento da resistência à fadiga, à luz dos parâmetros Nf , a baixos níveis de deformação, e af , e a prejudica reduzindo o parâmetro Nf a altos níveis de deformação e aumentando a temperatura crítica de fadiga ou o parâmetro G*.sen(δ). Tendo por base estas evidências, é possível concluir que a adição de TITAN, em linhas gerais, melhorou a estabilidade dos ligantes asfálticos modificados com até 5,0% de SBS. Com base nas análises realizadas, é possível afirmar que teores da ordem de 1 a 2% de TITAN, para teores de SBS entre 3,0 e 5,0%, são recomendáveis, à luz das propriedades, índices e parâmetros analisados neste trabalho. / The SBS copolymer is the most widely used additive in asphalt binder modification, since it enhances many of the properties of the original material. A critical problem that arises from this type of modification is phase separation, which can be minimized by adding other modifiers to the formulation. A new oxidized, high-density polyethylene with low molecular weight (commercial designation of \"TITAN 9686\") was used in the study with the purpose of verifying the hypothesis that the addition of suitable contents of this modifier can improve the rheological properties of the SBS-modified binder. The laboratory matrix of formulations was based on the experiments with mixtures, and nine types of materials were prepared with asphalt binder, SBS and TITAN. The SBS contents ranged from 0 to 5% by weight, whereas the polyethylene contents ranged from 0 to 2% by weight. These formulations also contained 4% of aromatic oil by weight. Three aging conditions were selected: unaged, short-term aged in the rolling thin-film oven (RTFO) and long-term aged in the pressurized aging vessel (PAV). The following tests were carried out: (i) dynamic oscillatory shear at different temperatures and frequencies of loading for the determination of the complex modulus, the phase angles and the master curves, as well as the performance grades and the numerical values of the parameters G*/sin(δ) and G*.sen(δ); (ii) rotational viscosity; (iii) creep and recovery at multiple stress levels for the determination and the percent recovery and the nonrecoverable compliance; (iv) linear amplitude sweep, in order to calculate the parameter a f and fit the fatigue model to the data; and (v) storage stability. With respect to the characteristics used in the evaluation of the properties of the AC+SBS mixtures after the addition of TITAN, the following observations can be made: (i) storage stability is improved when TITAN is added to the formulation, especially at contents ranging from 1 to 2%; (ii) the sensitivity to the short-term and long-term aging processes decreased with the incorporation of TITAN; (iii) the changes in the R and the Jnr values indicate that the addition of TITAN makes the asphalt binder more resistant to rutting, and also increases the sensitivity of the SBS-modified binders to sudden increases in the stress level; and (iv) the presence of TITAN in the material leads to an increase in the fatigue resistance as based on the parameters Nf and af at low strain levels and the increases in the critical fatigue temperature and the parameter G*.sen(δ). With reference to these evidences, it is possible to conclude that the addition of TITAN generally improves the storage stability of the SBS-modified binders with no more than 5% of copolymer by weight. Based on the results of the present study, it is possible to say that percentages between 1 and 2% of TITAN by weight are recommended for SBS contents between 3 and 5% by weight.

<p>U disertaciji su prikazani rezultati sopstvenog eksperimentalnog istraživanja mogućnosti primjene biopepela, nastalog sagorjevanjem žetvenih ostataka, kao mineralnog dodatka u cementnim kompozitima: malterima i betonima. Istraživanje je zasnovano na komparativnoj analizi 27 vrsta maltera u kojima je varirana vrsta biopepela i vrsta sitnozrnog agregata i 12 vrsta betona koje se razlikuju u vrsti veziva i u krupnom agregatu. Na očvrslom malteru su ispitani: konzistencija, čvrstoća pri pritisku i kapilarno upijanje vode, a na očvrslom betonu ispitivani su kapilarno upijanje vode, skupljanje pri sušenju, čvrstoća pri pritisku, dinamički modul elastičnosti, otpornost na habanje, vodonepropustljivost i čvrstoća na savijanje. Istaknuto je da se primjenom biopepela kao zamjene dijela cementa mogu dobiti konstrukcijski malteri i betoni, odnosno betoni sa zadovoljavajućim fizičkim i mehaničkim karakteristikama.</p> / <p>The dissertation presents the results of an own experimental research on the possibility of using biomass ash as a mineral additive in cement composites: mortar and concrete. The research is based on a comparative analysis of 27 types of mortars in which the type of biomass ash and the type of fine-grained aggregate were varied, as well as 12 types of concrete that differ in the type of binder and coarse aggregate. Following properties were tested on hardened mortars: consistency, compressive strength and capillary water absorption, and on hardened concrete: capillary water absorption, drying shrinkage, compressive strength, dinamic modulus of elasticity, wear resistance, waterpermeability and flexural strength. It was pointed out that biomass ash can be used as a replacement of a part of cement, thereby obtaining satisfactory physical and mechanical characteristics.</p>

Gelfill (GF) is made of tailings, water, binder and chemical additives (Fillset, sodium silicate gel). The components of GF are combined and mixed on the surface and transported (by gravity and/or pumping) to the underground mine workings, where the GF can be used for both underground mine support and tailings storage. Thermal (T), hydraulic (H), and mechanical (M) properties are important performance criteria of GF. The understanding of these engineering properties and their evolution with time are still limited due to the fact that GF is a new cemented backfill material. In this thesis, the evolution of the thermal, hydraulic, mechanical, and microstructural properties of small GF samples are determined. Various binder contents of Portland cement type I (PCI) are used. The GF is cured for 3, 7, 28, 90, and 120 days. It is found that the thermal, hydraulic and mechanical properties are time-dependent or affected by the degree of binder hydration index. Furthermore, a relationship is found between the compressive strength and the saturated hydraulic conductivity of the GF samples. The unsaturated hydraulic properties of GF samples have also been investigated. The outcomes show that unsaturated hydraulic conductivity is influenced by the degree of binder hydration index and binder content, especially at low suction ranges. Simple functions are proposed to predict the evolution of air-entry values (AEVs), residual water content, and fitting parameters from the van Genuchten model with the degree of hydration index (α). Furthermore, two columns are built to simulate the coupled thermo-hydro-mechanical (THM) behaviour of GF under drained and undrained conditions. The obtained results from the GF columns are compared with the small samples. It is observed that the mechanical properties, hydraulic properties (suction and water content), and temperature development are strongly coupled. The magnitude of these THM coupling factors is affected by the size of the GF. The findings also show that the mechanical, hydraulic and thermal properties of the GF columns are different from samples cured in plastic moulds.

Gelfill (GF) is made of tailings, water, binder and chemical additives (Fillset, sodium silicate gel). The components of GF are combined and mixed on the surface and transported (by gravity and/or pumping) to the underground mine workings, where the GF can be used for both underground mine support and tailings storage. Thermal (T), hydraulic (H), and mechanical (M) properties are important performance criteria of GF. The understanding of these engineering properties and their evolution with time are still limited due to the fact that GF is a new cemented backfill material. In this thesis, the evolution of the thermal, hydraulic, mechanical, and microstructural properties of small GF samples are determined. Various binder contents of Portland cement type I (PCI) are used. The GF is cured for 3, 7, 28, 90, and 120 days. It is found that the thermal, hydraulic and mechanical properties are time-dependent or affected by the degree of binder hydration index. Furthermore, a relationship is found between the compressive strength and the saturated hydraulic conductivity of the GF samples. The unsaturated hydraulic properties of GF samples have also been investigated. The outcomes show that unsaturated hydraulic conductivity is influenced by the degree of binder hydration index and binder content, especially at low suction ranges. Simple functions are proposed to predict the evolution of air-entry values (AEVs), residual water content, and fitting parameters from the van Genuchten model with the degree of hydration index (α). Furthermore, two columns are built to simulate the coupled thermo-hydro-mechanical (THM) behaviour of GF under drained and undrained conditions. The obtained results from the GF columns are compared with the small samples. It is observed that the mechanical properties, hydraulic properties (suction and water content), and temperature development are strongly coupled. The magnitude of these THM coupling factors is affected by the size of the GF. The findings also show that the mechanical, hydraulic and thermal properties of the GF columns are different from samples cured in plastic moulds.

Gelfill (GF) is made of tailings, water, binder and chemical additives (Fillset, sodium silicate gel). The components of GF are combined and mixed on the surface and transported (by gravity and/or pumping) to the underground mine workings, where the GF can be used for both underground mine support and tailings storage. Thermal (T), hydraulic (H), and mechanical (M) properties are important performance criteria of GF. The understanding of these engineering properties and their evolution with time are still limited due to the fact that GF is a new cemented backfill material. In this thesis, the evolution of the thermal, hydraulic, mechanical, and microstructural properties of small GF samples are determined. Various binder contents of Portland cement type I (PCI) are used. The GF is cured for 3, 7, 28, 90, and 120 days. It is found that the thermal, hydraulic and mechanical properties are time-dependent or affected by the degree of binder hydration index. Furthermore, a relationship is found between the compressive strength and the saturated hydraulic conductivity of the GF samples. The unsaturated hydraulic properties of GF samples have also been investigated. The outcomes show that unsaturated hydraulic conductivity is influenced by the degree of binder hydration index and binder content, especially at low suction ranges. Simple functions are proposed to predict the evolution of air-entry values (AEVs), residual water content, and fitting parameters from the van Genuchten model with the degree of hydration index (α). Furthermore, two columns are built to simulate the coupled thermo-hydro-mechanical (THM) behaviour of GF under drained and undrained conditions. The obtained results from the GF columns are compared with the small samples. It is observed that the mechanical properties, hydraulic properties (suction and water content), and temperature development are strongly coupled. The magnitude of these THM coupling factors is affected by the size of the GF. The findings also show that the mechanical, hydraulic and thermal properties of the GF columns are different from samples cured in plastic moulds.

Ce travail de thèse a pour but de suivre le comportement du liant ionomère après vieillissement en condition réelle d'utilisation de la pile. Dans un premier temps, diverses techniques de caractérisation en phase solide ont été utilisées afin d'étudier le ionomère présent dans les électrodes. La majeure partie de ces techniques se sont avérées insatisfaisantes pour le suivi du vieillissement du ionomère. Seule l'analyse par diffraction rayon X (DRX) a mis en avant un changement d'organisation structurale du ionomère dans les électrodes. Par la suite, nous avons choisi de caractériser le ionomère en solution après extraction par l'eau. Préalablement, un protocole de quantification en 2 à 3 étapes, dans lequel intervient une quantification via le rapport signal-sur-bruit (S/N), a été mis en place afin de quantifier le Nafion® et autres petites molécules fluorés. L'extraction Soxhlet a ensuite été réalisée sur les électrodes permettant de révéler la présence d'un produit de dégradation hydrosoluble après fonctionnement en pile, à la fois en cathode et en anode. Enfin, la macération des électrodes dans le diméthylacétamide (DMAc) a permis d'extraire le polymère Nafion® ainsi que deux acides : l'acide trifluoroacétique (TFA) et l'acide triflique (TFI). En conclusion, la corrélation de l'ensemble des observations nous a permis de proposer un mécanisme de dégradation du liant ionomère présent dans les électrodes. / The purpose of this study was to follow the behavior of ionomer binder after fuel cell operation. First, a series of techniques were used to investigate to characterize ionomer in electrode at solid state. Most of them were inefficient to study ionomer degradation. Only X-Ray Diffraction (XRD) pointed out a structural change of the binder in electrodes. Second, it has been decided to characterize ionomer in liquid state after water extraction. But first of all, a quantitative 19F NMR protocol composed of two to three steps, with a first step using a quantification through signal-to-noise ratio (S/N), was establish in order to quantify Nafion® and degradation products. Soxhlet extraction performed on electrodes allowed to detect a degradation product water-soluble. Finally, extraction with organic solvent (Dimethylacetamide) allowed to extract Nafion® and two acid: trifluoroacetic acid (TFA) and triflic acid (TFI) from electrodes. In conclusion, correlation between observation and literature allowed us to propose a degradation mechanism of ionomer in electrodes.