Ce travail de thèse vise à identifier les mécanismes par lesquels la fraction volumique de charges, la distribution de tailles des charges, le comportement mécanique du liant et les propriétés d’adhésion liant/charge des propergols composites influent sur le comportement mécanique jusqu’à rupture de ces matériaux. Des calculs de microstructures 2D par éléments finis sont mis en œuvre pour caractériser qualitativement l’évolution de la microstructure du composite au cours d’une sollicitation de traction uniaxiale à faible vitesse de déformation. Ils prennent notamment en compte un modèle de zone cohésive pour représenter la décohésion à l’interface liant/charge et un critère original de ruine de la microstructure. Les résultats numériques sont favorablement comparés aux tendances obtenues expérimentalement sur propergols composites industriels et modèles. Par ailleurs, une validation de l’approche qualitative précédente est conduite en effectuant une confrontation quantitative du comportement mécanique et de la variation volumique d’un composite modèle, obtenus par simulation de microstructures 3D et par caractérisations expérimentales. Enfin, la tenue du propergol dans un assemblage propergol/lieur soumis à un test de pelage est étudiée expérimentalement. / This work aims at understanding the relationship between solid propellants particles volume fraction, particles size distribution, binder mechanical properties and binder/particles bonding with the mechanical behavior up to failure of these materials. Finite elements analyses on 2D microstructures are performed in order to qualitatively characterize the microstructure evolution throughout uniaxial tensile loading at small strain rate. These simulations account for the binder/particles debonding with a cohesive zone model and implement an original failure criterion. Simulation and experimental results are consistent. Besides, a quantitative comparison between simulations on 3D microstructures and experimental data is drawn in order to validate the above qualitative results. It is performed on a model composite and compares both the mechanical behavior and the volume variations. At last, the propellant failure during a peeling test of the liner/propellant structure is studied experimentally.

Dans le cadre d’une Cifre avec Airbus Helicopters, le projet a pour but le développement d’un modèle pour le pré-dimensionnement de pièces lamifiées élastomère-métal dont le rôle est critique en termes de conception et de sécurité pour les architectures de rotors d’hélicoptères. Pour cela, un premier volet de la thèse a consisté à caractériser le comportement élasto-dissipatif du matériau d’étude (un butadiène chargé de noir de carbone) via une campagne d’essais statiques et dynamiques, sous différents modes de sollicitations (uniaxiales et biaxiales) et sur un spectre assez large de fréquences, d’amplitudes et de températures. A partir de ces observations, un modèle phénoménologique de comportement hyper-viscoélastique est proposé. Sur la base d’un modèle de Maxwell généralisé, il permet de traduire les phénomènes observés sur la gamme de sollicitations visées. Un accent particulier a été porté sur la prise en compte de l’effet Payne en adoptant une approche originale. Les paramètres du modèle sont identifiés par une méthode robuste et rapide. Le modèle est ensuite développé à la fois dans un code commercial de calcul par éléments finis et dans un outil de calcul basé sur une méthode de réduction de modèles. Enfin, une étude du comportement en fatigue est réalisée à travers une campagne d’essais originaux servant de point de départ à la proposition d’une loi d’endommagement continu. / In association with Airbus Helicopters, the aim of the project is to develop a model to pre-size elastomer-metal laminated devices whose role is critical in terms of design and safety for helicopters rotor architectures. To do so, the first part of this thesis consisted in characterizing the elasto-dissipatice behavior of the studied material (a carbon black filled butadiene rubber) thanks to static and dynamic tests, with several kind of loading (uni-axial and bi-axial) and over a wide range of frequences, amplitudes and temperatures. From these observations, a phenomenological hyper-viscoelastic model is proposed. Based on a generalized Maxwell model, it is able to describe the phenomena over the loading range of concern. A particular focus is made to take in account the Payne effect thanks to an original approach. The model parameters are identified with a fast and robust method. The model is then implemented in a commercial finite element code and in a tool based on a model reduction method. Last, a study of the behaviour in fatigue is performed with an original characterization campaign from which a continuous damage law is proposed.

A rapid digestion procedure for further determination of inorganic elements in carbon black-containing elastomers has been developed using sample combustion in closed quartz vessels with oxygen pressure. Microwave radiation was used for the ignition step. Samples containing high levels of carbon black (up to 30%) were digested using the proposed procedure: nitrile-butadiene rubber (NBR) and ethylenepropylene-diene monomer (EPDM). A quartz device was used simultaneously as a sample holder and for the protection of vessel cap. Sample was pressed as pellet and placed together a small piece of low-ash content paper in the holder. Ammonium nitrate solution (50 ml of 50% m/v) was added to the paper as aid for ignition. The influence of the absorption solution (nitric acid or water) and the necessity of an additional reflux step were evaluated. Determination of Al, Fe, Mn, Sr and Zn was performed by inductively coupled plasma optical emission spectrometry. A reference method (ASTM D 4004-064) based on conventional dry ashing followed by flame atomic absorption spectrometry determination was used for results comparison (Mn and Zn). Results were also compared to those obtained by using wet acid digestion in closed systems. As no certified reference elastomers were available analyte spikes were made for NBR and EPDM digests. Concentrated and diluted (4 mol l-1) nitric acid, with 5 min for reflux step after the combustion process, gave better recoveries for all analytes (from 97 to 101%). For Al and Mn recoveries were bellow 90% for both open and closed vessels using HNO3 and H2SO4 mixture. For dry ashing quantitative recoveries were found only for Zn (for Al recovery was 14%). Residual carbon content was bellow 0.5% for the proposed procedure. With the proposed procedure further determination of Al, Mn, Sr and Zn is feasible with only the combustion step but for Fe a reflux with diluted HNO3 was necessary. Then, using the proposed procedure complete sample digestion is obtained is less time than other procedures and no need of concentrated acids was considered necessary. / Neste trabalho foi proposto um procedimento para a decomposição de elastômeros (Etileno-propileno-dieno monômero e borracha do tipo nitrílica) em sistema fechado por combustão iniciada por microondas. Após a decomposição das amostras foram determinados Al, Fe, Mn, Sr e Zn por espectrometria de emissão óptica com plasma indutivamente acoplado (ICP OES). Para Mn e Zn, a metodologia proposta foi comparada com a metodologia oficial ASTM D 4004-064 para a decomposição de elastômeros e posterior determinação por espectrometria de absorção atômica com chama (F AAS). Os resultados obtidos foram concordantes com a metodologia oficial para a determinação de Mn e Zn. Adicionalmente, ensaios de recuperação foram empregados para Al, Fe, Mn, Sr e Zn para avaliação do método proposto. Além disso, foram estudados dois tipos de solução absorvedora (H2O e HNO3 diluído e concentrado), além da variação do emprego do tempo de aquecimento com microondas (1 min ou 5 min). Entretanto, para se obter recuperações quantitativas para todos os elementos, em ambas as amostras, é necessário que se utilize HNO3 4 molar ou concentrado como solução absorvedora e uma etapa adicional de refluxo ao procedimento de combustão. Cabe destacar que outras condições podem ser utilizadas, como por exemplo, HNO3 concentrado sem a etapa adicional de refluxo, entretanto nestas condições as recuperações podem ser quantitativas para todos os elementos com exceção de ferro. Cabe salientar que, o procedimento proposto foi comparado com o procedimento da norma ASTM, onde os valores encontrados para Zn e Mn nas amostras foram concordantes pelas duas técnicas. O teor de carbono residual é baixo e comparável aos do sistema de decomposição por via seca em mufla. Desta forma é possível propor este procedimento para a decomposição de elastômeros do tipo EPDM e NBR, sendo adequado para a posterior determinação de Al, Fe, Mn, Sr e Zn.

Made available in DSpace on 2014-06-11T19:25:20Z (GMT). No. of bitstreams: 0 Previous issue date: 2005-08-22Bitstream added on 2014-06-13T19:11:58Z : No. of bitstreams: 1 franca_dcc_me_araca.pdf: 2609587 bytes, checksum: 8a7904cdb64c406b06f726af6ac60fbc (MD5) / Universidade Estadual Paulista (UNESP) / No presente estudo foram utilizados 60 ratos submetidos a implantes subcutâneos de quatro elastômeros de silicone, sendo três usados em prótese bucomaxilofacial, LIM 6050, MDX 4-4210 e Silastic 732 RTV industrial e um indicado para cirurgia plástica, o Silimed. O objetivo do estudo foi avaliar os materiais em relação à compatibilidade biológica tecidual, nos tempos pós-operatórios de sete, quinze e trinta dias, quando os animais foram sacrificados e as peças processadas e coradas pela hematoxilina e eosina para análise qualitativa e quantitativa dos espécimes. Pelo estudo histomorfométrico, oito áreas de 60,11 mm2 foram analisadas, contando-se as células mesenquimais, inflamatórias mononucleares, eosinófilos e as células gigantes do tipo corpo estranho. O experimento foi desenvolvido em dois capítulos, estudando-se separadamente os silicones de uso em prótese e o Silimed. No primeiro capítulo, a análise da biocompatibilidade dos implantes subcutâneos dos elastômeros de silicone LIM 6050, MDX 4-4210 e Silastic 732 RTV industrial, observou-se biocompatibilidade aceitável em todos eles, considerando-se o fato de que sua indicação protética dependeria em especial das características físicas próprias de cada material, pela mínima reação tecidual observada, além de que em sua forma sólida é fácil a adaptação aos tecidos. No segundo capítulo, o estudo se baseou na análise das reações referentes ao implante de silicone utilizado em cirurgia plástica (Silimed), constatando-se a presença de processo inflamatório ligeiramente maior no silicone gel em relação aos outros grupos, porém com níveis aceitáveis de biocompatibilidade, confirmada pela rara presença de células gigantes do tipo corpo estranho. Todos os dados foram submetidos à análise de variância e teste de Tukey, demonstrando que todos os materiais implantados iniciaram uma resposta... / In the present study 60 rats were submitted to subcutaneous implant of four elastomers of silicon, being three of use in bucomaxillofacial prosthesis, LIM 6050, MDX 4-4210 and Silastic 732 RTV industrial and a suitable one for plastic surgery, Silimed. The objective of the study was to evaluate the materials in relation to the tissue biological compatibility, in the postoperative times of seven, fifteen and thirty days, when the animals were sacrificed and the processed pieces and stained for the hematoxilin and eosin for qualitative and quantitative analysis of the specimens. For the histomorphometric study, eight areas of 60,11 mm2 were analyzed, being counted the mesenchimal cells, inflammatory cells, eosinophile and giant cells. The experiment was developed in two chapters, being studied the use silicons separately in prosthesis and Silimed. In the first chapter, the analysis of the biocompatibility of the subcutaneous implant of the elastomers of silicon LIM 6050, MDX 4-4210 and Silastic 732 RTV industrial, acceptable biocompatibility was observed in all of them, being considered the fact that your prosthetic indication would especially depend on the own physical characteristics of each material, for the low tissue reaction observed, in addition in your solid form it is easy the adaptation to the tissues. In the second chapter, the study based on the analysis of the referring reactions to the it implants of silicon used in plastic surgery (silimed), being verified the presence of inflammatory process lightly larger in relation to the other groups, however with acceptable levels of biocompatibility confirmed by the rare presence of giant cells of the type strange body. All the data were submitted to the variance analysis and test of Tukey, demonstrating that all the implanted materials began an acceptable tissue inflammatory reaction, with tissue reactions of light intensity the moderate... (Complete abstract, click electronic address below)

Submitted by GIOVANNI BARRERA TORRES null (gbarrerat01@gmail.com) on 2017-08-04T04:24:40Z No. of bitstreams: 1 TESE VERSÃO FINAL Giovanni Barrera Torres.pdf: 6197644 bytes, checksum: d321626a0e947c39627bbfe43b7aaf87 (MD5) / Approved for entry into archive by LUIZA DE MENEZES ROMANETTO (luizamenezes@reitoria.unesp.br) on 2017-08-04T19:37:47Z (GMT) No. of bitstreams: 1 torres_gb_dr_prud.pdf: 6197644 bytes, checksum: d321626a0e947c39627bbfe43b7aaf87 (MD5) / Made available in DSpace on 2017-08-04T19:37:47Z (GMT). No. of bitstreams: 1 torres_gb_dr_prud.pdf: 6197644 bytes, checksum: d321626a0e947c39627bbfe43b7aaf87 (MD5) Previous issue date: 2017-06-21 / Asociación Universitaria Iberoamericana de Postgrado (AIUP) / A presente pesquisa foi projetada para promover o desenvolvimento de compósitos poliméricos a partir da mistura de polietileno de baixa densidade (PEBD) com borracha natural (BN) reforçada com a cinza, resíduo da queima do bagaço, a cinza da cana de açúcar (CBC). Uma das propostas desta pesquisa foi direcionar uma aplicação ao resíduo, que é um material abundante e descartado, gerado no processo usual das usinas. A borracha natural empregada foi obtida a partir do látex de seringueira de Hevea Brasiliensis, Clone RRIM 600 muito cultivado no Brasil. A fim de se estudar separadamente a interação entre a CBC junto a BN e os agentes de vulcanização. Foi estudada numa primeira etapa: a mistura de borracha natural com a cinza de bagaço da cana até desenvolver uma mistura chamada de master, com boas propriedades de tensão e deformação. Foram produzidos compósitos elastoméricos aplicando agente silano como sistema de acoplamento. Numa segunda etapa o master compatibilizado foi misturado ao PEBD sem o uso de agentes de vulcanização; a finalidade destes compósitos foi de estudar a interação dos constituintes visando obter um compósito com o mínimo de agentes químicos e funcional para a indústria. Numa última etapa foram desenvolvidas blendas e compósitos termoplásticos vulcanizáveis (TPV); nesta etapa foram aplicados os agentes de vulcanização empregados na primeira etapa da pesquisa. As amostras foram estudadas por meio das técnicas de análises estruturais (FT-IR); físico-mecânicas (tensão e deformação; dinâmicas e mecânicas, DMA); térmicas (DSC e TG); dureza (Shore A). Foram obtidos resultados sobressalientes em comparação com as amostras sem agentes de vulcanização nas amostras com 50 % de master e 50 % de PEBD na resposta de elongação e tensão; a dureza acima do Shore A 85 obtida, foi produto da porcentagem da fase de PEBD presente nas amostras; nas análises térmicas foi possível observar degradação acima dos 160 oC resultando uma boa característica para aplicações industriais. Com os resultados obtidos tornou-se possível direcionar tanto a CBC como os compósitos para aplicações tecnológicas a fim de serem utilizados na fabricação de cabos de ferramentas, amortecedores, produtos para o lar, entre outros. / The present research was aimed to promote the development of polymeric composites from the mixture of low density polyethylene (LDPE) with natural rubber reinforced with ash, residue of the burning of sugarcane bagasse (SCB). One of the proposals of this research was to direct an application to the residue, which is an abundant and discarded material, generated in the usual process of the plants. The natural rubber used was obtained from rubber latex clone of Hevea Brasiliensis, Clone RRIM 600 widely cultivated in Brazil. In order to study separately the interaction between SCB with NR and vulcanization agents. It was developed in the first stage: the mixing of natural rubber with the sugarcane bagasse ash to develop a mixture called master, with good tensile and deformation properties. Elastomeric composites were produced by applying silane as a coupling agent. In a second stage the compatibilized master was mixed to the LDPE without the use of vulcanization agents; the purpose of these composites was to study the interaction of the constituents in order to obtain a composite with the minimum of chemical and functional agents for the industry. In the latter stage vulcanizable thermoplastic blends and thermoplastic composites were developed; In this stage the vulcanization agents used in the first stage of the research were applied. The samples were studied using structural analysis techniques (FT-IR); Physical-mechanical (tension and deformation, dynamic and mechanical, DMA); (DSC and TG); Hardness (Shore A). Sparing results were obtained in comparison with the samples without vulcanization agents in samples with 50 % of master and 50 % of LDPE in the strain and stress response; the hardness above Shore A 85, obtained was the product of the percentage of the LDPE phase present in the samples; In the thermal analyzes it was possible to observe degradation above 160 oC resulting in a good characteristic for industrial applications. With the results obtained, it became possible to target both SCB and composites for technological applications in order to be used in the manufacture of tool cables, shock absorbers, household products, among others. / AIUP: A0 185864

Made available in DSpace on 2014-12-17T14:58:22Z (GMT). No. of bitstreams: 1 ValdicleideSM_DISSERT.PDF: 4448803 bytes, checksum: fa349b3064555b231f574c1ef787342f (MD5) Previous issue date: 2013-02-04 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior / The biodiesel use has become important due to its renewable character and to reduce environmental impacts during the fuel burning. Theses benefit will be valid if the fuel shows good performance, chemistry stability and compatibility with engines. Biodiesel is a good fuel to diesel engines due to its lubricity. Then, the aimed of this study was to verify the physicalchemistry properties of biodiesel and their correlations with possible elastomers damage after biodiesel be used as fuel in an injection system. The methodology was divided in three steps: biodiesels synthesis by transesterification of three vegetable oil (soybean, palm and sunflower) and their physical-chemistry characterization (viscosity, oxidative stability, flash point, acidity, humidity and density); pressurized test of compatibility between elastomers (NBR and VITON) and biodiesel, and the last one, analyze of biodiesels lubricity by tribological test ball-plan( HFRR). Also, the effect of mixture of biodiesel and diesel in different concentrations was evaluated. The results showed that VITON showed better compatibility with all biodiesel blends in relation to NBR, however when VITON had contact with sunflower biodiesel and its blends the swelling degree suffer higher influences due to biodiesel humidity. For others biodiesels and theirs blends, this elastomer kept its mechanical properties constant. The better tribological performance was observed for blends with high biodiesel concentration, lower friction coefficient was obtained when palm biodiesel was used. The main mechanisms observed during the HFRR tests were abrasive and oxidative wear / O uso do biodiesel tem ganhado for?a por seu car?ter renov?vel e por diminuir o impacto ambiental causado pela queima dos combust?veis f?sseis. Estes benef?cios valer?o a pena se o combust?vel apresentar bom desempenho, estabilidade qu?mica favor?vel e que n?o comprometa a integridade do sistema no qual venha a atuar. A sua aplica??o nos motores diesel tem sido indicada por apresentar maior lubricidade, que ? desej?vel para este sistema em raz?o do funcionamento da bomba. Desse modo, este trabalho teve como objetivo verificar o papel das propriedades f?sico-qu?micas do biodiesel e correlaciona-las com os poss?veis danos causados com o seu uso aos elast?meros aplicados no sistema de inje??o dos motores diesel. A metodologia foi dividida em tr?s etapas: s?ntese dos biodieseis por metan?lise a partir de tr?s oleaginosas (soja, dend? e girassol) e caracteriza??o f?sico-qu?mica (viscosidade, estabilidade oxidativa, ponto de fulgor, acidez, umidade e densidade); ensaio pressurizado de compatibilidade dos biodieseis com os elast?meros (NBR e VITON) e por fim, an?lise da lubricidade dos biodieseis atrav?s de ensaio tribol?gico esfera-plano( HFRR). Tamb?m foi avaliado o efeito da mistura do biodiesel ao diesel em diferentes propor??es, que limitam a deteriora??o dos materiais em contato com este combust?vel. O VITON apresentou maior compatibilidade com todos os combust?veis em rela??o ao NBR, no entanto para o contato com o biodiesel de Girassol e suas blendas o grau de inchamento sofreu maiores influ?ncias devido a este biodiesel apresentar maior umidade. Para as demais blendas e combust?veis analisados, este elast?mero manteve suas propriedades mec?nicas praticamente constantes. Em rela??o aos combust?veis estudados e suas blendas, os melhores desempenhos tribol?gicos foram observados para as maiores concentra??es dos biodieseis, com coeficientes de atrito menores para o biodiesel de dend?. Os principais mecanismos de desgaste observados foram abrasivo e oxidativo

Nous avons développé une stratégie de synthèse basée sur la cycloaddition 1,3‐dipolaire catalysée par le Cu(I) pour la préparation de LCPs et LCEs. Nous avons considéré deux approches. La première consiste en l’élaboration des monomères (protomésogènes) portant des fonctionnalités alcynes terminaux et des molécules portant des groupements azurés suivi de leur réaction selon un procédé en une seule étape. Dans la seconde approche, la formation du "protomésogène" se fait in situ lors de la réaction de cycloaddition (polymerisation) à partir de blocs complémentaires portant des fonctionnalités alcynes et azurés. Tous les composés synthétisés ont été caractérisés par des techniques classiques d'analyses chimiques ou physiques (élastomères). Dans tous les cas, les analyses thermiques (ATG et DSC) ont été menées afin de déterminer l’existence de mésophases et la stabilité des produits, et le cas échéant, les propriétés mésomorphes ont été analysées par POM et SAXS. / In this work we have developed a new strategy based on the Cu(I)‐catalyzed 1,3‐dipolar cycloaddition between azides and alkynes for the preparation of a variety of LCPs and LCEs. Two approaches are presented. The first one consists in clicking together appropriate alkyne‐difunctionalized potential mesogens with azide‐difunctionalized spacers (polymers) and crosslinker (elastomers) in a one‐pot procedure. In an alternative approach, the potential mesogens are formed in situ during the polymerization procedure by cliking prefunctionalized building blocks bearing alkyne and azide functions. All of the samples were chemically or physically (elastomers) characterized by typical analysis. Their thermal behavior was investigated by using techniques such as ATG and DSC and where necessary (mesomorphic materials) by using POM and SAXS.

Orientadores: Mario Alexandre Coelho Sinhoreti, Carlos Jose Soares / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Odontologia de Piracicaba / Made available in DSpace on 2018-08-11T16:18:48Z (GMT). No. of bitstreams: 1 Carlo_HugoLemes_D.pdf: 4484901 bytes, checksum: b6c246e6e05cdf7633210adfa7b73c84 (MD5) Previous issue date: 2008 / Resumo: Baseado no entendimento incompleto de como o conteúdo de partículas de carga influencia nas propriedades mecânicas dos materiais de moldagem este estudo avaliou quantitativa e qualitativamente o conteúdo de partículas de carga inorgânicas presente em cinco marcas comerciais de alginatos (Jeltrate; Jeltrate Plus, Jeltrate Chromatic Ortho, Hydrogum e Ezact Krom) e nove marcas comerciais de siliconas de adição e/ou condensação nas consistências massa e/ou fluida (Clonage, Elite HD+ Light Body, Express Light Body, Flexitime, Optosil P Confort/Xantopren VL Plus, Oranwash L, Reprosil A+, Silon 2 APS e Virtual Extra Light Body). Foram realizados testes para determinar recuperação elástica e deformação sob compressão dos alginatos e dos elastômeros e estabelecer, dessa forma, uma correlação entre os resultados para partículas de carga e os testes mecânicos. O conteúdo volumétrico das partículas de carga foi determinado pesando-se as amostras submersas em água antes e após a queima das mesmas durante 3h a 450°C (alginatos) e a 600°C (siliconas). Quantidades determinadas de materiais não polimerizados foram lavadas em acetona e clorofórmio e recobertas com ouro para avaliação da morfologia e tamanho das partículas em M.E.V. A composição foi determinada por EDX. A recuperação elástica e a deformação sob compressão foram determinadas de acordo as especificações ? 1563 (alginatos) e 4823 (elastômeros) da ISO. O alginatos Jeltrate e Jeltrate Plus apresentaram os maiores valores médios para quantidade volumétrica de partículas de carga (%) enquanto o material Hydrogum apresentou os menores valores. A silicone de adição Flexitime Easy Putty apresentou os maiores valores de quantidade volumétrica de partículas, enquanto que a silicone de condensação Xantopren VL Plus apresentou os menores. As partículas de carga dos alginatos apresentaram-se, de forma geral, como objetos esféricos e com perfurações. O material Hydrogum apresentou forma de bastões cilíndricos e perfurados. As siliconas apresentaram morfologias variadas ¿ partículas trituradas, esféricas, esferóides, bastões cilíndricos perfurados e bastões misturados a partículas usinadas. O alginato Ezact Krom apresentou os maiores valores médios de tamanho de partícula, enquanto que o alginato Hydrogum as menores. A silicone de condensação Clonage massa apresentou os maiores valores médios de tamanho de partícula, enquanto a silicone de adição Elite HD os menores. A análise da composição das partículas apresentou o silício como o elemento em maior quantidade. Com relação aos resultados de recuperação elástica, o alginato Ezact Krom e as siliconas Reprosil A+ massa e Flexitime fluida apresentaram os maiores valores de recuperação elástica, enquanto o alginato Jeltrate Plus e as siliconas Optosil P Confort e Clonage fluida apresentaram os menores. Os resultados de deformação sob compressão foram maiores para o alginato Jeltrate Plus e para as siliconas Silon 2 APS massa e fluida. Os menores resultados foram apresentados pelo alginato Ezact Krom e as siliconas Reprosil A+ massa e Xantopren VL Plus. Todos os materiais estão em conformidade com a norma ISO ?1563, mas nem todos estão em relação à norma ?4823 / Abstract: Based on the incomplete understanding on how filler features influence the properties of elastomeric impression materials, the purpose of this study was to determine the inorganic filler fraction and size of five commercially available alginates (Jeltrate; Jeltrate Plus, Jeltrate Chromatic Ortho, Hydrogum e Ezact Krom) and nine addition/condensation silicones using the putty/light consistence (Clonage, Elite HD+ Light Body, Express Light Body, Flexitime, Optosil P Confort/Xantopren VL Plus, Oranwash L, Reprosil A+, Silon 2 APS e Virtual Extra Light Body). A SEM/EDX analysis was done to qualitatively characterize the materials. Soon afterwards elastic recovery and strain in compression of the alginates and some the silicones was carried. The inorganic particles volumetric fractions were accessed by weighing a previously determined mass of each material in water before and after burning samples for 3 hours at 450ºC (alginates) and 600ºC (silicones). Unsettled materials were soaked in acetone and chloroform and sputter-coated with gold for SEM evaluation of fillers¿ morphology and size. The filler composition was determined by EDX. Elastic recovery and strain in compression tests were conducted according to ISO specification number 1563 and 4823. Jeltrate and Jeltrate Plus presented the highest mean values of percentage content of inorganic particles in volume, while Jeltrate Chromatic Ortho presented the lowest values. Flexitime Easy Putty was the silicone with the highest mean value, while Xantopren VL Plus had the lowest value. The alginate fillers presented a circular appearance with helical form and various perforations. Hydrogum fillers looked like cylindrical, perforated sticks. SEM pictures of the silicone inorganic particles showed numerous morphologies ¿ lathe-cut, spherical, spherical-like, sticks, and sticks mixed to lathe-cut powder. Ezact Krom was the alginate with the highest values for diameter size, while Hydrogum had the lowest. Clonage Putty showed the highest values, while Elite HD+ Light Body presented the lowest values. The component in higher concentration in the materials is silicon. The alginate Ezact Krom, and the addition cure silicones Reprosil A+ putty and Flexitime Correct Flow had the highest mean values of elastic recovery, while the alginate Jeltrate Plus and the condensation cured silicones Optosil P Confort and Clonage Putty presented the lowest values. Strain in compression test showed the alginate Jeltrate Plus and the condensation cured silicones Silon 2APS Putty and Fluid as the materials with the highest values. The alginate Ezact Krom and the silicones Reprosil A+ Putty and Xantopren VL Plus had lowest values. All materials are in conformity with the requirements of ISO specification number 1563, but not all materials are in conformity with the requirements of ISO specification number 4823 / Doutorado / Materiais Dentarios / Doutor em Materiais Dentários

L'objectif de ce travail est d'étudier l'influence de l'état de dispersion de la silice sur les propriétés viscoélastiques et mécaniques des élastomères chargés silice pour l'application pneumatique. En effet, il est montré qu'une grande partie de la résistance au roulement dépend de la dissipation d'énergie de l'élastomère chargé. De plus, les propriétés mécaniques pourraient intervenir dans les propriétés ultimes telles la propagation de fissure en fatigue et l'usure : l'étude de ces différentes propriétés est donc primordiale. La première partie s'attèle donc à l'identification des leviers pouvant moduler la dispersion de la silice dans les élastomères. La dispersion pouvant être vue comme la compétition entre les forces de cohésion des charges et les forces appliquées au système pour les rompre, ces paramètres ont été étudiés de manière systématique. Enfin, l'influence des interactions silice-matrice est abordée (modification de l'état de surface de la silice, nature de l'élastomère) : le nombre d'interactions silice-élastomère par chaîne de polymère pourrait intervenir dans les mécanismes de dispersion. Dans la seconde partie, l'influence de ces différents états de dispersion sur les propriétés viscoélastiques et mécaniques est discutée. L'amélioration de la dispersion à iso-formulation permet de diminuer le module élastique linéaire dans le domaine linéaire et entraîne une augmentation des modules aux grandes déformations en traction. Concernant l'étude des propriétés ultimes, notre dispositif expérimental n'a pas permis de mettre en évidence, sur les formulations testées, d'influence de la dispersion sur la dynamique de propagation de fissure en fatigue. En revanche, l'amélioration de la dispersion entraîne une amélioration de la résistance à l'usure et ce malgré une diminution de la dureté / Filled elastomers are used in tread tires. It has been demonstrated that most of rolling resistance of tires is due to filled elastomer energy dissipation. In that way, understanding viscoelastic properties of these materials is a key point. Then, filled elastomer behavior at high deformations may be involved in ultimate properties of tire application such as fatigue crack propagation and wear. The aim of this work is to study the impact of silica dispersion on viscoelastic and mechanical properties of filled elastomers. First, levers impacting silica dispersion are evaluated. Dispersion of fillers can be considered as a competition between fillers cohesion forces and applied forces to the system to break them, these parameters have been studied methodically. Finally, the impact of silica-matrix interactions is studied, changing silica surface treatments or elastomer natures. The quantity of interactions possible per polymer chain between the silica and the elastomer may play a role in silica dispersion. Secondly, the impact of silica dispersion on viscoelastic and mechanical properties is discussed. It is shown than increasing silica dispersion leads to a decrease of linear elastic modulus and an increase of reinforcement in tensile at high deformations. Finally, regarding ultimate properties, our experimental device on the selected formulations has not shown any impact of silica dispersion on fatigue crack propagation. Nevertheless, we observe a better wear resistance with increasing dispersion, despite the lower materials hardness

The first magnetization loop and the first stress–strain cycle of magnetoactive elastomers (MAEs) in a magnetic field differ considerably from the following loops and cycles, possibly due to the internal restructuring of the magnetic filler particles and the matrix polymer chains. In the present study, the irreversible magnetization processes during the first magnetization of MAEs with different filler compositions and tensile moduli of the matrix are studied by first-order reversal curve (FORC) measurements. For MAEs with mixed magnetic NdFeB/Fe fillers the FORC distributions and magnetization distributions of the first major loop reveal a complex irreversible magnetization behavior at interaction fields Hu < −50 kA m−1 due to the magnetostatic coupling between the magnetically hard NdFeB and the magnetically soft Fe particles. This coupling is enhanced either if the interparticle distance is reduced by particle motion and restructuring or by an increase in the particle densities. If the stiffness of the matrix is increased, the structuring and thus the interparticle interactions are suppressed and the magnetization reversal is dominated by domain processes in the NdFeB particles at high coercive fields of Hc > 600 kA m−1.