The mechanically compressive flow stress sensitivities of various polymers are investigated at high strain rates above 103 s-1. Temperatures near the glass transition temperature are investigated and the polymer stress-strain responses have been studied from ambient temperature to 100°C. Previous work has reported peaks in flow stress as a function of strain rate [Al-Maliky/Parry 1994, Al-Maliky 1997]. The analyses showed rapid increases of flow stress followed by a sudden drop at elevated strain rates, which is unlike the well known linear relationship documented at the low strain rates. The mechanics and stipulation of what bring about this phenomenon, or the types of polymers influenced are still unclear. Two fluoropolymers, polytetrafluoroethylene (PTFE) and polychlorotrifluoroethylene (PCTFE), and two vinyl polymers, polyvinylchloride (PVC) and polymethylmethacrylate (PMMA), are chosen for this study. PTFE, PCTFE and PVC are semi-crystalline polymers with different percentage of crystallinity contents, whereas PMMA is an amorphous polymer. The glass transition temperature, Tg, is the characteristic of the amorphous content in polymers, which has been suggested to influence the flow stress peaks [Swallowe/Lee 2003]. Tg of the semi-crystalline polymers are within the test temperature range. High strain rate compression tests have been carried out using the split Hopkinson pressure bar (SHPB). This is a well-established method for determining the stress, strain, and strain rate of materials. The strain rate range of interest is 103 s-1 to 105 s-1 where the strain rate sensitivity has previously been identified [Al-Maliky/Parry 1994, Al-Maliky 1997, Walley/Field 1994]. Two thermal analyses techniques are used to quantify the dependency of the viscoelastic behaviour in relation to time and temperature. Differential scanning calorimetry (DSC) measures the enthalpy of the polymers to show how the materials are affected by heat, and Dynamic mechanical analysis (DMA) is used to characterise the time-temperature dependence of the elastic storage and loss moduli of the polymers A total of 42 PCTFE, 44 PTFE, 45 PVC and 55 PMMA specimens were tested using the SHPB system, with the strain rate varying between 1600 s-1 and 6100 s-1. Initial results for PMMA have been reported [Forrester/Swallowe 2009]. The rate of strain where specimens begin to show crazing is identified. The value of yield stress increases with the increase of strain rate and the decrease in temperature. Large strain hardening can be seen in all three semi-crystalline polymers at higher strain rates. The temperature rise during plastic flow of compression is calculated by the stress-strain rate curves. In this thesis, the emphasis is on the relation of yield/flow stress to strain rate as the polymers deform under high strain compression. The mechanism behind the cause of high strain rate deformation responses for amorphous to semi-crystalline polymers in ductile state is discussed, with a view to understanding the sensitivity of yield/flow stresses as a function of strain rate. Also, the modelling of the polymers has been carried in order to alleviate doubts about the validity of the real experimental results that may arise due to the nature of the decomposition of the polymers. It has been shown that the strain energy density pulses through the sample in response to the compression wave in various circular intensities.

Este estudo teve como objetivo investigar uma provável função mecânica da fíbula no complexo tíbio-fibular de ratos. Para tanto, os complexos tíbio-fibulares de 20 ratos da raça Norvegicus Albinus, variedade Wistar, foram submetidos a esforços de compressão axial e flexão em três pontos. Os animais eram adultos jovens, todos machos com peso corporal médio de 350 g. Foram utilizados 20 pares de tíbias para cada ensaio, sendo que, de um dos lados de cada par, a fíbula foi mantida e, do outro lado, removida. Foi utilizado uma máquina universal de ensaio para a realização de ambos os ensaios mecânicos. Os valores foram obtidos na forma de carga versus deformação (ensaio de compressão), e carga versus deflexão (ensaio de flexão). Os seguintes parâmetros foram analisados: carga máxima, deformação máxima e rigidez. Da análise dos resultados foi concluído que a fíbula, no rato, não aumenta a resistência do complexo tíbio-fibular. Assim, a presença da fíbula parece estar mais relacionada com função de inserções musculares do que fortalecimento tíbio-fibular. / This study was conducted to investigate the contribution of the fibula to the mechanical resistance of the tibiofibular complex in the rat (both banes are fused distally). Twenty adult wistar rats were used as donor animals of twenty paired tibias. For each pair of bones in one side the fibula was excited and in the other side it was maintained. In a test machine the mechanical tests were done in three flexion and axial compression. The results were plotted either in load x deformation or load x deflection graphs the following parameters were analysed: ultimate load, ultimate deformation and rigidity. It was concluded that the fibula does not increase the mechanical strength of the tibiofibular complex, but it may play a role as an anchorage for the muscles that act on the foot.

Neste trabalho foi realizada a caracterização de um poliuretano derivado de óleo vegetal para ser utilizado na confecção de dispositivos de assistência ventricular, DAVs. Esses dispositivos são muito importantes na área cardiovascular, pois, possuem a função de suprir a falha dos ventrículos direitos ou esquerdo do coração durante o bombeamento em casos de transplante. Para que esse material seja apto para ser utilizado, precisa-se ter propriedades mecânicas, térmicas e biológicas compatíveis com as necessidades médicas da área cardiovascular. Neste estudo foram utilizadas as técnicas de ensaio mecânico de tração e compressão, as técnicas termoanalíticas DMA, TGA, DSC, bem como espectroscopia de absorção na região do infravermelho. Para os ensaios biológicos foram feitos os teste de tempo de coagulação sanguínea (método Lee White) e o estudo de crescimento celular acompanhado por análise de microscopia eletrônica de varredura (MEV). Os resultados obtidos nos ensaios mecânicos mostraram que o poliuretano possui propriedades que não comprometem sua utilização na confecção dos DAVs. Com relação às análises térmicas, os resultados obtidos pelas curvas DMA mostraram que o poliuretano aumenta seu grau de cura e sua rigidez com o tratamento térmico. As curvas TG e as TG/DSC-FTIR mostram que o poliuretano é termicamente estável e não libera nenhum tipo de substância prejudicial ao ser humano até a temperatura de 200°C, viabilizando uma condição de serviço satisfatória a temperatura corpórea entre 36ºC e 40°C. Os testes biológicos demonstraram que o poliuretano possui potencial para ser utilizado em dispositivos médicos que entram em contato com o sangue, tornando-se necessários estudos para a sua total comprovação de ser um material hemocompatível. / In this study the characterization of a polyurethane derived from vegetable oil was studied for the use in the production of ventricular assistance devices, VADs. These devices are very important in the cardiovascular area, therefore they have the function of supplying the failure of the right or left ventricles of the heart while pumping in transplants. For this material to be used in this application, it must have mechanical, thermal and biological properties compatible with the medical require of the cardiovascular area. In this study was to used the techniques of mechanical tensile and compressive, the thermoanalytical techniques such as DMA, TGA, DSC and absorption spectroscopy in the infrared region. The biological analysis were the test of blood coagulation time (Lee White method) and the study of cellular growth measured by scanning electron microscopy (SEM). The results obtained in the mechanical tests showed that the polyurethane has properties that do not compromise their use in the production of VADs. In relation the thermal analysis of the results obtained by DMA, the curves showed that the polyurethane increases its cure and rigity degrees with thermal treatment. The TG and TG/DSC-FTIR curves showed that the polyurethane is thermally stable does not release any prejudicial substances to the human body until the temperature of 200°C, enabling a satisfactory service condition to body temperature between 36 and 40°C. The biological tests showed that the polyurethane has the potential to be used in medical devices that come into contact with blood, however it\'s needing more studies for its full proof of being a hemocompatible material.

La détermination des conditions de chargements limites qui produisent une localisation du matériau est toujours un enjeu important, notamment lorsqu'il s'agit d'optimiser les dimensions d'outillage lors d'opérations durant lesquelles le matériau est fortement sollicité. Différents travaux récents ont montré que l'hétérogénéité structurale intrinsèque à tout matériau métallique joue un rôle important dans les différents stades de déformation. Le rôle des hétérogénéités sur la localisation n'est cependant pas abordé. L'objectif de cette thèse est donc de déterminer si l'hétérogénéité structurale des matériaux a un impact sur la localisation des matériaux ductiles. Une action corollaire est alors de valider le recours à des modèles qui intègre cette hétérogénéité pour obtenir des meilleurs résultats.Cette étude comprend deux volets. Le premier volet expérimental a pour objectif de constituer un référentiel expérimental qui met en évidence l'impact du facteur hétérogénéité sur la localisation. Différentes éprouvettes de titane ont été préparées de façon à obtenir différents degrés d'hétérogénéités. Deux paramètres ont été utilisés à cette fin : l'épaisseur et la structure cristalline. Le titane permet en effet de disposer de matériaux à structure hexagonale et cubique centrée qui présentent des possibilités d'accommodation plastique très différentes. Des essais de traction et d'expansion ont ainsi été pratiqués sur des éprouvettes de titane de tôle fine et épaisse dans les structures α et β du titane de nuance T40. Trois tôles différentes : Tiα(tôle fine); Tiα(tôle épaisse) et Tiα+β(tôle épaisse) ont été utilisées lors des essais. Pour obtenir les tôles Tiα+β un traitement thermique a été optimisé et l’analyse des tôles a été effectuée à l’aide de plusieurs techniques comme le MEB, les rayons X et l'ATD. Un second volet numérique s'est appuyé sur deux modèles pour réaliser la simulation des essais expérimentaux. Un premier modèle de type phénoménologique "classique", sans facteur d'hétérogénéité a tout d'abord été utilisé pour simuler le comportement idéal d'un matériau homogène. Dans un second temps, le recours à un modèle qui intègre une dimension physique, l'hétérogénéité, a montré que cette dernière a une incidence notable et permet d'améliorer la prédiction du phénomène de localisation. / The determination of limit loading conditions producing the localization in the material is always an important subject, notably as it is about the optimization of tool dimension during operations during which material is strongly solicited. Different recent works have shown that intrinsic structural heterogeneity inside any metallic material plays an important role in the different stages of deformation. However, the role of heterogeneities in localization is not addressed.The objective of this PhD thesis is therefore to determine if the structural heterogeneity of materials has an impact on the localization of ductile materials. A corollary action is then to validate the use of models which integrate this heterogeneity for best results.This study has two parts.The first experimental part has for objective to constitute an experimental base which highlights the impact of the heterogeneity factor on localization. Different titanium specimens were prepared so as to obtain different degrees of heterogeneities.Two parameters were used for this purpose: thickness and crystal structure. Titanium makes it possible to have materials with hexagonal structure and cubic centered that present possibilities of very different plastic accommodation.Tensile and equi-axial tests have thus been carried out on titanium specimens for thin and thick metal sheet in the structures α and β for T40 grade Titanium.Three different sheets Tiα(thin); Tiα(thick) et Tiα+β(thick) were used during the tests. To obtain the sheets Tiα+β, a heat treatment has been optimized and sheets analysis was done using several techniques such as SEM, X Rays and ATD. A second numerical part was based on two models to realize numerical simulation of the experimental tests. A first classical phenomenological model without heterogeneity factor was firstly used to simulate the ideal behavior of a homogeneous material. In a second time, the use of a model that incorporates a physical dimension that is to say the heterogeneity, has shown that this latter has a significant impact and makes it possible to improve the prediction of localization phenomenon.

Following the continually increasing demand for high-density interconnection and multilayer packaging for chips, solder bump size has decreased significantly over the years, this has led to some challenges in the reliability of interconnects. This thesis presents research into the resulting effects of miniaturization on the interconnection with Sn-solder, especially focusing on the full intermetallics (IMCs) micro-joints which appear in the 3D IC stacking packaging. Thereby, systematic studies have been conducted to study the microstructural evolution and reliability issues of Cu-Sn and Cu-Sn-Ni IMCs micro-joints. (1) Phenomenon of IMCs planar growth: The planar IMCs interlayer was asymmetric and composed of (Cu,Ni)6Sn5 mainly in Ni/Sn (2.5~5 μm)/Cu interconnect. Meanwhile, it was symmetric two-layer structure in Cu/Sn (2.5~5 μm)/Cu interconnect with the Cu3Sn fine grains underneath Cu6Sn5 cobblestone-shape-like grains for each IMCs layer. Besides, it is worth noticing that the appearance of Cu-rich whiskers (the mixture of Cu/Cu2O/SnOx/Cu6Sn5) could potentially lead to short-circuit in the cases of ultra-fine ( < 10 μm pitch) interconnects for the miniaturization of electronics devices. (2) Microstructural evolution process of Cu-Sn IMCs micro-joint: The simultaneous solidification of IMCs interlayer supressed the scalloped growth of Cu6Sn5 grains in Cu/Sn (2.5 μm)/Cu interconnect during the transient liquid phase (TLP) soldering process. The growth factor of Cu3Sn was in the range of 0.29~0.48 in Cu-Cu6Sn5 diffusion couple at 240~290 °C, which was impacted significantly by the type of substrates. And the subsequent homogenization process of Cu3Sn grains was found to be consistent with the description of flux-driven ripening (FDR) theory. Moreover, Kirkendall voids appeared only in the Cu3Sn layer adjacent to Cu-plated substrate, and this porous Cu3Sn micro-joint was mechanically robust during the shear test. (3) Microstructural evolution of Cu-Sn-Ni IMCs micro-joint: There was obvious inter-reaction between the interfacial reactions in Ni/Sn (1.5 μm)/Cu interconnect. The growth factor of (Cu,Ni)3Sn on Cu side was about 0.36 at 240 °C, and the reaction product on Ni side was changed from Ni3Sn4 into (Cu,Ni)6Sn5 with the increase of soldering temperature. In particular, the segregation of Ni atoms occurred along with phase transformation at 290 °C and thereby stabilized the (Cu,Ni)6Sn5 phase for the high Ni content of 20 at.%. (4) Micro-mechanical characteristics of Cu-Sn-Ni IMCs micro-joint: The Young s modulus and hardness of Cu-Sn-Ni IMCs were measured by nanoindentation test, such as 160.6±3.1 GPa/ 7.34±0.14 GPa for (Cu,Ni)6Sn5 and 183.7±4.0 GPa/ 7.38±0.46 GPa for (Cu,Ni)3Sn, respectively. Besides, in-situ nano-compression tests have been conducted on IMCs micro-cantilevers, the fracture strength turns out to be 2.46 GPa. And also, the ultimate tensile stress was calculated to be 2.3±0.7 GPa from in-situ micro-bending tests, which is not sensitive with the microstructural change of IMCs after dwelling at 290 °C.

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / This study aimed to evaluate the bond strength using different test types for bonding evaluation, between a yttrium tetragonal zirconia polycrystals (Y-TZP) ceramic and composite resin, considering two types of Y-TZP surface treatments. Three hundred and sixty Y-TZP blocks, received one of the two surface treatments (N= 180): UT- control (untreated) and SS- silica coating + silanization. Specimen of composite resin were made in different geometries and cemented with resin cement to Y-TZP blocks. The 180 specimens for each surface treatment were divided into six subgroups (n = 30) according to the configuration of bond test: tensile (TBS); microtensile (μTSB); shear (SBS); microshear (μSBS); push-out (PSH) and micropush-out (μPSH). For data analysis were used Weibull parameters, Weibull modulus (m) and resistance characteristic (σ0), to check the dispersion and magnitude of the resistance data, One-way ANOVA test to evaluate the results with normal distribution and Mann-Whitney for those with non-normal distribution. Both the surface treatment s type and specimen size showed a statistically significant difference between groups (p = 0.00). Independent of the type of surface treatment, microtensile test and microshear had higher values than their equivalent macro test. On contrary, push-out presented higher values in the macro tests. The tests that showed higher m and σ0, were: PSH, μPSH, μTBS and μSHS. Silica coating + silanization significantly increased bond strength. Push-out, micropush-out, microshear and microtensile tests have proved to be more appropriate for evaluating bond strength, although the microtensile be inapplicable for Y-TZP untreated, due to the impossibility of obtaining the bar shaped specimens during cutting. / Esse trabalho teve como objetivo avaliar a resistência adesiva, utilizando diferentes geometrias de teste, entre uma cerâmica policristalina tetragonal estabilizada por óxido de ítrio (Y-TZP) e uma resina composta, em função de dois tipos de tratamentos de superfície. Trezentos e sessenta blocos de Y-TZP, receberam dois tratamentos de superfície (N=180): UT- controle (sem tratamento) e SS- silicatização + silanização. Espécimes de resina composta foram confeccionados para as diferentes geometrias e cimentados aos blocos de Y-TZP com cimento resinoso. Para cada tratamento de superfície, os espécimes foram distribuídos em 6 subgrupos (n=30) segundo os ensaios mecânicos: tração (TBS); microtração (μTBS); cisalhamento (SBS); microcisalhamento (μSBS); push-out (PSH) e micropush-out (μPSH). Para análise dos dados, foi utilizados os parâmetros de Weibull, módulo de Weibull (m) e resistência característica (σ0), para verificar a dispersão e magnitude dos dados de resistência, o teste One-way ANOVA para avaliar os resultados com distribuição normal e Mann-Whitney para os com distribuição não-normal. Tanto o tipo de tratamento de superfície quanto a área adesiva foram fatores significantes, apresentando diferença estatística entre os grupos (p=0,00). Independente do tipo de tratamento de superfície, os valores obtidos nos testes de microtração e microcisalhamento foram mais elevados que seus correspondentes macro , porém no push-out foram encontrados valores superiores nos testes macro . Os testes que apresentaram maiores valores de m e σ0, foram PSH, μPSH, μTBS e μSHS. A silicatização + silanização aumentou significativamente a resistência adesiva. Os testes de push-out, micropush-out, microcisalhamento e microtração mostraram-se testes mais satisfatórios para avaliar resistência de união, apesar do teste de microtração ser inviável para Y-TZP não tratada, devido à impossibilidade de obtenção dos espécimes em forma de barra durante o corte.

Neste trabalho foi realizada a caracterização de um poliuretano derivado de óleo vegetal para ser utilizado na confecção de dispositivos de assistência ventricular, DAVs. Esses dispositivos são muito importantes na área cardiovascular, pois, possuem a função de suprir a falha dos ventrículos direitos ou esquerdo do coração durante o bombeamento em casos de transplante. Para que esse material seja apto para ser utilizado, precisa-se ter propriedades mecânicas, térmicas e biológicas compatíveis com as necessidades médicas da área cardiovascular. Neste estudo foram utilizadas as técnicas de ensaio mecânico de tração e compressão, as técnicas termoanalíticas DMA, TGA, DSC, bem como espectroscopia de absorção na região do infravermelho. Para os ensaios biológicos foram feitos os teste de tempo de coagulação sanguínea (método Lee White) e o estudo de crescimento celular acompanhado por análise de microscopia eletrônica de varredura (MEV). Os resultados obtidos nos ensaios mecânicos mostraram que o poliuretano possui propriedades que não comprometem sua utilização na confecção dos DAVs. Com relação às análises térmicas, os resultados obtidos pelas curvas DMA mostraram que o poliuretano aumenta seu grau de cura e sua rigidez com o tratamento térmico. As curvas TG e as TG/DSC-FTIR mostram que o poliuretano é termicamente estável e não libera nenhum tipo de substância prejudicial ao ser humano até a temperatura de 200°C, viabilizando uma condição de serviço satisfatória a temperatura corpórea entre 36ºC e 40°C. Os testes biológicos demonstraram que o poliuretano possui potencial para ser utilizado em dispositivos médicos que entram em contato com o sangue, tornando-se necessários estudos para a sua total comprovação de ser um material hemocompatível. / In this study the characterization of a polyurethane derived from vegetable oil was studied for the use in the production of ventricular assistance devices, VADs. These devices are very important in the cardiovascular area, therefore they have the function of supplying the failure of the right or left ventricles of the heart while pumping in transplants. For this material to be used in this application, it must have mechanical, thermal and biological properties compatible with the medical require of the cardiovascular area. In this study was to used the techniques of mechanical tensile and compressive, the thermoanalytical techniques such as DMA, TGA, DSC and absorption spectroscopy in the infrared region. The biological analysis were the test of blood coagulation time (Lee White method) and the study of cellular growth measured by scanning electron microscopy (SEM). The results obtained in the mechanical tests showed that the polyurethane has properties that do not compromise their use in the production of VADs. In relation the thermal analysis of the results obtained by DMA, the curves showed that the polyurethane increases its cure and rigity degrees with thermal treatment. The TG and TG/DSC-FTIR curves showed that the polyurethane is thermally stable does not release any prejudicial substances to the human body until the temperature of 200°C, enabling a satisfactory service condition to body temperature between 36 and 40°C. The biological tests showed that the polyurethane has the potential to be used in medical devices that come into contact with blood, however it\'s needing more studies for its full proof of being a hemocompatible material.

Este estudo teve como objetivo investigar uma provável função mecânica da fíbula no complexo tíbio-fibular de ratos. Para tanto, os complexos tíbio-fibulares de 20 ratos da raça Norvegicus Albinus, variedade Wistar, foram submetidos a esforços de compressão axial e flexão em três pontos. Os animais eram adultos jovens, todos machos com peso corporal médio de 350 g. Foram utilizados 20 pares de tíbias para cada ensaio, sendo que, de um dos lados de cada par, a fíbula foi mantida e, do outro lado, removida. Foi utilizado uma máquina universal de ensaio para a realização de ambos os ensaios mecânicos. Os valores foram obtidos na forma de carga versus deformação (ensaio de compressão), e carga versus deflexão (ensaio de flexão). Os seguintes parâmetros foram analisados: carga máxima, deformação máxima e rigidez. Da análise dos resultados foi concluído que a fíbula, no rato, não aumenta a resistência do complexo tíbio-fibular. Assim, a presença da fíbula parece estar mais relacionada com função de inserções musculares do que fortalecimento tíbio-fibular. / This study was conducted to investigate the contribution of the fibula to the mechanical resistance of the tibiofibular complex in the rat (both banes are fused distally). Twenty adult wistar rats were used as donor animals of twenty paired tibias. For each pair of bones in one side the fibula was excited and in the other side it was maintained. In a test machine the mechanical tests were done in three flexion and axial compression. The results were plotted either in load x deformation or load x deflection graphs the following parameters were analysed: ultimate load, ultimate deformation and rigidity. It was concluded that the fibula does not increase the mechanical strength of the tibiofibular complex, but it may play a role as an anchorage for the muscles that act on the foot.

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第20700号 / 工博第4397号 / 新制||工||1683(附属図書館) / 京都大学大学院工学研究科機械理工学専攻 / (主査)教授 北村 隆行, 教授 西脇 眞二, 教授 平方 寛之 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

Ce travail de thèse est consacré à l’étude de la dissipation mécanique produite par des alliages à mémoire de forme Cu-Zn-Al lors d'un chargement mécanique cyclique, ainsi qu'à l’influence de la composition chimique sur cette grandeur. Divers alliages ont été élaborés dans ce but, chacun présentant une faible variation de composition par rapport à l’autre. Une procédure expérimentale originale a été mise au point pour mesurer cette dissipation mécanique car elle se traduit par une source de chaleur très inférieure à celles dues à d’autres phénomènes comme la chaleur latente de changement de phase ou le couplage thermoélastique. Les éprouvettes ont ainsi été soumises à divers essais cycliques à température ambiante constante alors qu’une caméra infrarouge filmait les champs thermiques sur leur surface. Ces films thermiques ont ensuite été traités pour en extraire cette dissipation mécanique. Divers niveaux de dissipation correspondant à divers niveaux d’irréversibilité mécanique ont ainsi été mis en évidence. / The study deals with the mechanical dissipation in Cu-Zn-Al shape memory alloys subjected to cyclic mechanical loading, as well as with the influence of the chemical composition on this dissipation. Various alloys were prepared for this purpose, each of them featuring a slight change with respect to the others. An original procedure has been proposed to measure mechanical dissipation because it is very low compared to other heat sources such as latent heat or thermoelastic coupling. The specimens have been subjected to cyclic tests at constant ambient temperature while an infrared camera grabbed the thermal images. These thermal maps have been then processed to extract mechanical dissipation. Various levels have been found, corresponding to various levels of mechanical irreversibilities.