The demands for high density, fine pitch interconnections in electronics systems has seen solder-based approaches for such interconnections miniaturized to the scale of tens of micro meters. At such a small scale, such 'micro joints' may contain only one or a few grains and the resultant mechanical behaviour may not be that for a polycrystalline aggregate, but rather for a single crystal. Since the ~-Sn matrix of SnAgCu solder has a contracted body-centred tetragonal (BCT) structure, such a solder grain is expected to demonstrate a considerably anisotropic behaviour. In such cases the reliability of a Phfree solder is strongly dependent on the local microstructural features, such as the size and orientation of the grains. This thesis presents the investigation of the evolution of microstructure within a joint or at the interface and, the influence of such microstructural features on the meso-scale mechanical behaviour of the Ph-free solder. It includes Evolution of the interface between a molten solder and the Cu substrate To form a joint, the solder alloy is heated and molten, wetting a solid under-bump metallization. After solidification, layers of brittle intermetallic compounds (IMCs) are formed at the interface. In this project, facilities were set up to obtain interfacial reactants at an arbitrary moment of the liquid/solid reaction. Formation and evolution ~ during reflow of SnCu IMCs at the interface between the molten SnAgCu alloy and the Cu UBM was captured and presented for the first time. Formation of phases and IMCs with the body of a liquid SnAgCu solder during solidification The formation behaviour of basic components for a SnAgCu grain (including Sn dendrites, AIDSn and Cu6Sns IMCs) during solidification was investigated. Relationships between the growth behaviour of these components and their internal lattice orientation were studied. The characteristic growth and coupling of AIDSn IMCs and the Sn matrix to form eutectics has been elaborated and presented in this study for - 1- the first time. Based on the results, the forming process of a eutectic SnAgCu grain under the non-equilibrioum solidification condition was illustrated; and major factors that determine the lattice-orientation, size and substructure of the grain were discussed. Meso- and Micro- scale mechanical behaviour of a SnAgCu solder joint To study the size effect on the microstructure, and subsequently, the meso-scale mechanical behaviour, solder joints were manufactured with varying geometries. Shearing tests were performed on these meso-scale joints. The results first demonstrated that the anisotropic characteristics of a SnAgCu grain play an important role in the mechanical behaviour of both a meso-scale solder joint and the adjacent interfacial IMCs. To further investigate the micro-scale deformation and damage mechanisms, micro-mechanical tests were preformed within a SnAgCu grain. Constitutive equations for a SnAgCu grain Based on the experimental results, a crystal model was established to describe the local microstructure-dependent mechanical behaviour. The constitutive equation was implemented by means of the finite element approach, and applied in solder joints of a Flip Chip (FC) package by a multi-scale method. To describe the crystal behaviour at the higher temperature, the model was improved to account for deformations due to vacancy diffusion and thermal expansion. This model was integrated by an implicit approach, and implemented in a full three dimension (3D) finite element (FE) model.

Recombinant synthesis of elastin-mimetic proteins has been employed for several decades, however, long-term biocompatibility and biostability of such proteins was not fully defined. We present virtually crosslinked elastin-mimetic proteins which exhibit exceptional biocompatibility and long-term biostability over a period of at least seven months. This report is the first evidence of a non-chemically or ionically crosslinked system that exhibits long-term in vivo stability. Although, physically crosslinked protein-based materials possess a number of advantages over their chemically crosslinked counterparts, physical crosslinks and the related domains so formed may be deformed or damaged at applied stresses lower than those required to disrupt covalent crosslinks. In this regard, we have synthesized a new class of recombinant elastin-mimetic triblock copolymer capable of both physical and chemical crosslinking. We have demonstrated that chemical crosslinking provides an independent mechanism for control of protein mechanical responses. Specifically, elastic modulus was enhanced and creep strain reduced through the addition of chemical crosslinking sites. A number of reports have described the design of synthetic genes, which encode elastin-like proteins for bacterial expression in Escherichia coli. Although advantages with this expression system exist, significant limitations including the lack of eukaryotic post-translational systems, the tendency to sequester mammalian proteins into inclusion bodies, difficult purification protocols, and endotoxin contamination have been noted. We demonstrate the expression of a recombinant elastin-mimetic protein from P. pastoris. A novel synthetic strategy, monomer library concatamerization, was utilized in designing non-repetitive elastin genes for highly repetitive protein sequences. It is likely that this strategy will be useful for creating large, repetitive genes for a variety of expression systems in order to more closely approach the genetic diversity inherent to native DNA sequences. All told, elastin-based protein polymers are a promising class of material characterized by high degree of biocompatibility, excellent biostability, and a tunable range of mechanical properties from plastic to elastic. A variety of options facilitate the processing of these biopolymers into chemically crosslinked or non-crosslinked gels, films, or nanofibers for any of a number of implant applications including structural components of artificial organs and engineered living tissues, carriers for controlled drug release, or biocompatible surface coatings.

Lower urinary tract disorders are significant prognostic indicators of institutionalisation and lower quality of life in the elderly and their incidence increases with age. Urodynamics, the gold standard in diagnosis, replicates symptoms to assess functionality through controlled filling and voiding of the bladder but its interpretation is subjective and may be inconclusive; often requiring further testing or leading to inappropriate treatment. Normal filling and voiding biomechanics of the bladder relate directly to the structural composition of the bladder wall. Alterations to tissue composition in aging and pathology have significant impacts on biomechanics but are yet to be fully described. The aim of this thesis was to gain insight into the individual microstructural components of the bladder wall and how they relate to the gross mechanical response. Additionally, representation of these observations in a mathematical model that can be used to improve our understanding of urodynamic data. This aim was achieved through a combination of in situ mechanical testing and the development of a microstructural constitutive model, which was then included within an overall micturition framework to simulate filling and voiding functions, and evaluated with clinical data. Coupled systems of multiphoton microscopy and uniaxial, biaxial and inflation testing were used to correlate extra cellular matrix interactions with the mechanical response of young and aged murine bladder. Wall-layer specific collagen fibre orientation, dispersion and recruitment were quantified and implemented into a novel microstructural constitutive model. The bladder was modelled as a nonlinear elastic, constrainedmixture planar membrane with contribution from smooth muscle and collagen fibres in the detrusor. Collagen recruitment in the detrusor was observed to occur at a finite stretch; correlated with a steep increase in stiffness of the tissue, while collagen of the lamina propria plays a capacitance role. Collagen recruitment was modelled using a triangular probability density function; quantified from sequential microscopy images and fitted to mechanical data. Increased collagen area fraction and changes in dominant fibre orientation were attributed to reduced compliance in aged bladder. This behaviour was captured by the model. The microstructural model was modified to an isotropic thin-walled spherical membrane for the filling phase of a micturition model framework, consisting of a bladder outlet relation and urethral resistance relation. A contractile smooth muscle element was included in the active response. In the first steps towards clinical application the model was applied to male and female 'normal' patient urodynamic data to observe quality of model fit and estimate baseline parameter values. The model simulated key filling and voiding features seen in normal male and female clinical data. Mechanobiological modelling combined with clinically relevant micturition modelling has the potential to quantify bladder dysfunction. Moreover, improved understanding of how the microstructure influences macroscopic mechanics will yield improved understanding of how changes to the bladder impair its functionality. We predict that modelling will become a clinically relevant tool in urodynamics; leading to new options for diagnosis and management of patients with bladder dysfunction.

O presente trabalho avalia a evolução das microestruturas e das propriedades mecânicas em tubos API 5L X65 soldados por fricção com auxílio de um anel centralizador na posição de topo. A soldagem foi realizada em tubos de 114,3 mm (4,5’’) de diâmetro nominal e 8 mm de espessura. A avaliação mecânica foi realizada segundo normas ASTM para os ensaios de tração, dobramento de raiz, dobramento de face, ensaio de impacto Charpy V e perfis de microdurezas. Os ensaios de fadiga foram realizados para análise da vida em fadiga das juntas soldadas. Os ensaios mecânicos realizados comprovam que houve a união metalúrgica dos materiais, sendo registradas regiões com defeitos de falta de adesão o que prejudicou as propriedades mecânicas ocasionando rupturas com baixa ductilidade nas interfaces de soldagem nestes locais. Nos resultados dos ensaios de microdurezas houve um pequeno aumento das microdurezas registradas próximo às interfaces de soldagem e uma redução nas microdurezas registradas nas regiões de ZACs. Os resultados do ensaio de impacto Charpy -20 °C foi aceitável segundo a norma API 5L. As microestruturas formadas nas interfaces de soldagem são compostas por ferrita de Widmanstätten e ferrita poligonal com crescimento de grão quando comparado com o tamanho de grão do material de base. Nas regiões de ZACs houve um reordenamento de carbonetos aliado a refino de grão sendo registrada uma redução nas microdurezas destas regiões. / This paper assesses the evolution of microstructures and mechanical properties in pipes API 5L X65 welded by friction with the aid of centering ring on top position. The welding was performed in tubes of 114.3 mm (4.5'') nominal diameter and 8 mm in thickness. The mechanical evaluation was performed according to ASTM standards for tensile, root bending, face folding, Charpy V impact test and microhardness profile. Fatigue tests were performed to analyze the fatigue life of the welded joints. The mechanical tests prove that there was a metallurgical union of the materials, regions with lack of adhesion defects being recorded which affected the mechanical properties causing fractures with low ductility in the weld interfaces in these places. Microhardness test results registered a small increase in the microhardness near the weld interfaces and a reduction in the microhardness recorded in the HAZ regions. The results of the Charpy impact test at -20°C was acceptable according to API 5L. The microstructures formed at the weld interfaces are composed of Widmanstatten ferrite and polygonal ferrite with grain growth when compared to the grain size in the base material. In HAZ regions there was a reorganization of carbides combined with grain refinement, with a reduction in microhardness of these regions being registered.

A implantação de Sistemas de Gestão da Qualidade em ambiente laboratorial vem se tornando uma necessidade frequente, devido à demanda dos clientes por resultados confiáveis e rastreáveis. No Brasil, a Coordenação Geral de Acreditação do Inmetro (Cgcre) é o órgão responsável pela acreditação de laboratórios segundo a NBR ISO/IEC 17025, sendo o Laboratório de Metalurgia Física (LAMEF) da Universidade Federal do Rio Grande do Sul acreditado para a realização de ensaios de materiais metálicos desde 2010. Em 2013, tendo passado por um processo de aumento de escopo de acreditação para os ensaios mecânicos, evidenciou-se o não atendimento ao item de garantia da qualidade da NBR ISO/IEC 17025 e da NIT-DICLA-026. Para atender aos requisitos, foram conduzidas análises através de Ensaios de Proficiência e por monitoramento interno da qualidade pelos métodos do Erro Normalizado e de Análise de Variância. Quando identificados desvios dos critérios de aceitação, ações corretivas foram tomadas, visando a melhoria contínua dos sistemas de medição. Os resultados do trabalho demonstraram que a implantação sistemática de métodos estatísticos para o monitoramento da qualidade dos ensaios foi fundamental para o processo de aumento do escopo de acreditação do LAMEF, o qual foi consolidado no início de 2014. / The implementation of Quality Management Systems in laboratory environment is being an increasing necessity, due to customer demand for reliable and traceable test results. The General Coordination for Accreditation of Inmetro (Cgcre/Inmetro) is the Brazilian body responsible for the accreditation of laboratories according to ISO/IEC 17025 standard, and the Physical Metallurgy Laboratory (LAMEF) from the Federal University of Rio Grande do Sul (UFRGS) has been accredited in performance of metallic materials tests since 2010. In 2013, during the process of accreditation scope extension on mechanical testing, there were identified nonconformities to the quality assurance requirements of ISO/IEC 17025 and NIT-DICLA-026. In order to comply with these requirements, studies have been carried out through Proficiency Testing and internal quality monitoring via Normalized Error and Analysis of Variance methods. Corrective actions were taken when deviations from the acceptance criteria were identified, aiming the measurement systems continuous improvement. The results of this work have demonstrated that the systematic implementation of statistical methods for monitoring the testing quality was critical to the process of LAMEF extension of scope, which was consolidated in the early 2014.

Made available in DSpace on 2016-12-23T13:53:37Z (GMT). No. of bitstreams: 1 Edson Vilela de Melo Filho.pdf: 1187344 bytes, checksum: 27f35634735962b8fdae9dc2162b0ffd (MD5) Previous issue date: 2010-04-30 / Objetivou-se com esse trabalho avaliar a resistência mecânica de placas ósseas produzidas a partir de osso cortical bovino, conservadas em diferentes meios, e a eficiência desses meios em inibir o crescimento de micro-organismos. Foram utilizadas 168 placas confeccionadas a partir de tíbia bovina e conservadas em glicerina a 98% (n=28), solução salina a 150% (n=28), solução de açúcar a 300% (n=28), líquido de Dakin (n=28), congeladas em N2L a - 196°C (n=28), ou esterilizadas em óxido de etileno (n=28). Após reidratação em solução de cloreto de sódio a 0,9% por seis horas, estas foram submetidas a ensaios mecânicos de tração, compressão, flexão e torção. Foi realizada avaliação microbiológica das placas anterior e imediatamente após a reidratação, com ou sem adição de enrofloxacina a 0,5%. Não se observou diferença significativa (P<0,01) da resistência ao ponto de ruptura entre as placas conservadas nos diferentes meios, congeladas-descongeladas ou esterilizadas. Micro-organismos foram isolados das placas conservadas em solução saturada de sal, açúcar, Dakin ou congeladas em N2L, anterior e após a reidratação. Entretanto, após o uso da solução de cloreto de sódio 0,9% acrescida de enrofloxacina a 0,5%, não foram isolados micro-organismos. Portanto, placas de osso bovino, conservadas em solução saturada de açúcar ou sal, glicerina a 98%, solução de Dakin, congeladas em N2L ou esterilizadas em óxido de etileno assemelham-se em relação à biomecânica, e a reidratação com solução de cloreto de sódio a 0,9% acrescida de enrofloxacina a 0,5% inibe o crescimento microbiano / The objective of this study was to evaluate the mechanical strength of bone plates yielded from bovine cortical bone, conserved in different solutions, and the efficiency of these solutions in the inhibition of microorganism s growth. 168 plates yielded from bovine tibiae were conserved in 98% glycerin (n=28), 150% saline solution (n=28), 300% sugar solution (n=28), Dakin solution (n=28), frozen in LN2 at - 196°C (n=28), or sterilized in ethylene oxide gas (n=28). After rehydratated in NaCl 0.9% solution for six hours, plates were subjected to tensile, compression, bending and twisting testing. Bone plates microbiological evaluation was carried out before and immediately after rehydratation, with or without enrofloxacin 0.5% addition. There was no significant difference (P<0.01) on resistance to the rupture point in plates conserved in the different solutions, frozen-thawed or sterilized. Microorganisms were isolated from plates conserved in satured salt solution, sugar satured solution, Dakin solution or frozen in LN2, before and after rehydratation. However, after the use of NaCl 0.9% solution added enrofloxacin 0.5%, microorganisms were not isolated. Therefore, bovine bone plates conserved in sugar or salt satured solution, 98% glycerin, Dakin solution, frozen in LN2 or sterilized in ethylene oxide gas present similar biomechanical tests results, and NaCl 0.9% solution added enrofloxacin 0.5% rehydratation inhibits microbial growth

abstract: Nanocrystalline (NC) and Ultrafine-grained (UFG) metal films exhibit a wide range of enhanced mechanical properties compared to their coarse-grained counterparts. These properties, such as very high strength, primarily arise from the change in the underlying deformation mechanisms. Experimental and simulation studies have shown that because of the small grain size, conventional dislocation plasticity is curtailed in these materials and grain boundary mediated mechanisms become more important. Although the deformation behavior and the underlying mechanisms in these materials have been investigated in depth, relatively little attention has been focused on the inhomogeneous nature of their microstructure (particularly originating from the texture of the film) and its influence on their macroscopic response. Furthermore, the rate dependency of mechanical response in NC/UFG metal films with different textures has not been systematically investigated. The objectives of this dissertation are two-fold. The first objective is to carry out a systematic investigation of the mechanical behavior of NC/UFG thin films with different textures under different loading rates. This includes a novel approach to study the effect of texture-induced plastic anisotropy on mechanical behavior of the films. Efforts are made to correlate the behavior of UFG metal films and the underlying deformation mechanisms. The second objective is to understand the deformation mechanisms of UFG aluminum films using in-situ transmission electron microscopy (TEM) experiments with Automated Crystal Orientation Mapping. This technique enables us to investigate grain rotations in UFG Al films and to monitor the microstructural changes in these films during deformation, thereby revealing detailed information about the deformation mechanisms prevalent in UFG metal films. / Dissertation/Thesis / Doctoral Dissertation Mechanical Engineering 2017

O presente trabalho avalia a evolução das microestruturas e das propriedades mecânicas em tubos API 5L X65 soldados por fricção com auxílio de um anel centralizador na posição de topo. A soldagem foi realizada em tubos de 114,3 mm (4,5’’) de diâmetro nominal e 8 mm de espessura. A avaliação mecânica foi realizada segundo normas ASTM para os ensaios de tração, dobramento de raiz, dobramento de face, ensaio de impacto Charpy V e perfis de microdurezas. Os ensaios de fadiga foram realizados para análise da vida em fadiga das juntas soldadas. Os ensaios mecânicos realizados comprovam que houve a união metalúrgica dos materiais, sendo registradas regiões com defeitos de falta de adesão o que prejudicou as propriedades mecânicas ocasionando rupturas com baixa ductilidade nas interfaces de soldagem nestes locais. Nos resultados dos ensaios de microdurezas houve um pequeno aumento das microdurezas registradas próximo às interfaces de soldagem e uma redução nas microdurezas registradas nas regiões de ZACs. Os resultados do ensaio de impacto Charpy -20 °C foi aceitável segundo a norma API 5L. As microestruturas formadas nas interfaces de soldagem são compostas por ferrita de Widmanstätten e ferrita poligonal com crescimento de grão quando comparado com o tamanho de grão do material de base. Nas regiões de ZACs houve um reordenamento de carbonetos aliado a refino de grão sendo registrada uma redução nas microdurezas destas regiões. / This paper assesses the evolution of microstructures and mechanical properties in pipes API 5L X65 welded by friction with the aid of centering ring on top position. The welding was performed in tubes of 114.3 mm (4.5'') nominal diameter and 8 mm in thickness. The mechanical evaluation was performed according to ASTM standards for tensile, root bending, face folding, Charpy V impact test and microhardness profile. Fatigue tests were performed to analyze the fatigue life of the welded joints. The mechanical tests prove that there was a metallurgical union of the materials, regions with lack of adhesion defects being recorded which affected the mechanical properties causing fractures with low ductility in the weld interfaces in these places. Microhardness test results registered a small increase in the microhardness near the weld interfaces and a reduction in the microhardness recorded in the HAZ regions. The results of the Charpy impact test at -20°C was acceptable according to API 5L. The microstructures formed at the weld interfaces are composed of Widmanstatten ferrite and polygonal ferrite with grain growth when compared to the grain size in the base material. In HAZ regions there was a reorganization of carbides combined with grain refinement, with a reduction in microhardness of these regions being registered.

A implantação de Sistemas de Gestão da Qualidade em ambiente laboratorial vem se tornando uma necessidade frequente, devido à demanda dos clientes por resultados confiáveis e rastreáveis. No Brasil, a Coordenação Geral de Acreditação do Inmetro (Cgcre) é o órgão responsável pela acreditação de laboratórios segundo a NBR ISO/IEC 17025, sendo o Laboratório de Metalurgia Física (LAMEF) da Universidade Federal do Rio Grande do Sul acreditado para a realização de ensaios de materiais metálicos desde 2010. Em 2013, tendo passado por um processo de aumento de escopo de acreditação para os ensaios mecânicos, evidenciou-se o não atendimento ao item de garantia da qualidade da NBR ISO/IEC 17025 e da NIT-DICLA-026. Para atender aos requisitos, foram conduzidas análises através de Ensaios de Proficiência e por monitoramento interno da qualidade pelos métodos do Erro Normalizado e de Análise de Variância. Quando identificados desvios dos critérios de aceitação, ações corretivas foram tomadas, visando a melhoria contínua dos sistemas de medição. Os resultados do trabalho demonstraram que a implantação sistemática de métodos estatísticos para o monitoramento da qualidade dos ensaios foi fundamental para o processo de aumento do escopo de acreditação do LAMEF, o qual foi consolidado no início de 2014. / The implementation of Quality Management Systems in laboratory environment is being an increasing necessity, due to customer demand for reliable and traceable test results. The General Coordination for Accreditation of Inmetro (Cgcre/Inmetro) is the Brazilian body responsible for the accreditation of laboratories according to ISO/IEC 17025 standard, and the Physical Metallurgy Laboratory (LAMEF) from the Federal University of Rio Grande do Sul (UFRGS) has been accredited in performance of metallic materials tests since 2010. In 2013, during the process of accreditation scope extension on mechanical testing, there were identified nonconformities to the quality assurance requirements of ISO/IEC 17025 and NIT-DICLA-026. In order to comply with these requirements, studies have been carried out through Proficiency Testing and internal quality monitoring via Normalized Error and Analysis of Variance methods. Corrective actions were taken when deviations from the acceptance criteria were identified, aiming the measurement systems continuous improvement. The results of this work have demonstrated that the systematic implementation of statistical methods for monitoring the testing quality was critical to the process of LAMEF extension of scope, which was consolidated in the early 2014.

A implantação de Sistemas de Gestão da Qualidade em ambiente laboratorial vem se tornando uma necessidade frequente, devido à demanda dos clientes por resultados confiáveis e rastreáveis. No Brasil, a Coordenação Geral de Acreditação do Inmetro (Cgcre) é o órgão responsável pela acreditação de laboratórios segundo a NBR ISO/IEC 17025, sendo o Laboratório de Metalurgia Física (LAMEF) da Universidade Federal do Rio Grande do Sul acreditado para a realização de ensaios de materiais metálicos desde 2010. Em 2013, tendo passado por um processo de aumento de escopo de acreditação para os ensaios mecânicos, evidenciou-se o não atendimento ao item de garantia da qualidade da NBR ISO/IEC 17025 e da NIT-DICLA-026. Para atender aos requisitos, foram conduzidas análises através de Ensaios de Proficiência e por monitoramento interno da qualidade pelos métodos do Erro Normalizado e de Análise de Variância. Quando identificados desvios dos critérios de aceitação, ações corretivas foram tomadas, visando a melhoria contínua dos sistemas de medição. Os resultados do trabalho demonstraram que a implantação sistemática de métodos estatísticos para o monitoramento da qualidade dos ensaios foi fundamental para o processo de aumento do escopo de acreditação do LAMEF, o qual foi consolidado no início de 2014. / The implementation of Quality Management Systems in laboratory environment is being an increasing necessity, due to customer demand for reliable and traceable test results. The General Coordination for Accreditation of Inmetro (Cgcre/Inmetro) is the Brazilian body responsible for the accreditation of laboratories according to ISO/IEC 17025 standard, and the Physical Metallurgy Laboratory (LAMEF) from the Federal University of Rio Grande do Sul (UFRGS) has been accredited in performance of metallic materials tests since 2010. In 2013, during the process of accreditation scope extension on mechanical testing, there were identified nonconformities to the quality assurance requirements of ISO/IEC 17025 and NIT-DICLA-026. In order to comply with these requirements, studies have been carried out through Proficiency Testing and internal quality monitoring via Normalized Error and Analysis of Variance methods. Corrective actions were taken when deviations from the acceptance criteria were identified, aiming the measurement systems continuous improvement. The results of this work have demonstrated that the systematic implementation of statistical methods for monitoring the testing quality was critical to the process of LAMEF extension of scope, which was consolidated in the early 2014.