Made available in DSpace on 2014-06-11T19:34:58Z (GMT). No. of bitstreams: 0 Previous issue date: 2006-12Bitstream added on 2014-06-13T19:44:43Z : No. of bitstreams: 1 silva_ap_dr_guara.pdf: 3551125 bytes, checksum: 3f75e8c0e99826910556f8cd772c1403 (MD5) / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) / Este trabalho analisa a transformação da austenita retida induzida por deformação, em um aço AISI 4340 com estruturas multifásicas. O aço foi submetido a duas rotas de tratamentos isotérmicos selecionadas e foi analisado quanto à fração volumétrica das fases e características mecânicas através da valiação dos limites de escoamento. Os corpos de prova foram submetidos a três diferentes níveis de tensões de tração, acima do limite de escoamento, para que se produzissem deformações plásticas determinadas. A influência destas deformações, na microestrutura e nos novos limites de escoamento, foram avaliadas. Mostrando variações significativas nas frações volumétricas das fases, com diminuição das quantidades de austenita, indicando uma transformação, por efeito TRIP (Transformation Induced Plasticity), em martensita o que provocou um aumento nos valores dos limites de escoamento e envelhecimento por deformação. / The Transformation induced plasticity of austenite on the multiphase microstructure in a AISI 4340 steel was studied. Two sequences of isothermal treatments were performed. The volume fractions of the phases were analyzed and evaluation of mechanical characteristics through the yield point measurements. The samples were submitted at three different levels of traction above of the yield strength, so that definitive plastic deformations were produced. The influence of these deformations in the microstructure and in the new yield strength was evaluated. Significant variations were showed in the phase volume fraction, with reduction of the amounts of austenite indicating a martensitic transformation, by effect TRIP (Transformation Induced Plasticity) which results increases in the values of the yield strength and deformation ageing.

Submitted by Claudinei Pracidelli (cpracide@ipen.br) on 2015-07-23T10:56:10Z No. of bitstreams: 0 / Made available in DSpace on 2015-07-23T10:56:10Z (GMT). No. of bitstreams: 0 / Dissertação (Mestrado em Tecnologia Nuclear) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Este trabalho teve como objetivo observar o resultado da variação dos parâmetros do processo FHPP (Friction Hydro Pillar Processing), dando-se atenção aos efeitos destes na microestrutura e na qualidade do reparo. O estudo foi realizado através de investigações metalográficas nos reparos obtidos, bem como análises via perfis de microdureza Vickers. Foram utilizadas diferentes forças axiais, que levaram a obtenção de reparos isentos de defeitos no seu preenchimento. Observou-se que o utilizando forças axiais maiores contribuíram para obter microestrutura mais refinada e homogênea, com formação predominante de martensita, menor tempo de processamento, menor quantidade de constituinte Martensita-Austenita e uma Zona Termicamente Afetada (ZTA) de menor tamanho. / This study aimed to observe the result of the variation of the Friction Hydro Pillar Processing parameters, giving attention to the microestructural effects and quality of repair. The study was carried out by metallographic investigations in repairs obtained and Vickers microhardness profiles. Were used different axial forces, which led to obtain no defects in repairs. It was observed that using higher axial forces helped to get more refined and homogeneous microstructure with predominant formation of martensite, lower processing time, less amount of Martensite-Austenite constituent and lower Heat Afecfted Zone (HAZ) size.

Este trabalho teve como objetivo observar o resultado da variação dos parâmetros do processo FHPP (Friction Hydro Pillar Processing), dando-se atenção aos efeitos destes na microestrutura e na qualidade do reparo. O estudo foi realizado através de investigações metalográficas nos reparos obtidos, bem como análises via perfis de microdureza Vickers. Foram utilizadas diferentes forças axiais, que levaram a obtenção de reparos isentos de defeitos no seu preenchimento. Observou-se que o utilizando forças axiais maiores contribuíram para obter microestrutura mais refinada e homogênea, com formação predominante de martensita, menor tempo de processamento, menor quantidade de constituinte Martensita-Austenita e uma Zona Termicamente Afetada (ZTA) de menor tamanho. / This study aimed to observe the result of the variation of the Friction Hydro Pillar Processing parameters, giving attention to the microestructural effects and quality of repair. The study was carried out by metallographic investigations in repairs obtained and Vickers microhardness profiles. Were used different axial forces, which led to obtain no defects in repairs. It was observed that using higher axial forces helped to get more refined and homogeneous microstructure with predominant formation of martensite, lower processing time, less amount of Martensite-Austenite constituent and lower Heat Afecfted Zone (HAZ) size.

Uma das técnicas para fabricar microestruturas em diamante é usar moldes em silício microfabricados. Assim, microestruturas são produzidas em laminas de silício, um filme de diamante é depositado sobre essa lamina e o silício é corroído. Dessa forma é possível se obter réplicas de diamante das microestruturas que estavam presentes na superfície do molde de silício. Nesta técnica é muito importante a fidelidade morfológica da réplica de diamante, quando comparada ao molde de silício, previamente microfabricado. Um dos objetivos deste trabalho é analisar quantitativamente a fidelidade de reprodução de microestruturas em filmes de diamante, utilizando moldes de silício microfabricados. Nossos resultados mostram que a rugosidade das réplicas de diamante é sistematicamente maior que a rugosidade dos moldes de silício. Medindo degraus em escala de centenas de nanômetros, o erro na reprodução morfológica está entre 6 e 11 %. No caso de medidas de degraus em escala de dezenas de nanômetros, o erro na reprodução é de aproximadamente 18 %. O segundo objetivo deste trabalho consiste em comparar a variação da rugosidade de uma superfície devido ao recobrimento com filmes de DLC. Os resultados sugerem que, para substratos com rugosidade original de centenas de nanômetros, a variação da rugosidade tende a aumentar com a espessura do filme de DLC até um valor máximo, a partir do qual ela tende a diminuir. Para substratos com rugosidade original de alguns poucos nanômetros, a variação da rugosidade oscila aleatoriamente, não apresentando tendências de aumentar ou diminuir com a espessura do filme de DLC. Finalmente, a última parte desta Tese foi fabricar um microbocal de diamante utilizando a técnica de moldes microfabricados em silício. / One of the techniques to fabricate microstructures in diamond is to use microfabricated silicon molds. Microstructures are produced on silicon wafer; diamond film is deposited on it and the silicon is etched. In this way, it is possible to obtain diamond replicas of the microstructures that were present in the silicon surface. In this technique it is very important the morphological fidelity of the diamond replica, when compared with the silicon mold previously microfabricated. One of our objectives in this work is to analyze quantitatively the reproduction fidelity of microstructures in diamond films, using microfabricated silicon molds. The results show that, roughnesses of the diamond replicas are systematically higher than the roughness of the silicon molds. Measuring steps in scales of hundreds of nanometers, the reproduction error is between 6 and 11 %. In the case of steps measured in scales of tenth of nanometers, the reproduction error is about 18 %. A second objective of this work is to compare the roughness change of rough surfaces coated with DLC films. The results suggest that, for substrates with original roughness of hundreds of nanometers, the roughness shift tends to increase with the DLC film thickness until a maximum value and then it tends to decrease. For substrates with original roughness of few nanometers, the roughness shift oscillates erratically and it does not tend to increase or decrease with the DLC film thickness. Finally, the last part of this Thesis was to fabricate a diamond micronozzle, using the technique of silicon molds microfabricated.

Les émulsions sont très utilisées dans le domaine des cosmétiques, notamment pour les crèmes et les lotions. En fonction de leur composition, elles présentent diverses propriétés en matière de stabilité, de texture, de microstructure et de macrostructure. Il n’existe pas, à l’heure actuelle, d’étude dans la littérature qui se soit intéressée à l’effet de la composition sur ces différentes propriétés et aux relations qui peuvent exister entre celles-ci, tout en mettant en œuvre une maîtrise de la formulation. Pour répondre à cette double problématique, quatorze émulsions huile-dans-eau ont été formulées, avec un protocole maîtrisé, pour lesquelles les concentrations en phase grasse, en gomme acacia et en xanthane varient. Des solutions de xanthane et de gomme acacia ont également été préparées pour comparer l’effet des gommes en émulsion et en phase aqueuse seule. Les produits ont été ensuite caractérisés, de façon la plus complète et objective possible, pour mettre en évidence l’influence de la composition sur les propriétés de l’émulsion et leurs interactions. De nombreux paramètres ont ainsi été collectés par : analyse sensorielle, des observations microscopiques et des mesures en granulométrie laser, des mesures rhéologiques et mécaniques. On peut en conclure que chacun des paramètres de l’émulsion impacte ses propriétés, avec des différences notables, la teneur en phase grasse étant, globalement, prépondérante. Des relations entre l’ensemble des données ont été mises en évidence et permettent de proposer des hypothèses quant à l’impact de la formulation sur les propriétés tactiles des crèmes cosmétiques. / Emulsions are widely used in cosmetics. Depending on their composition, they exhibit various properties in terms of stability, texture, microstructure and macrostructure. At the present time, there a few to no studies in the literature interested in the effect of the emulsions composition on these different properties and the existing link between these characteristics that are implementing a command of the formulation. To address this dual problem, fourteen oil-in-water emulsions were formulated, with a controlled formulation protocol, for which the concentration of oil phase, acacia gum and xanthan gum evolve. Solutions of xanthan and acacia gums were also prepared to compare the effect of the gums on emulsions to the one on aqueous phase alone. The products were then characterized, in the most complete and objective way possible, to illustrate the influence of the composition on the properties of the emulsions and how these interact. Numerous parameters were collected through : ensory analysis, mcroscopic observations and static light scattering measurements, rhlogical and instrumental texture analyses. t can be concluded that the emulsions are well differentiates and that each of the emulsion parameter impacts its properties with significant differences, the oil phase content being preponderant overall. elationships between the data set were highlighted and suggest hypotheses about the impact of the formulation on the tactile properties of cosmetic creams.

This work explores the processing-microstructure-property relationships in two-phase titanium alloys such as Ti-6Al-4V and Ti-5Al-5V-5Mo-3Cr that are used for aerospace applications. For this purpose, an Integrated Computational Materials Engineering approach is used. Microstructure and texture of titanium alloys are characterized using optical microscopy, electron backscatter diffraction and x-ray diffraction. To model their properties, threedimensional synthetic digital microstructures are generated based on experimental characterization data. An open source software package, DREAM.3D, is used to create heterogeneous two-phase microstructures that are statistically representative of two-phase titanium alloys. Both mean-field and full-field crystal plasticity models are used for simulating uniaxial compression at different loading conditions. A viscoplastic self-consistent model is used to match the stress-strain response of the Ti-5553 alloy based on uniaxial compression tests. A physically-based Mechanical Threshold Stress (MTS) model is designed to cover wide ranges of deformation conditions. Uncertainties in the parameters of the MTS model are quantified using canonical correlation analysis, a multivariate global sensitivity analysis technique. An elastoviscoplastic full-field model based on the fast Fourier transform algorithm was used to used to simulate the deformation response at both microscopic and continuum level. The probability distribution of stresses and strains for both the phases in the two-phase material is examined statistically. The effect of changing HCP phase volume fraction and morphology has been explored with the intent of explaining the ow softening behavior in titanium alloys.

With the discovery of conductivity in doped polyacetylene (PA), a new era in synthetic metals has emerged by breaking the traditionally accepted view that polymers were always insulating. Conducting polymers are essentially characterized by the presence of conjugated bonding on the polymeric back bone, which facilitates the formation of polarons and bipolarons as charge carriers. Among the numerous conducting polymers synthesized to date, polypyrrole (PPy) is by far the most extensively studied because of prodigious number of applications owing to its facile polymerizability, environmental stability, high electrical conductivity, biocompatibility, and redox state dependent physico-chemical properties. Electrochemically prepared PPy is more interesting than the chemically prepared polymer because it adheres to the electrode surface and can be directly used for applications such as supercapacitors, electrochemical sensors, electromechanical actuators and drug delivery systems. In quest for improvement in quality of the device performances in the mentioned applications, micro and nano structured polymeric materials which bring in large surface area are studied. Finding a simple and efficient method of synthesis is very important for producing devices of PPy microstructures. Till date, Hard and soft template methods are the most employed methods for synthesis of these structures. Soft template based electrochemical methods are better than hard template methods to grow clean PPy microstructures on electrode substrates as procedures for removal of hard templates after the growth of microstructures are very complex. As per the literature, there is no unique method available to grow PPy microstructures which can demonstrate several applications. Although gas bubble based soft template methods are exploited to grow conducting polymer microstructures of sizes in few hundreds of micrometers, studies on applications of the same are limited. Hence it is planned to develop procedures to grow microstructures that can be used in several applications. In the current work, PPy microstructures with high coverage densities are synthesized on various electrode substrates by soft template based electrochemical techniques. Hollow, hemispherical and spherical PPy microstructures are developed by a two step method using electro generated hydrogen bubble templates on SS 304 electrodes. In the first step, Hydrogen bubbles are electro generated and stabilized on the electrode in the presence of β- naphthalene sulfonic acid (β-NSA). In the second step, Pyrrole is oxidised over the bubble template to form PPy microstructures. Microstructures (open and closed cups) of average size 15 μm are uniformly spread on the surface with a coverage density of 2.5×105 units /cm2. Globular PPy microstructures are developed by a single step method using concomitantly electro generated oxygen bubble templates on SS 304 electrodes during electropolymerization. Microstructures of average size 4 μm are uniformly spread on the surface with a coverage density of 7×105 units/cm2. Surfactant properties of Zwitterionic 4-(2-hydroxyethyl)-1-piperazine ethane sulfonic acid (HEPES) are exploited for the first time to grow conducting polymer microstructures. Ramekin shaped PPy microstructures are developed using HEPES as the surfactant to stabilize hydrogen bubble templates in a two step electrochemical synthesis method. Microramekins of size 100 µm are uniformly spread on the surface with a coverage density of 3000 units/cm2. Micropipettes and microhorns of PPy are synthesised by a single step electrochemical route using HEPES as a surfactant. Hollow micropipettes of length 7 µm with an opening of 200 nm at the top of the structure are observed. Similarly microhorn/celia structures are observed with length 10-15 µm. Microcelia are uniformly distributed over the surface with each structure having a diameter of 2 µm at the base to 150 nm at the tip. Growth mechanism based on contact angle of the reactant solution droplets on the substrate is proposed. PPy microstructures are characterized by scanning electron microscopy, X-Ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, Raman Spectroscopy and UV-Visible spectroscopy to study morphology, ‘chemical bonding and structure’ , ‘defects and charge carriers’. Applicability of the electrodes with PPy microstructures in supercapacitors is investigated by cyclic voltammetry, chronopotentiometry and electrical impedance spectroscopy. Electrodes developed by all the above methods demonstrated very good supercapacitance properties. Supercapacitor studies revealed very high specific capacitances (580, 915, 728 and 922 F/g,) and specific powers (20, 25, 13.89 and 15.91 kW/kg) for electrodes with PPy microstructures (H2 bubble based two step method, O2 bubble based single step method, HEPES stabilized H2 bubbble method and HEPES based microhorn/celia structures respectively). Supercapacitive behavior of all the electrodes is retained even after an extended charge-discharge cycling in excess of 1500 cycles. Horseradish peroxidase entrapped, bowl shaped PPy microstructures are developed for H2O2 biosensing. Amperometric biosensor has a performance comparable to the sensors reported in the literature with high sensitivity value of 12.8 μA/(cm2.mM) in the range 1.0 mM to 10 mM. Glucose oxidase entrapped PPy amperometric biosensor is developed for Glucose sensing. Sensitivity of 1.29 mA/(cm2.mM) is observed for β-D-Glucose sensing in the 0.1 mM to 5.0 mM range while 58 μA/(cm2.mM) is observed in the 5.0 to 40 mM range. Potentiometric urea sensor with urease entrapped PPy microstructures on SS electrode is developed. It is able to sense urea in the micromolar ranges down to 0.1 μM. It represented an excellent performance with sensitivity of 27 mV/decade. Sensitivity in the micromolar range is 4.9 mV/(μM.cm2). Drug encapsulation and delivery is successfully demonstrated by two actuation means (i) by electrochemical actuation, (ii) by actuation based on pH changes. Concepts are proved by delivering a fluorescent dye into neutral and acidic solutions. Drug delivery is confirmed by UV-Visible spectroscopy and Fluorescence microscopy. Finally, Micro/nanostructures with Tangerine, Hollow globular (Pani Poori), Chip, Flake, Rose, Worm, Horn and Celia shapes are synthesized electrochemically and scanning electron microscopic studies are presented. Controlled growth of microstructures on lithographically patterned gold interdigital electrodes is demonstrated with a future goal of creating addressable microstructures. The studies reported in the thesis provide an insight on various applications of PPy microstructures (supercapacitors, sensors and drug delivery systems) developed by a unique methodology based on electrochemically generated gas bubble templates.

No / As the weakest zone in concrete, the interfacial transition zone (ITZ) between aggregates and cement mortars has important effects on the properties of concrete. This paper aims to investigate the effects and mechanisms of nanofillers on the bond strength and interfacial microstructures between aggregates and cement mortars. A total of 8 representative types of nanofillers (namely nano-SiO2, nano-TiO2, nano-ZrO2, untreated multi-walled carbon nanotubes (MWCNTs), hydroxyl-functionalized MWCNTs, nickel-coated MWCNTs, multi-layer graphenes (MLGs), and nano boron nitride (nano-BN)) were selected to fabricate specimens with scale-up aggregate-cement mortar interface that can be characterized by the three-point bend test. The experimental results indicate that all types of nanofillers can enhance the bond strength between aggregates and cement mortars. The highest relative/absolute increases of 2.1 MPa/35.1%, 2.32 MPa/38.8% and 2.56 MPa/42.8% in interfacial bond strength are achieved by incorporating 2 wt% of nano-ZrO2, 0.3 wt% of nickel-coated MWCNTs, and 0.3 wt% of nano-BN, respectively. Scanning electron microscope observations show the presence of nanofillers can improve hydration products and increase interfacial compactness. Energy dispersive spectrometer results suggest that local content of nanofillers in the ITZ is higher than that in the bulk cement mortars. These findings indicate the nanofillers can transfer with water migration toward aggregates and enrich in ITZ, thus improving the bond strength and interfacial microstructures between aggregates and cement mortars through the nano-core effect. / National Science Foundation of China (51978127 and 51578110), and the Fundamental Research Funds for the Central Universities in China(DUT18GJ203)

Yes / This study investigates the interfacial characteristics between aggregates and cement paste matrix in nanofillers modified concrete. A three-point bend test on the specimens composed of two pieces of aggregates bonded with a thin layer of cement pastes with/without nanofillers was carried out to characterize the interfacial bond strength of the composites. The scanning electron microscope observations and energy dispersive x-ray spectrometry analysis were also performed to characterize the interfacial microstructures and compositions of the composites. The experimental results indicated that the nanocomposites have higher interfacial bond strength and narrower interfacial transition zone thickness as well as more optimized intrinsic compositions and microstructures than that of composites without nanofillers. Specifically, the interfacial bond strength of nanocomposites can reach 7.67 MPa, which is 3.03 MPa/65.3% higher than that of composites without nanofillers. The interfacial transition zone thickness of nanocomposites ranges from 9 μm to 12 μm, while that of composites without nanofillers is about 18 μm. The ratio of CaO to SiO2 in the interface of composites without nanofillers is 0.69, and that of nanocomposites increases to 0.75–1.12. Meanwhile, the nanofiller content in nanocomposite interface is 1.65–1.98 times more than that in the bulk matrix. The interfacial microstructures of nanocomposites are more compact and the content and crystal size of calcium hydroxide were significantly reduced compared with that of composites without nanofillers. / The National Science Foundation of China (51978127 and 51908103), and the China Postdoctoral Science Foundation (2019M651116).