O aço ferrítico-martensítico ODS Eurofer com 9%pCr (ODS - do inglês oxide dispersion strengthened), objeto de estudo dessa dissertação, é um potencial candidato para fins estruturais em reatores de fusão nuclear. Este material foi produzido via metalurgia do pó e consolidado por prensagem isostática. Em seguida sofreu laminação cruzada a quente e revenimento em 750°C por 2h. Esta foi a condição como recebida desse aço, o qual foi cedido pelo KIT (Karlsruher Institut für Technologie - Alemanha). Este aço possui 0,3%p de partículas de ítria (Y2O3) com diâmetro entre 10 e 30 nm. Uma das finalidades dessa dispersão de partículas de óxido é impedir a livre movimentação de contornos de grão no material, de modo a garantir a estabilidade microestrutural do mesmo sob recozimento. O aço ODS Eurofer como recebido foi laminado a frio com reduções de 20, 40, 60 e 80% da espessura e, posteriormente, foi recozido em diversas temperaturas entre 300 e 1350°C por 1h. Como o enfoque desse trabalho é sobre o aço ODS Eurofer recozido em altas temperaturas, para as temperaturas de 1250, 1300 e 1350°C foram feitos recozimentos adicionais (para o material com 80% de redução) variando-se o tempo de recozimento de 1 a 8 h. Para todos os recozimentos, com exceção dos realizados em 1350°C, o resfriamento das amostras se deu ao ar. Para a temperatura de 1350°C isso não foi possível e o resfriamento das amostras se deu no interior do forno. As amostras foram caracterizadas utilizando-se de medidas de dureza, medidas magnéticas e microscopia eletrônica de varredura (MEV). Amostras representativas também foram analisadas utilizando-se de difração de elétrons retroespalhados (EBSD) e espectroscopia por energia dispersiva (EDS). Para recozimentos em temperaturas acima de 800°C seguidos de resfriamento ao ar o material sofreu uma transformação martensítica. Na faixa de temperatura entre 800°C e 1300°C verificou-se um ligeiro decréscimo na dureza do material. Para as amostras com 80% de redução e recozidas em 1250 e 1300°C por diversos tempos até 8 h, seguido de resfriamento ao ar, não ocorreu uma variação significativa tanto nos valores de dureza e de campo coercivo das amostras com o tempo de recozimento. Estes valores se mantiveram em um patamar bem superior ao verificado para as amostras sem recozimento. Para as amostras recozidas em 1350°C, devido às características do resfriamento a microestrutura resultou em grãos ferríticos, aproximadamente equiaxiais e com tamanho de grão médio da ordem de 15 ?m. Observou-se uma notável queda tanto no valor de dureza como de campo coercivo dessas amostras. A observação mais importante nesse caso foi a observação de partículas da ordem de 100 nm ricas em ítrio no interior dos grãos, uma evidência de que ocorre o engrossamento das partículas de ítria nessa temperatura. Em virtude disso, a capacidade dessa dispersão de óxidos em impedir a livre movimentação de contornos de grãos no material fica prejudicada em 1350°C. / The object of this study is Eurofer 9% Cr Oxide Dispersion Strengthened (ODS) steel. This ferritic/martensitic steel is a potential candidate for structural applications in nuclear fusion reactors. It is produced through powder metallurgy and consolidated by hot isostatic pressing. The material undergoes hot cross lamination and is tempered at 760 °C. This was the condition of the steel as received, which was provided by KIT (Karlsruher Institut für Technologie, Germany). This steel contains 0.3 wt% yttria particles (Y2O3) with a diameter in the range 10-30nm. The main purpose of this oxide particle dispersion is to prevent the free movement of the grain boundaries in the material, so as to ensure stability of the microstructure during annealing. The material as received was cold rolled to reduce thickness by 20, 40, 60 and 80%. It was annealed at different temperatures from 300 to 1350 °C for 1 h. The focus of this study is the effects of high temperature annealing on the microstructure of ODS Eurofer. For this purpose, additional heat treatments were carried out on the steel that had been rolled to reduce thickness by 80% at temperatures of 1250, 1300 and 1350 °C. Annealing time varied between 15 min and 8 h. For all annealing conditions, except those carried out at 1350 °C, the samples were air cooled. For the temperature of 1350 °C, this was not possible. These samples were cooled in the oven. The samples were characterized using hardness testing, magnetic testing, and scanning electron microscopy (SEM). Representative samples were also analyzed using electron backscatter diffraction (EBSD) and energy dispersive spectroscopy (EDS). For annealing at temperatures above 800 °C, the material underwent a martensitic transformation after air cooling. Between 800 and 1300 °C, there was a slight decrease in the hardness of the material. For samples with 80% reduction annealed at 1250 and 1300 °C followed by air cooling, annealing time up to 8h didn\'t lead to a significant variation in either the hardness or the coercive field. Both hardness and coercive field of these samples were at a level well above the samples without annealing. For samples annealed at 1350 °C, due to the cooling characteristics of the samples, the microstructure took on a ferritic matrix with equiaxed grains with an average grain size of 15 um. There was a remarkable decrease in hardness and coercive field values of these samples. The most important result in this case was the observation of yttria-rich particles of the order of 100nm inside the grains. This is an evidence of the coarsening of the yttria particles at this temperature. As a result, the capacity of oxide dispersion to prevent the free movement of grain boundaries in the material is impaired at 1350°C.

O estudo de usinabilidade de um material é muito importante para a determinação das características de fabricação por usinagem. Este estudo se aplica ao aço inoxidável martensítico AISI 420 C endurecido, usado na fabricação de peças de alta precisão, instrumentos cirúrgicos, eixos, turbinas e cutelaria. Deste modo, realizaram-se investigações utilizando corpos de prova endurecidos (têmpera e revenimento) com durezas de (48  1) e (53  2) HRC no torneamento a seco utilizando ferramentas de metal-duro classe ISO S com grãos extrafinos e revestimento PVD. Para estes corpos de prova variaram-se a velocidade de corte e o avanço e avaliaram-se as forças de usinagem e as tensões residuais geradas na peça. Para o material com 53 HRC, também foram analisadas a vida da ferramenta e a rugosidade. Na análise dos resultados obtidos para o material com 48 HRC, as tensões residuais tornaram-se menos compressivas (circunferencial) e mais trativas (axial) com o aumento do avanço. Além disso, os menores valores de tensão residual foram gerados utilizando menor avanço com maior velocidade de corte. Nos ensaios para o material a 53 HRC, o tempo de vida da ferramenta ficou entre 100 e 350 min para as condições ensaiadas. Os desgastes de flanco e entalhe foram evidenciados em todas as situações. O flanco da ferramenta também apresentou adesão de material da peça em todas as condições. Ao analisar os insertos em seu fim de vida, constatou-se que os mecanismos de desgastes predominantes foram a abrasão e o atrittion. Nas condições mais severas, a superfície da ferramenta exibiu trincas mecânicas e a camada subsuperficial da peça apresentou modificações microestruturais. Os perfis e os parâmetros de rugosidade registrados foram afetados pelo desgaste ao longo da vida da ferramenta. Com relação às tensões residuais circunferenciais geradas com a ferramenta nova, estas foram, em sua maioria, tensões de compressão. Com a progressão do desgaste de flanco, houve um aumento dos valores das tensões (de compressivas para menos compressivas ou até mesmo trativas). Já para as tensões axiais, os valores mostraram a tendência de se manterem compressivos. Observou-se para os perfis de tensões analisados que as tensões residuais foram compressivas e dependeram da profundidade da camada subsuperficial. Portanto, dentro das condições estudadas, conclui-se que peças de AISI 420 C endurecido podem ser fabricadas por torneamento de acabamento com ferramentas de metal-duro, permitindo obter vida longa para a ferramenta de corte, baixos valores de rugosidade, bem como valores de tensão residual compressiva, que são dados de usinabilidade importantes para esse material. / The study of the material’s machinability is very important for the determination of important machining properties. This logic applies to hardened martensitic stainless steel AISI 420 C used in the manufacture of high precision parts, surgical instruments, shafts, turbines and cutlery. In this way, investigations were carried out using hardened workpieces (quenching and tempering) with hardness of (48  1) and (53  2 HRC) in dry turning using ISO-S grade carbide tools with extra-fine grains and PVD coating. For these workpieces, the cutting speed and the feed rate were varied and the machining forces and the residual stresses generated in the part were evaluated. For the material with 53 HRC, the tool-life and the surface roughness were also analyzed. In the analysis of the results obtained for the material with 48 HRC, residual stresses become less compressive (circumferential direction) and more tensile (axial direction) with increasing feed-rate. Moreover, smaller values of residual stress were generated using lower feed-rate at higher cutting speed. In the tests for the material at 53 HRC, the tool-life was between 100 and 350 min for the conditions tested. Flank and notch wear were evidenced in all situations. The flank face of the tool also showed adhesion of the workpiece material under all cutting conditions. When analyzing the inserts at their end of life, it was verified that the main mechanisms of tool wear were abrasion and attrition. In addition, under the most severe cutting conditions, the flank face of the tool exhibited mechanical cracks and the subsurface layer of the workpieces presented microstructural modifications. The registered profiles and roughness parameters were affected by wear during the tool-life. With respect to the circumferential residual stresses generated with the fresh tool, these were mostly compressive stresses. With the progression of tool flank wear, there was an increase in the values of the residual stress (from compressive to less compressive or even tractive). For the axial residual stresses, the values showed a tendency to remain compressive. It was observed for the residual stress profiles analyzed that the residual stresses were compressive and depended on the depth of subsurface layer. Therefore, within the cutting conditions considered, it can be concluded that hardened martensitic stainless steel AISI 420 C parts can be manufactured by finishing turning with carbide tools, allowing long tool-life, low surface roughness values, as well as compressive residual stress values, which are important machinability information for this material.

Martensite is considered to be the backbone of the high strength of many commercial steels. Martensite is formed by a rapid diffusionless phase transformation, which has been the subject of extensive research studies for more than a century. Despite such extensive studies, martensitic transformation is still considered to be intriguing due to its complex nature. Phase-field method, a computational technique used to simulate phase transformations, could be an aid in understanding the transformation. Moreover, due to the growing interest in the field of “Integrated computational materials engineering (ICME)”, the possibilities to couple the phase-field method with other computational techniques need to be explored. In the present work a three dimensional elastoplastic phase-field model, based on the works of Khachaturyan et al. and Yamanaka et al., is developed to study the athermal and the stress-assisted martensitic transformations occurring in single crystal and polycrystalline steels. The material parameters corresponding to the carbon steels and stainless steels are considered as input data for the simulations. The input data for the simulations is acquired from computational as well as from experimental works. Thus an attempt is made to create a multi-length scale model by coupling the ab-initio method, phase-field method, CALPHAD method, as well as experimental works. The model is used to simulate the microstructure evolution as well as to study various physical concepts associated with the martensitic transformation. The simulation results depict several experimentally observed aspects associated with the martensitic transformation, such as twinned microstructure and autocatalysis. The results indicate that plastic deformation and autocatalysis play a significant role in the martensitic microstructure evolution. The results indicate that the phase-field simulations can be used as tools to study some of the physical concepts associated with martensitic transformation, e.g. embryo potency, driving forces, plastic deformation as well as some aspects of crystallography. The results obtained are in agreement with the experimental results. The effect of stress-states on the stress-assisted martensitic microstructure evolution is studied by performing different simulations under different loading conditions. The results indicate that the microstructure is significantly affected by the loading conditions. The simulations are also used to study several important aspects, such as TRIP effect and Magee effect. The model is also used to predict some of the practically important parameters such as Ms temperature as well as the volume fraction of martensite formed. The results also indicate that it is feasible to build physically based multi-length scale model to study the martensitic transformation. Finally, it is concluded that the phase-field method can be used as a qualitative aid in understanding the complex, yet intriguing, martensitic transformations. / QC 20120525 / Hero-m

No description available.

In this thesis two kinds of phase change i.e., solid state phase transformation in steels and solid-to-liquid phase transformation in paraffin, have been modeled and numerically simulated. The solid state phase transformation is modeled using the phase field theory while the solid-to-liquid phase transformation is modeled using the Stokes equation and exploiting the viscous nature of the paraffin, by treating it as a liquid in both states.The theoretical base of the solid state, diffusionless phase transformation or the martensitic transformation comes from the Khachaturyan's phase field microelasticity theory. The time evolution of the variable describing the phase transformation is computed using the time dependent Ginzburg-Landau equation. Plasticity is also incorporated into the model by solving another time dependent equation. Simulations are performed both in 2D and 3D, for a single crystal and a polycrystal. Although the model is valid for most iron-carbon alloys, in this research an Fe-0.3\%C alloy is chosen.In order to simulate martensitic transformation in a polycrystal, it is necessary to include the effect of the grain boundary to correctly capture the morphology of the microstructure. One of the important achievements of this research is the incorporation of the grain boundary effect in the Khachaturyan's phase field model. The developed model is also employed to analyze the effect of external stresses on the martensitic transformation, both in 2D and 3D. Results obtained from the numerical simulations show good qualitative agreement with the empirical observations found in the literature.The microactuators are generally used as a micropump or microvalve in various miniaturized industrial and engineering applications. The phase transformation in a paraffin based thermohydraulic membrane microactuator is modeled by treating paraffin as a highly viscous liquid, instead of a solid, below its melting point.  The fluid-solid interaction between paraffin and the enclosing membrane is governed by the ALE technique. The thing which sets apart the presented model from the previous models, is the use of geometry independent and realistic thermal and mechanical properties. Numerical results obtained by treating paraffin as a liquid in both states show better conformity with the experiments, performed on a similar microactuator. The developed model is further employed to analyze the time response of the system, for different input powers and geometries of the microactuator. / <p>QC 20130219</p>

Shape memory alloys (SMAs) are an important class of smart materials that have the ability to remember a shape. Current practical uses of SMAs are limited to below 100 degrees C which is the limit for the transformation temperatures of most commercially successful SMAs such as NiTi and Cu-based alloys. In recent years, the CoNiGa system has emerged as a new ferromagnetic shape memory alloy with some compositions exhibiting high martensitic transformation temperatures which makes CoNiGa a potential high temperature shape memory alloy (HTSMA). In this study, the microstructural evolution and martensitic transformation characteristics of CoNiGa (mainly Co46Ni27Ga27 and Co44Ni26Ga30 in at.percent) HTSMAs were investigated in as-cast and hot-rolled conditions as a function of different heat treatments. Heat treatment conditions were selected to introduce single, two, and three phase structures, where two precipitate phases (ductile Y and hard Y') do not martensitically transform. Calorimetry, X-ray analysis, scanning and transmission electron microscopy, thermo-mechanical process and cycling techniques are applied to understand the structural and chemical factors influencing the thermal stability and transformation characteristics. The main findings include improvement of ductility, most cyclically stable compositions with narrow transformation hysteresis (<40 degrees C) and transformation temperatures in the range of 100 degrees C to 250 degrees C, formation of new phases and their effects, and associated compositional changes in the matrix, on the transformation temperatures and on the microstructural evolution. In addition, Ms temperature depends linearly on the valence electron concentration (e/a) of the matrix, only if the Ga content is constant, and the samples with narrow transformation hysteresis demonstrate reversible martensitic transformation in constant-stress thermal cycling experiments.

Porous TiNi alloys (Ti-50.4 at. %Ni and Ti-50.6 at. %Ni) with porosities in the range 21%-81% were prepared successfully applying a new powder metallurgy fabrication route in which magnesium was used as space holder resulting in either single austenite phase or a mixture of austenite and martensite phases dictated by the composition of the starting prealloyed powders but entirely free from secondary brittle intermetallics, oxides, nitrides and carbonitrides. Magnesium vapor do not only prevents secondary phase formation and contamination but also provides higher temperature sintering opportunity preventing liquid phase formation at the eutectic temperature, 1118 &deg / C resulting from Ni enrichment due to oxidation. By two step sintering processing (holding the sample at 1100 &deg / C for 30 minutes and subsequently sintering at temperatures higher than the eutectic temperature, 1118 &deg / C) magnesium may allow sintering probably up to the melting point of TiNi. The processed alloys exhibited interconnected (partially or completely depending on porosity content) open macro-pores spherical in shape and irregular micro-pores in the cell walls resulting from incomplete sintering. It has been found that porosity content of the foams have no influence on the phase transformation temperatures while deformation and oxidation are severely influential. Porous TiNi alloys displayed excellent superelasticity and shape memory behavior. Space holder technique seems to be a promising method for production of porous TiNi alloys. Desired porosity level, pore shape and accordingly mechanical properties were found to be easily adjustable.

Effect of stress-assisted aging on stress induced martensitic transformation in hot-rolled Ni-rich 50.7at. Ni%-Ti alloy has been investigated. Alloys are aged freely and under 20 MPa, 100 MPa, and 200 MPa stress at 400 o C for 90 minutes. Aging procedure affected both stress-induced and thermally induced transformation behavior. Superelasticity behavior is correlated with the multistep transformation in aged Ni-rich NiTi alloys and the aging stress level is found to be effective. Relative to the free aged alloy, the alloy aged under 20 MPa exhibited a slight and the alloy aged under 100 MPa exhibited a considerable reduction, whereas the alloy aged under 200 MPa exhibited an increase in the critical transformation stress. DSC studies have shown that the transformation is multistep for freely aged and aged under 20 MPa alloys, whereas it is single step and two-step for alloys aged under 100 MPa and 200 MPa, respectively, and this has been attributed to the effect of stress on nucleation and growth rates. As a result of the different response mechanisms to the applied stress upon loading during superelasticity testing, the recovered strain amounts varied considerably depending on the aging conditions and the test temperatures.

No description available.

Kyoto University (京都大学) / 0048 / 新制・課程博士 / 博士(工学) / 甲第18986号 / 工博第4028号 / 新制||工||1620 / 31937 / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 田中 功, 教授 乾 晴行 / 学位規則第4条第1項該当