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Este trabalho visa caracterizar a seqüência de precipitação do aço inoxidável ferrítico do tipo AISI 430 convencional, durante a etapa de laminação a quente. Esta caracterização foi realizada através do estudo de três condições industriais e de seis condições tratadas termicamente. Todas as amostras foram avaliadas por microscopia ótica e eletrônica de varredura, extração de precipitados e difração de raios-X do material como um todo e dos precipitados extraídos. Foi realizada a modelagem termodinâmica do aço utilizando-se o programa ThermoCalc® v.R aliado ao banco de dados TCFE2. Como meio de prever a cinética das transformações de fases, de modo superficial, foi realizado um ensaio de análise térmica diferencial com três taxas de resfriamento com redução progressiva (10°/min, 5°/min e 2°/min), sendo os resultados comparados com os resultados experimentais obtidos pelas demais técnicas empregadas. O aço AISI 430 convencional mostrou-se bifásico a alta temperatura, apresentando o campo bifásico (ferrita/austenita) entre 900°C e 1250°C. Após tratamentos térmicos por 5h nas temperaturas de 900°C, 1000°C e 1100°C, seguido de têmpera em água e partindo-se da condição laminado a quente e recozido (BQB), o aço apresentou microestrutura dúplex (ferrita/martensita). As amostras tratadas a 900°C e 1000°C apresentaram pequenas frações residuais de carbonetos do tipo M23C6. As amostras tratadas a 600°C, 700°C, e 800°C por 5h e temperadas em água mostraram-se ferríticas com presença de carboneto do tipo M23C6 com teores de carboneto decrescentes com o aumento da temperatura do tratamento térmico. As amostras da condição industrial e as amostras tratadas a 600°C, 700°C, 800°C e a 900°C apresentaram a presença de nitretos do tipo (Cr,Fe)2N, sendo que a amostra tratada a 900°C apresentou apenas resíduos deste nitreto, em pleno acordo com a termodinâmica computacional que prevê decomposição deste na temperatura de 866°C, indicando que a cinética de decomposição deste nitreto é lenta. A temperatura de precipitação do carboneto do tipo M23C6 rico em (Cr,Fe)23C6 foi avaliada entre 900°C e 1000°C. / This work aims to characterize the precipitation path of the conventional ferritic stainless steel AISI 430, during the hot rolling process. This characterization had been carried out with the study of three industrial conditions, and six thermal treated conditions. All the samples were evaluated by optical and scanning electron microscopy, by extraction of precipitates and X-Ray diffraction of the bulk material and of the extracted precipitates. It was done a thermodynamic modeling of the steel with the use of the ThermoCalc® v.R program and TCFE2 data base. In a way to determine the phase transformations kinetics, in a superficial way, it was carried out differential thermal analysis with three cooling rates progressively reduced (10°/min, 5°/min e 2°/min), all the results were compared wit h the experimental results got with the others techniques employed. The conventional AISI 430 steel is two-phase at high temperatures, showing a two-phase field (ferrite/austenite) between 900°C and 1250°C. After the thermal treatments for 5h, steel in the hot rolled and annealed (BQB) initial condition, at 900°C, 1000°C and 1100°C, followed by water quench, the steel showed a duplex microstructure (ferrite/martensite). The samples heat treated at 900°C and 1000°C showed a residual volumetric fraction of the M23C6 carbide. The samples heat treated for 5h at 600°C, 700°C and 800°C and water quenched showed a ferritic microstructure with the presence of M23C6 carbide, with its content decreasing with the heat treatment temperature increase. The samples in the industrial condition and the samples heat treated at 600°C, 700°C, 800°C and at 900°C showed a (Cr,Fe) 2N nitrite presence, the sample heat treated at 900°C showed only a residual volumetric fraction of it. This is in great deal with the computational thermodynamic modeling that predicts nitride decomposition at 866°C, indic ating that the nitrite decomposition kinetic is slow. The precipitation temperature of the M23C6 carbide rich in (Cr,Fe)23C6 was evaluated between 900°C and 1000°C.

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Orientador: Amauri Garcia / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia Mecanica / Made available in DSpace on 2018-08-04T03:14:59Z (GMT). No. of bitstreams: 1 Ferreira_IvaldoLeao_D.pdf: 8636771 bytes, checksum: fb3623e9e0a9c93143f4b34ba87844cf (MD5) Previous issue date: 2004 / Resumo: o presente trabalho analisa as influências do teor de soluto, do superaquecimento e do coeficiente global de transferência de calor metal/fluido (hg), na macrossegregação inversa durante a solidificação unidirecional vertical ascendente de ligas binárias AI-Cu e ternária AI-Cu-Si. Os perfis experimentais de segregação ao longo dos lingotes para as ligas AI4,5%Cu, AI-6,2%Cu, AI-8,I%Cu e Al-8,I%Cu-3%Si são comparados com as predições teóricas fomecidas por modelos numérico e analítico, com perfis transitórios de (hg) sendo determinados em cada experimento. O modelo analítico é baseado num modelo analítico de transferência de calor [Garcia, 2001], acoplado a uma formulação clássica para a redistribuição local de soluto proposta por Flemings e Nereo (Flemings e Nereo, 1967]. O modelo numérico é aquele proposto por V oller [V oller, 1997], com modificações introduzidas levando em consideração diferentes propriedades termofisicas para as fases líquida e sólida, coeficiente global de transferência de calor metal/fluido variável com o tempo e malha com distribuição de comprimento de nós variável ao longo do domínio, o que garantiu a precisão dos resultados sem aumento excessivo do número de nós. AIém dessas modificações, fez-se necessária à mudança no critério de convergência para melhor representar os gradientes térmicos e taxas de resfriamento. Um modelo semi-analítico para a macrossegregação inversa, baseado na solução por variável de similaridade, é aplicado para validação do modelo numérico. Observa-se que as predições numéricas apresentam boa concordância com as medidas experimentais, e que as predições analíticas, apesar de sua relativa simplicidade, também é capaz de representar satisfatoriamente os resultados experimentais, exceto para condições de elevado superaquecimento. O modelo numérico é aplicado com sucesso para a situação de solidificação de ligas multicomponentes, representada pela liga Al-8,1%Cu-3%Si, onde é observada boa representatividade dos resultados experimentais / Abstract: The present work focuses on the influences of alloy solute content, melt superheat, and meta1/fluid heat transfer coefficients on inverse segregation during upward solidification of AI-Cu and AI-Cu-Si alloys. The experimental segregation profiles of AI4,5 wt % Cu, AI-6,2 wt % Cu, AI-8,1 wt % Cu and AI-8,1 wt % Cu-3 wt % Si alloys are compared with theoretical predictions fumished by analytical and numerica1 models, with transient (hg) profiles being determined in each experimento The analytical model is based on an ana1ytica1 heat transfer model coupled with the classica1loca1 solute redistribution equation proposed by Flemings and Nereo. The numerica1 model is that proposed by V oller, with some changes introduced to take into account different thermophysica1 properties for liquid and solid phases, time variable meta1/fluid interface heat-transfer coefficient, and a variable space grid along the domain in order to assure the accuracy of results without raising the number of nodes. Furthermore, changes in the convergence criterion were necessary to improve the accuracy of the therma1 gradients and solidification rates ca1culated numerlcally. A sophisticated semi-ana1ytica1 solution for the inverse segregation based on the similarity variable is carried out to valida te the numerica1 model. It is observed that the numerical predictions generally conform with the experimental segregation measurements and that the predicted analytical segregation, despite its simplicity, also compares favorably with the experimental scatter except for high melt superheat. The numerical model is successfully applied for a situation of multicomponent alloy solidification, Le., AI-8,1 wt % Cu-3 wt % Si alloy, and it is found be in good agreement with experimental results / Doutorado / Materiais e Processos de Fabricação / Doutor em Engenharia Mecânica

No presente trabalho verificou-se a precisão de um critério que prevê composições de ligas vítreas aplicado ao sistema Zr-Ni-Cu. Este critério combina o parâmetro de instabilidade topológica (\'lâmbda\'), e o parâmetro termodinâmico (\'delta\' h) entre os elementos de liga. Os dois parâmetros correlacionam quantitativamente à composição química a tendência à formação de vidros metálicos. Este critério é uma ferramenta promissora e simples para guiar e reduzir o trabalho tedioso e intensivo de encontrar composições altas tendências a vitrificação em sistemas metálicos. Para comprovar a eficiência desta ferramenta, a metodologia foi calcular o parâmetro para o sistema de interesse e preparar ligas de acordo com algumas composições fornecidas. A metodologia de preparação das ligas seguiu a fusão a arco elétrico e subsequentemente o emprego das técnicas de resfriamento rápido, melt-spinning e splat-cooling, para a produção de fitas e discos metálicos respectivamente, e o coquilhamento para a produção de amostras maciças em forma de cunha. Para as amostras confeccionadas por melt-spinning e splat-cooling, verificou-se a precisão do critério de seleção através da quantificação das porcentagens de fases vítreas a partir de análises de difratogramas de raios-X e seus comportamentos térmicos a partir dos termogramas de análises por calorimetria exploratória diferencial (DSC). Já para as ligas coquilhadas em cunha, obtiveram-se alguns resultados com indícios de estruturas vítreas que foram caracterizadas por difração de raios-X e metalografia. Desta forma chegou-se à conclusão que o critério de seleção aplicado ao sistema Zr-Ni-Cu pode ser utilizado para o desenvolvimento de composições favoráveis à formação de vidro antes da produção das ligas. Conclui-se que o critério que combina o parâmetro de instabilidade topológica (\'lâmbda\' min) e o parâmetro termodinâmico (\'delta\' h) é uma ferramenta que pode ser utilizada como guia para encontrar as composições mais fáceis de formar vidro, reduzindo assim o trabalho experimental de tentativa e erro. / In the present work it was verified the accuracy of a proposed criterion to predict compositions of glassy alloys applied in the Zr-Ni-Cu system. This criterion combines the topological instability parameter (\'lâmbda\') and a thermodynamic parameter (\'delta\' h) among the alloying elements. The two parameters correlate quantitatively the chemical composition with the glass forming ability. This criterion is a promising and simple tool to guide and reduce the tedious and intensive work of finding good compositions of glasses in metallic systems. In an attempt to prove the efficiency of such tool, the methodology was to calculate the parameter for the system of interest and prepare alloys in accordance with the compositions provided by the tool. The methodology of preparation of the alloys followed the electric arc- melting and subsequent use of fast cooling techniques, melt-spinning and splat-cooling for the production of metallic ribbons and discs, respectively, and a wedge-shaped chiller mold to produce bulk metallic samples. For samples prepared from the melt-spinning and splat-cooling, it was verified the accuracy of the selection criteria by quantifying the percentage of glassy phases from X-ray diffractograms and their thermal behaviors from thermograms produced by differential scanning calorimetry (DSC). For alloys produced from the wedge-shaped mold, some results were obtained with evidence of vitreous structures that were characterized by X-ray diffraction and metallography. Therefore the conclusion is that the selection criteria applied to the system Zr-Ni-Cu can be used to develop favorable compositions for the formation of glasses before the production of the alloys. It is concluded that the selection criterion is a good tool and can be used as a guide to find the best glass forming alloys, thus reducing the experimental procedures of trial and error.

No description available.

Casting, Solidification, Aluminum, Physical Metallurgy, Mechanical Metallurgy, Strengthening Model, Aluminum Wrought Alloys, Aluminum 7xxx Series, Al-Zn-Mg-Cu / Over the past decades, researchers in casting fields, especially in semi-solid metal state, have endeavored to find new ways to enable the Al wrought alloys of casting using the conventional casting processes; mainly in order to improve the product properties and decrease the product cost. The thixoforming and rheocasting processes have been presented as ways by which the microstructure of Al-base wrought alloys can be changed into non-dendritic, which in turn can lead to improvement to the mechanical properties. This can be because the effect of the non-dendritic microstructure on the mechanical properties of the material. Unfortunately, these processes have proved to be cost prohibitive and be a bit complicated for commercial applications. Further, conventional casting of Al-base wrought alloys along with their superior properties and performance have been a challenge for foundry industry due to the main disadvantage of hot tearing or hot cracking during solidification process. This can render the cast component ineffective. To overcome the disadvantages of thixoforming and rheocasting processes, Controlled Diffusion Solidification (CDS) process was innovated mainly to enable casting of aluminum wrought alloys with a non-dendritic morphology of the primary Al phase in the resultant cast microstructure and thus alleviating the problem of hot tearing and obtaining a cost effective product with improved mechanical properties. The CDS is a simple process involving mixing of two precursor alloys of different thermal masses (temperature and solute) and subsequently casting the resultant mixture of the desired solute composition and temperature as a near net shaped cast product. The process can easily be commercialized with a marginal capital cost required for set up such as the addition of an extra holding furnace. Further, the CDS process would prove itself to be unique in its ability to cast Al-based wrought alloys into near net shaped components without additional processes and cost. The originality of this study is to present a viable casting process for the Al-7xxx wrought alloys (Al-Zn-Mg-Cu); by which the Al-7xxx family alloys are presented in cast condition to have an acceptable uniaxial property range that is comparable with their wrought counterparts. This study presents the process and alloy parameters necessary for the casting of Al-7xxx wrought alloys (Al-Zn-Mg-Cu), by using the CDS process coupling with tilt pour gravity casting (TPGC) machine. The uniaxial tensile mechanical properties of several Al-7xxx CDS castings under various heat treatment conditions, namely, solutionizing (T4), peak aged (T6) and annealing (O), necessary for development of an ageing process on the material were investigated and presented. The tilt pour gravity casting process coupled with the CDS technology was employed to demonstrate the ability to cast Al-7xxx wrought alloys into high integrity components with high strength and ductility. The microstructure characterization was carried out by Electron Microscopy (TEM, SEM and EDS) and DSC test experiments for all the as cast (F), T4, T6 and anneals (O) conditions of the CDS cast components. Also, the predictive capabilities for the yield strength of Al 7xxx alloys CDS cast components was investigated using structural-properties modeling for the various strengthening effects that are recently proposed specifically for the Al-7xxx wrought counterparts. The study has successfully led to a more in-depth understanding of the innovative CDS casting process by applying it to several compositions of Al-7xxx wrought alloys in an industrial scale CDS casting experiments, using tilt pour gravity casting (TPGC) machine. This will hopefully lead us to a clearer path towards commercializing the CDS process and obtaining a viable casting process for Al-base wrought alloys into near net shape components without much change to economics of the casting process. / Dissertation / Doctor of Philosophy (PhD) / Casting, Solidification, Aluminum, Physical Metallurgy, Mechanical Metallurgy, Strengthening Model, Aluminum Wrought Alloys, Aluminum 7xxx Series, Al-Zn-Mg-Cu

The factors controlling the reliability of Pb-free solders when subject to thermomechanical regimes relevant to the harsh aerospace environment have been studied. Ball grid array (BGAs) typical of microelectronic devices have been manufactured in-house and subjected to isothermal ageing and thermal cycling. The BGAs comprised both Cu and Ni-Au metallizations, Pb-free Sn-Ag-Cu 400 and 600μm solder balls, FR4 and Al₂O₃ boards, and included circuits to measure resistance changes due to damage in the joints during thermal cycling. Microstructural evolution within the solders balls and complex interfacial reactions were studied in all configurations using various types of electron microscopy. The mechanical properties of the different phases formed within solder joints were studied using nanoindentation at room and elevated temperatures up to 175°C for the first time. Intermetallic compounds (IMCs) were stiff, hard and brittle with very low creep rates, while the softer primary Sn, eutectic regions and Cu metallization readily underwent creep. Two-dimensional finite element analysis (FEA) of nanoindentation was used to understand better the physical meaning of nanoindentation creep data. Reliability experiments comprised both thermal cycling and FEA of BGAs. The difference in coefficient of thermal expansion (CTE) in the BGA materials caused interfacial fatigue damage in the solder joints, which was detected primarily at the solder/metallization interface of the outermost, most strained solder joint. Accumulated creep strain per cycle at this interface was evaluated using 3D FEA of the stress-strain state of the BGA and results calibrated against experimental BGA mean lifetimes using the Coffin-Mason relationship. Nanoindentation combined with FEA has been shown to be a viable route for the rapid assessment of creep performance and lifetime in lead-free solders under aerospace thermal cycles.

A liga de alumínio designada AA4006 é muito utilizada na indústria. É uma liga do sistema Al-Fe-Si, com teores (% em massa) de Si na faixa de 0,8 a 1,2% e Fe entre 0,5 e 0,8%. Apesar de ser bastante utilizada, ela foi pouco estudada. Neste trabalho foi realizado um estudo comparativo da microestrutura e da textura cristalográfica entre chapas da liga AA4006 produzidas por dois processos industriais de lingotamento: contínuo (Twin roll caster TRC) e semicontínuo (Direct chill DC). Para a caracterização microestrutural, foram utilizadas as técnicas de microscopia óptica com luz polarizada, microscopia eletrônica de varredura com microanálise química, medidas de condutividade elétrica e ensaios de dureza Brinell. A textura cristalográfica foi determinada por difração de raios X. Foram detectadas e discutidas diferenças significativas nas morfologias e distribuições de grãos e de partículas de fases intermetálicas. O estudo da textura cristalográfica foi realizado ao longo da espessura das tiras e os resultados mostraram variações significativas da textura entre as chapas ao longo da espessura. A chapa produzida por lingotamento contínuo apresentou uma típica textura de cisalhamento nas proximidades de sua superfície, enquanto nas regiões mais internas a fibra foi observada. O estudo da recristalização de chapas metálicas laminadas a frio é muito útil para a obtenção da temperatura de amolecimento do material submetido a um tratamento térmico. Tratamentos térmicos isócronos no intervalo de uma hora foram feitos em amostras das duas chapas e a chapa produzida pelo processo TRC apresentou a temperatura para 50% de recristalização em torno de 290 ºC e a amostra da chapa produzida pelo processo DC em torno de 270 ºC. A textura cristalográfica pode mudar com a recristalização e com a laminação do metal. Utilizando estas etapas de processamento do material, a orientação dos grãos de uma tira metálica pode ser otimizada, a fim de, por exemplo, melhorar a estampabilidade de chapas na obtenção de um dado produto com valor agregado. Neste trabalho as curvas de amolecimento para duas chapas produzidas por lingotamento contínuo e lingotamento semicontínuo da liga de alumínio AA4006 também foram determinadas e comparadas. Embora as diferenças detectadas entre as curvas de amolecimento tenham sido pequenas, foi possível verificar que a recristalização da chapa produzida por twin roll caster TRC ocorre em temperaturas mais elevadas do que na chapa produzida pelo processo direct chill DC. Resultados da textura cristalográfica em amostras destas chapas (laminadas e recozidas) foram obtidos utilizando difração de raios X e difração de elétrons retroespalhados EBSD. Estes resultados indicaram a presença da textura de cisalhamento na superfície e a fibra no centro da amostra laminada a frio (70% de redução) da chapa obtida por lingotamento contínuo. Na amostra da chapa obtida por lingotamento semicontínuo, a componente cubo e a fibra foram vistas na superfície e no centro. Uma textura fraca com grãos orientados ao acaso foi vista nas duas amostras (TRC e DC) recristalizadas das duas chapas, possivelmente, devido à nucleação estimulada por partículas. A fibra desapareceu nas amostras (TRC e DC) recristalizadas. / AA4006 Aluminum alloy is extensively used in industry. It belongs to the Al-Fe-Si system, with Si between 0,8 and 1,2 % mass, and Fe between 0,5 and 0,8 % mass. This alloy is less studied despite its extensive use. A comparative microstructural study has been performed in as-received AA4006 alloy strip produced by two industrial casting processes: twin roll caster (TRC) and direct chill (DC). Polarized optical microscopy, scanning electron microscopy with microanalysis, electrical conductivity measurements and Brinnel hardness tests have been used for microstructural characterization. Significant differences in the grain and intermetallic particle sizes, morphologies and distributions were detected and are discussed. Thermal treatments effects on the silicon content in solid solution were also studied. Crystallographic textures have been also determined. Textures across thickness of both sheets have been analyzed and compared. Results showed significant texture changes across thickness of the specimens. Texture analysis was carried out using X-ray diffraction technique. Twin roll caster (TRC) sheet presented the typical shear texture near the surface, while, in internal regions, the -fibre was observed. A recrystallization study of cold rolled metallic sheets is very important to obtain softening temperature for the material during annealing. After cold rolling with 70% of reduction in thickness, followed by isochronous heat treatments, the samples of the two sheets produced by TRC and DC presented a 50% recrystallization temperature around 290 ºC and 270 ºC, respectively. Crystallographic texture can change during the metal rolling and recrystallization. These processing steps can optimize the grain orientation distribution in a metal strip to improve, for instance, the stamping process, in order to obtain an aggregated value product. Softening curves were also compared and determined for the two sheets (rolled and annealed) of the AA4006 aluminum alloy produced by twin roll caster TRC and direct chill DC processes. It was detected that the recrystallization of the strip produced by TRC process occurs at a higher temperature than that for the DC process, despite the little differences in their softening curves. Crystallographic texture results, for the sheet samples, were obtained by using X-ray diffraction and electron back scatter diffraction EBSD techniques. These results indicated the shear texture presence on the surface and fiber at the center of the cold rolled (70% area reduction) sample for the sheet produced by TRC process. In the sheet sample produced by the DC process, under the same conditions, the cube component and fiber texture (at the surface and at the center) were observed. A texture with random oriented grains was detected in two deformed and recrystallized samples of the two sheets (TRC and DC). It is suggested that this texture occurs due to the particle stimulated nucleation. There was fiber absence in the recrystallized samples (TRC and DC).

The processes leading to the retention of small quantities of austenite following the bainite and martensite phase transformations have been examined, together with the influence of retained austenite on the properties of low alloy steels. It was found that the upper and lower bainite transformations are separate reactions, although both involve a displacive transformation mode, Growth seems to occur by the repeated nucleation of martensitic sub-units, and this leads to an apparently slow growth rate, The partitioning of carbon from bainitic ferrite into residual austenite was thermodynamically proven to occur subsequent to transformation, and was shown to be directly responsible for the 'incomplete reaction phenomenon'. The nature of sympathetic nucleation and of the limited size of bainitic sub-units was rationalised in terms of the relatively low driving force available for bainite transformations. It was shown that the retention, stability and morphology of austenite could be directly derived from the basic transformation mechanism. Under certain circumstances, the bainitic retained austenite conferred exceptional strength/toughness properties to silicon steels; these were· shown to be superior to the properties associated with tempered martensite microstructures, Using thermodynamics, a model was established which could predict the toughness behaviour of silicon steel bainites simply from a knowledge of the composition. The tempered martensite embrittlement phenomenon was not found to be directly linked to the decomposition of retained austenite films, but to the coarsening of inter- or intra-lath carbides. In dislocated martensites, it was found that the distribution and quantity of retained austenite could be rationalised in terms of the degree of accommodation between adjacent martensite variants. The incipient twins generally observed in lath martensites were shown to be accommodation defects such that the extent of twinning was the greatest when adjacent martensite units had twin-related lattices. The thermodynamics of dislocated martensites have been briefly examined, The inhomogeneous deformation behaviour of dual-phase steels has been analysed in terms of available models.