This research is aimed at understanding the effect of thermal cycles on the metallurgical and microstructural characteristics of the heat affected zone of a multi-pass pipeline weld. Continuous Cooling Transformation (CCT) diagrams of the pipeline steel grades studied (X65, X70 and X100) were generated using a thermo mechanical simulator (Gleeble 3500) and 10 mm diameter by 100 mm length samples. The volume change during phase transformation was studied by a dilatometer, this is to understand the thermodynamics and kinetics of phase formation when subjected to such varying cooling rates. Samples were heated rapidly at a rate of 400°C/s and the cooling rates were varied between t8/5 of 5.34°C/s to 1000°C/s. The transformation lines were identified using the dilatometric data, metallographic analysis and the micro hardness of the heat treated samples. Two welding processes, submerged arc welding (SAW) and tandem Metal Inert Gas (MIG) Welding, with vastly different heat inputs were studied. An API-5L grades X65, X70 and X100 pipeline steels with a narrow groove bevel were experimented with both welding processes. The welding thermal cycles during multi-pass welding were recorded using thermocouples. The microstructural characteristics and metallurgical phase formation was studied and correlated with the fracture toughness behaviour as determined through the Crack Tip Opening Displacement (CTOD) tests on the welded specimens. It was observed that SAW process is more susceptible to generate undesirable martensite-austenite (M-A) phase which induce formation of localised brittle zones (LBZ) which can adversely affect the CTOD performance. Superimposition of the multiple thermal cycles, measured in-situ from the different welding processes on the derived CCTs, helped in understanding the mechanism of formation of localised brittle zones. Charpy impact samples were machined from the two X65 and X70 grades, for use in thermal simulation experiments using thermo mechanical simulator (Gleeble). The real thermal cycles recorded from the HAZ of the SAW were used for the thermal simulations, in terms of heating and cooling rates. This is to reproduce the microstructures of the welds HAZ in bulk on a charpy impact sample which was used for impact toughness testing, hardness and metallurgical characterisation. The three materials used were showing different response in terms of the applied thermal cycles and the corresponding toughness behaviours. The X65 (a) i.e. the seamless pipe was showing a complete loss of toughness when subjected to the single, double and triple thermal cycles, while the X65 (b), which is a TMCP material was showing excellent toughness in most cases when subjected to the same thermal cycles at different test temperatures. The X70 TMCP as well was showing a loss of toughness as compared to the X65 (b). From the continuous cooling transformation diagrams and the thermally simulated samples results it could be established that different materials subjected to similar thermal cycle can produce different metallurgical phases depending on the composition, processing route and the starting microstructure.

O crescente consumo de energia produzida a partir do petróleo e do gás natural conduz a melhoria das propriedades mecânicas dos aços microligados empregados na construção dos oleodutos e gasodutos para incrementar o transporte dos recursos a menores custos e elevar a confiabilidade. O aumento do controle das diferentes fases, agregados eutetóides, microconstituintes e precipitados neste tipo de aço, garante a melhoria na resistência mecânica, tenacidade e soldabilidade. Dentro deste contexto foi realizado um trabalho de caracterização microestrutural do aço um microligado para tubos API 5L X80 em amostras de aço como recebido e em diferentes condições de resfriamento. Para o estudo da cinética das transformações de fase, o aço microligado foi submetido a ensaios de dilatometria onde foram identificadas as temperaturas e tempos de início e fim de transformação de fases, para varias velocidades de resfriamento. A partir das diferentes temperaturas e tempos obtidos, em função das taxas de resfriamento, foi possível extrair a curva de Transformação por Resfriamento Continuo (TRC). Os dados da curva TRC foram comparados com as microestruturas de cada corpo de prova por meio de microscopia óptica (MO), microscopia eletrônica de varredura (MEV), microscopia eletrônica de varredura com Field Emission Gun (FEG) e microdureza, caracterizando a evolução morfológica da matriz ferrítica, agregados eutetóides e microconstituinte austenita/martensita (MA). Para a caracterização microestrutural das amostras também foram utilizadas técnicas de análise microestrutural como, nanodureza, análise por difração de raios X em amostras obtidas por extração de precipitados, saturação magnética e microscopia de força atômica (AFM). A técnica de saturação magnética foi desenvolvida por médio de curvas de histerese medidas em um histeresígrafo com peças polares e anel de Rowland para diversas amplitudes de intensidade de campo magnético. Esta técnica permitiu a detecção da saturação magnética do aço sem tratamento térmico e a saturação máxima nos aços com tratamento térmico, o que indicou a total transformação da austenita retida. A relação das duas saturações permitiu determinar a fração de austenita retida no MA. Para as medidas de nanodureza foi utilizado um nanodurômetro acoplado ao microscópio de força atômica (AFM). As nanodurezas obtidas em diferentes grãos foram comparadas com os valores constantes na literatura para identificar as fases, agregados eutetóides e possíveis precipitados da microestrutura. / The continuous increase of energy generated from petroleum and natural gas created the need to improve the mechanical properties of microalloyed steels used in gas and oil pipelines, in order to increase their flow with smaller costs and higher reliability. The control of the different phases, morphology of microconstituents like ferrite plus carbide aggregates and precipitates in this kind of steels is essential to the improvement of mechanical strength, toughness and weldability. In this context, a work of microestrutural characterization of a microalloyed steel for API X80 pipelines was carried out both on an as-received steel sample as in samples submitted to different cooling conditions. The kinetics of austenite transformations was investigated using dilatometric experiments, identifying start and end of the phase transformations as well as the time spent temperatures for the phase transformations at each cooling rate. The temperature and time curves obtained as a function of the cooling rates allowed the determination of a Continuous Cooling Transformation curve (CCT). The data from the CCT curve was compared with the microstructures of each sample through optical microscopy (OM), scanning electron microscopy (SEM), scanning electron microscopy with Field Emission Gun (FEG) and microhardness, characterizing the morphologic evolution of the ferritic matrix, ferrite plus carbide eutectoid aggregates (perlite and bainite) and the microconstituent martensite/austenite (MA). The microestrutural characterization of the samples was performed also using different techniques of microestrutural analysis: precipitate extraction followed by Xrays diffraction analysis, magnetic saturation and atomic force microscopy (AFM) measurements. The magnetic saturation technique was developed through hysteresis curves measured with a hysteresigraph with polar pieces and Rowland ring for several ranges of magnetic field intensity. This technique allowed to detect the magnetic saturation of the steel without thermal treatment and the maximum saturation in the heat treated steels were the retained austenite has transformed. The relationship between those saturations curves allowed a determination of the retained austenite fraction in the MA microconstituent. The nanohardness was measured using a specific device coupled to a atomic force microscope (AFM). The nanohardness of different grains were compared with the hardness values from the literature in order to help identify phases and microconstituents, as well as possible precipitates.

O crescente consumo de energia produzida a partir do petróleo e do gás natural conduz a melhoria das propriedades mecânicas dos aços microligados empregados na construção dos oleodutos e gasodutos para incrementar o transporte dos recursos a menores custos e elevar a confiabilidade. O aumento do controle das diferentes fases, agregados eutetóides, microconstituintes e precipitados neste tipo de aço, garante a melhoria na resistência mecânica, tenacidade e soldabilidade. Dentro deste contexto foi realizado um trabalho de caracterização microestrutural do aço um microligado para tubos API 5L X80 em amostras de aço como recebido e em diferentes condições de resfriamento. Para o estudo da cinética das transformações de fase, o aço microligado foi submetido a ensaios de dilatometria onde foram identificadas as temperaturas e tempos de início e fim de transformação de fases, para varias velocidades de resfriamento. A partir das diferentes temperaturas e tempos obtidos, em função das taxas de resfriamento, foi possível extrair a curva de Transformação por Resfriamento Continuo (TRC). Os dados da curva TRC foram comparados com as microestruturas de cada corpo de prova por meio de microscopia óptica (MO), microscopia eletrônica de varredura (MEV), microscopia eletrônica de varredura com Field Emission Gun (FEG) e microdureza, caracterizando a evolução morfológica da matriz ferrítica, agregados eutetóides e microconstituinte austenita/martensita (MA). Para a caracterização microestrutural das amostras também foram utilizadas técnicas de análise microestrutural como, nanodureza, análise por difração de raios X em amostras obtidas por extração de precipitados, saturação magnética e microscopia de força atômica (AFM). A técnica de saturação magnética foi desenvolvida por médio de curvas de histerese medidas em um histeresígrafo com peças polares e anel de Rowland para diversas amplitudes de intensidade de campo magnético. Esta técnica permitiu a detecção da saturação magnética do aço sem tratamento térmico e a saturação máxima nos aços com tratamento térmico, o que indicou a total transformação da austenita retida. A relação das duas saturações permitiu determinar a fração de austenita retida no MA. Para as medidas de nanodureza foi utilizado um nanodurômetro acoplado ao microscópio de força atômica (AFM). As nanodurezas obtidas em diferentes grãos foram comparadas com os valores constantes na literatura para identificar as fases, agregados eutetóides e possíveis precipitados da microestrutura. / The continuous increase of energy generated from petroleum and natural gas created the need to improve the mechanical properties of microalloyed steels used in gas and oil pipelines, in order to increase their flow with smaller costs and higher reliability. The control of the different phases, morphology of microconstituents like ferrite plus carbide aggregates and precipitates in this kind of steels is essential to the improvement of mechanical strength, toughness and weldability. In this context, a work of microestrutural characterization of a microalloyed steel for API X80 pipelines was carried out both on an as-received steel sample as in samples submitted to different cooling conditions. The kinetics of austenite transformations was investigated using dilatometric experiments, identifying start and end of the phase transformations as well as the time spent temperatures for the phase transformations at each cooling rate. The temperature and time curves obtained as a function of the cooling rates allowed the determination of a Continuous Cooling Transformation curve (CCT). The data from the CCT curve was compared with the microstructures of each sample through optical microscopy (OM), scanning electron microscopy (SEM), scanning electron microscopy with Field Emission Gun (FEG) and microhardness, characterizing the morphologic evolution of the ferritic matrix, ferrite plus carbide eutectoid aggregates (perlite and bainite) and the microconstituent martensite/austenite (MA). The microestrutural characterization of the samples was performed also using different techniques of microestrutural analysis: precipitate extraction followed by Xrays diffraction analysis, magnetic saturation and atomic force microscopy (AFM) measurements. The magnetic saturation technique was developed through hysteresis curves measured with a hysteresigraph with polar pieces and Rowland ring for several ranges of magnetic field intensity. This technique allowed to detect the magnetic saturation of the steel without thermal treatment and the maximum saturation in the heat treated steels were the retained austenite has transformed. The relationship between those saturations curves allowed a determination of the retained austenite fraction in the MA microconstituent. The nanohardness was measured using a specific device coupled to a atomic force microscope (AFM). The nanohardness of different grains were compared with the hardness values from the literature in order to help identify phases and microconstituents, as well as possible precipitates.

No description available.

Non-metallic inclusions in steels are generally considered to be detrimental for mechanical properties. However, it has been recognized that certain inclusions, such as Ti-oxide and TiN, can serve as potent nucleation sites for the formation of intragranular ferrite (IGF) in low-alloy steels. The formation of IGF could improve the toughness of the coarse grained heat affected zone (CGHAZ) of weld metals. Thus, the present thesis mainly focuses on the effect of size of nucleation sites on the IGF formation. Quantitative studies on the composition, size distribution and nucleation probability for each size of the inclusions as well as the area fraction, starting temperature and morphology of an IGF have been carried out. In the present work, the Ti-oxide and TiN powders were mixed with metallic powders. The mixed powders were heated up to the liquid state and cooled with a slow cooling rate of 3.6 ºC/min. These as-cast steels with Ti-oxide and TiN additions were used to simulate the IGF formation in the CGHAZ of weld metals. Specifically, the inclusion and microstructure characteristics in as-cast steels have been investigated. The results show that the nucleant inclusion was identified as a TiOx+MnS phase in steels with Ti2O3 additions and as a TiN+Mn-Al-Si-Ti-O+MnS phase in steels with TiN additions. In addition, the TiOx and TiN phases are detected to be the effective nucleation sites for IGF formation. It is clearly shown that an increased inclusion size leads to an increased probability of IGF nucleation. This probability of IGF nucleation for each inclusion size of the TiOx+MnS inclusions is clearly higher than that of the complex TiN+Mn-Al-Si-Ti-O+MnS inclusions. In addition, the area fraction of IGF in the steels with Ti2O3 additions is larger than that of the steels with TiN additions. This result agrees with the predicted tendency of the probability of IGF nucleation for each inclusion size in the steels with Ti2O3 and TiN additions. In order to predict the effective inclusion size for IGF formation, the critical diameters of the TiO, TiN and VN inclusions, which acted as the nucleation sites of IGF formation, were also calculated based on the classical nucleation theory. The critical diameters of TiO, TiN and VN inclusions for IGF formation were found to be 0.192, 0.355 and 0.810 μm in the present steels. The calculation results were found to be in agreement with the experiment data of an effective inclusion size. Moreover, the effects of the S, Mn and C contents on the critical diameters of inclusions were also calculated. It was found that the critical diameter of the TiO, TiN and VN inclusions increases with an increased content of Mn or C. However, the S content doesn’t have a direct effect on the critical diameter of the inclusions for IGF formation. The probability of IGF nucleation for each inclusion size slightly decreases in the steel containing a higher S content. This fact is due to that an increased amount of MnS precipitation covers the nucleant inclusion surface. In the as-cast experiment, it was noted that an IGF can be formed in steels with Ti2O3 and TiN additions with a cooling rate of 3.6 ºC/min. In order to control the microstructure characteristics, such as the area fraction and the morphology of an IGF, and to investigate the starting temperature of IGF and grain boundary ferrite (GBF) formation, the dynamic transformation behavior of IGF and GBF was studied in-situ by a high temperature confocal laser scanning microscope (CLSM). Furthermore, the chemical compositions of the inclusions and the morphology of IGF after the in-situ observations were investigated by using scanning electron microscopy (SEM), electron backscatter diffraction (EBSD) and electron probe microanalysis (EPMA) which equipped wavelength dispersive spectrometer (WDS). The results show that the area fraction of IGF is larger in the steels with Ti2O3 additions compared to the steels with TiN additions, after the same thermal cycle has been imposed. This is due to that the TiOx phase provides more potent nucleation sites for IGF than the TiN phase does. Also, the area fraction of IGF in the steels is highest after at an intermediate cooling rate of 70 ºC/min, since the competing phase transformations are avoided. This fact has been detected by using a hybrid methodology in combination with CLSM and differential scanning calorimetry (DSC). In addition, it is noted that the morphology of an IGF is refined with an increased cooling rate. / <p>QC 20150325</p>

No description available.

More complex and bigger structures have increased the applicability of low alloy high strength steels due to weight and cost reductions in these projects. One of the requirements for the use of these materials is the preservation of performance after welding. Meanwhile, the norms on which the Welding Procedures Specifications (WPS) are based have not yet considered the development of modern steel and its new production process, resulting in unnecessary welding costs that diminish the profits of the application of this type of steel. This thesis aimed to develop and evaluate an experimental methodology to guide the creation and control of welding procedures for structural steel through a microstructural atlas of the heat affected zone (HAZ) in a thermomechanical control process (TMCP), 65 ksi steel (ASTM A572 Grade 65). This steel was used in the project of an industrial building for CBMM in Araxá, Minas Gerais, Brazil. It is proposed that through a microstructural atlas of a given steel, it is possible to determine the range of cooling rates that the steel may suffer during welding without affecting mechanical properties and without risking cold cracks. When comparing the microstructure of steel welds performed in field conditions, it is possible to determine the heat input range for a given process in the preparation of a WPS. The selected case study is from a high strength low alloy class 65 ksi steel (ASTM A572 Grade 65) that was used in the structure of an industrial building. The steel was produced using TMCP. The atlas was created via the construction of a continuous cooling transformation diagram using physical simulation (dilatometer and Gleeble) of the coarse grain HAZ (GCHAZ). The characterization of the simulated region was performed by metallography and mechanical tests. The microstructure of real welds made by a qualified WPS were compared to the atlas in order to certify the correct use of parameters and to validate the method. The methodology was also qualified and the potential economic benefits were quantified (based only on the reduction of consumables used and the increased availability of the welding process machine) for the selected industrial project. The mapped microstructures varied from martensite (at high cooling rates) to pearlite/ferrite with large grain size (at low cooling rates). There was remarkable prevalence of bainitic microstructure in a wide range of cooling rates, consistent with the chemical composition of the steel studied. Comparisons with real weld microstructures showed the atlas is compatible with them, and that it can more accurately describe the effective thermal cycle xi that occurs in the coarse grain region of the HAZ (other regions were not included). The application of this methodology in the development of new WPS would allow greater flexibility in the welding procedures, including welding without preheating. In this respect alone, it was possible to forecast savings of approximately R$200,000.00, 1,000 hours of processing and 172 tonnes of carbon equivalent emissions. / Estruturas cada vez mais complexas e de maiores dimensões vêm aumentando a aplicabilidade de aços de baixa liga e alta resistência, devido à redução de peso e custo dessas estruturas. Um dos requisitos para o uso desses materiais é a manutenção do desempenho após soldagem. Entretanto, as normas em que se baseiam as Especificações de Procedimentos de Soldagem (EPS) ainda não consideram aços mais modernos em termos de rota de fabricação, o que pode fazer com que custos desnecessários de soldagem minimizem os ganhos da aplicação desses aços. Este trabalho teve como objetivo o desenvolvimento e avaliação de uma metodologia para, experimentalmente, orientar a elaboração e o controle da aplicação de procedimentos de soldagem para aços estruturais, através de atlas microestrutural de regiões da zona afetada pelo calor (ZAC). Propõe-se que, através de um atlas microestrutural de um dado aço, seja possível determinar a faixa otimizada de energia de soldagem para um dado processo na elaboração e aplicação da EPS e, consequentemente, as velocidades de resfriamento que o aço possa sofrer durante a soldagem, sem perder as propriedades mecânicas e sem colocálo em risco quanto a trincas a frio. Tomou-se como estudo de caso o aço produzido por laminação controlada de classe de resistência de 65 ksi (ASTM A572 Grau 65), utilizado em um projeto de um prédio industrial na empresa CBMM. Trata-se de um aço fabricado pelo processo TMCP com resfriamento acelerado. A elaboração do Atlas se deu através da construção de um diagrama CCT, por simulação física (dilatômetro e Gleeble), da região de grãos grosseiros da zona afetada pelo calor (ZAC GG). Foram feitas caracterizações metalográficas e mecânicas das regiões simuladas. Microestruturas de soldas realizadas com EPS qualificadas foram comparadas com as do Atlas para se certificar da adequabilidade dos parâmetros utilizados e validação da abordagem. Foram realizadas ainda a qualificação e quantificação de potenciais benefícios econômicos no citado projeto industrial, obtidos pelo uso desta metodologia. As microestruturas apresentadas no mapa variavam de martensíta, para altas taxas de resfriamento, até perlita/ferrita de tamanho de grão elevado, para baixas taxas de resfriamento. Observou-se notável predominância da microestrutura bainítica em uma larga faixa de taxas de resfriamento, compatível com as propriedades e composição do aço estudado (alta soldabilidade). As comparações com as microestruturas de soldas reais mostraram que o Atlas pode descrever de forma precisa o ciclo térmico efetivamente imposto ix na ZAC GG. Concluiu-se que a aplicação desta metodologia na elaboração de novas EPS permitiria uma maior flexibilidade nos procedimentos de soldagem, admitindo inclusive soldagem sem pré-aquecimento. Em relação a não necessidade de pré-aquecimento, podese prever uma economia significante de custos e redução de emissão de gases que provocam efeito estufa. / Mestre em Engenharia Mecânica