Os aÃos inoxidÃveis austenÃticos tÃm sido bastante utilizados em equipamentos de utilidades de dessulfurizaÃÃo de petrÃleo devido à sua boa resistÃncia à corrosÃo em temperatura elevada.Contudo, esses materiais estÃo sujeitos a sensitizaÃÃo (deficiÃncia em cromo na regiÃo vizinha ao contorno de grÃo) quando expostos a temperaturas de 425 a 815ÂC, durante a operaÃÃo ou processos de fabricaÃÃo. A sensitizaÃÃo torna o equipamento suscetÃvel à corrosÃo sob tensÃo causada por aÃos politiÃnicos, formados pela interaÃÃo de compostos sulforoso, umidade e ar em temperatura ambiente. A resistÃncia à corrosÃo sob tensÃo de amostras de aÃo inoxidÃvel austenÃtico AISI 321 e 347, removidas de um tubo, foi investigada atravÃs do procedimento ASTM 262 Pr. E â ensaio alternativo e de execuÃÃo mais fÃcil do que a simulaÃÃo dos aÃos politiÃnicos. Os corpos de prova foram submetidos aos tratamentos tÃrmicos de estabilizaÃÃo (900ÂC, durante 75 minutos) e de sensitizaÃÃo (600ÂC, durante 20, 40, 80, 120 e 140 horas), apÃs o que foram expostos ao meio corrosivo de CuSO4 + H2SO4 durante 72 horas e depois dobradas, nÃo apresentando trincamento. A agressividade do meio utilizado no ensaio foi verificada atravÃs da utilizaÃÃo de amostras de aÃo AISI 304L sensitizadas (600ÂC, 24, 28 e 72 horas e 677ÂC durante 4, 45 e 72 horas). Neste caso, somente as amostras com acabamento superficial feito com lixa n 100 sofreram um intensivo processo corrosivo. / Os aÃos inoxidÃveis austenÃticos tÃm sido bastante utilizados em equipamentos de utilidades de dessulfurizaÃÃo de petrÃleo devido à sua boa resistÃncia à corrosÃo em temperatura elevada.Contudo, esses materiais estÃo sujeitos a sensitizaÃÃo (deficiÃncia em cromo na regiÃo vizinha ao contorno de grÃo) quando expostos a temperaturas de 425 a 815ÂC, durante a operaÃÃo ou processos de fabricaÃÃo. A sensitizaÃÃo torna o equipamento suscetÃvel à corrosÃo sob tensÃo causada por aÃos politiÃnicos, formados pela interaÃÃo de compostos sulforoso, umidade e ar em temperatura ambiente. A resistÃncia à corrosÃo sob tensÃo de amostras de aÃo inoxidÃvel austenÃtico AISI 321 e 347, removidas de um tubo, foi investigada atravÃs do procedimento ASTM 262 Pr. E â ensaio alternativo e de execuÃÃo mais fÃcil do que a simulaÃÃo dos aÃos politiÃnicos. Os corpos de prova foram submetidos aos tratamentos tÃrmicos de estabilizaÃÃo (900ÂC, durante 75 minutos) e de sensitizaÃÃo (600ÂC, durante 20, 40, 80, 120 e 140 horas), apÃs o que foram expostos ao meio corrosivo de CuSO4 + H2SO4 durante 72 horas e depois dobradas, nÃo apresentando trincamento. A agressividade do meio utilizado no ensaio foi verificada atravÃs da utilizaÃÃo de amostras de aÃo AISI 304L sensitizadas (600ÂC, 24, 28 e 72 horas e 677ÂC durante 4, 45 e 72 horas). Neste caso, somente as amostras com acabamento superficial feito com lixa n 100 sofreram um intensivo processo corrosivo. / Because of their resistance to high temperature corrosion by hydrogen sulfide, austenitic stanless steels are commonly used for equipment in desulfurization process. However, these materials are subject to sensitization (chromium carbide precipitation) from exposure in the temperature range 425 to 815ÂC during fabrication or operation. Sensitization makes the equipment susceptible to failure from intergranular stress corrosion cracking caused by polythionic acid. Polythionic acid is formed by sulfur compounds, moisture, and air at ambient temperature. The main goal of the present work is to investigate the stress corrosion cracking susceptibility of stainless steels AISI 321 and 347 in polythionic acids using an alternative process that is to submit the samples to cooper-cooper sulfate-16% sulfuric acid test (ASTM A262 Pr.E). After the stabilization heat treatment at 900ÂC for 75 minutes, samples were heat treated at 600ÂC during 20, 40, 80, 120 and 140 hours and then exposed to boiling acidified copper sulfate solution for 72 hours. After exposure, the specimens were bent. The appearance of fissures or cracks was not observed in AISI 321 and 347 samples. The effectiveness of the solution has been made by submitting AISI 304L samples to the same environment . The AISI 304L samples with higher finishing have been cracked. The ones with fine-ground finishing have not been attacked. / Because of their resistance to high temperature corrosion by hydrogen sulfide, austenitic stanless steels are commonly used for equipment in desulfurization process. However, these materials are subject to sensitization (chromium carbide precipitation) from exposure in the temperature range 425 to 815ÂC during fabrication or operation. Sensitization makes the equipment susceptible to failure from intergranular stress corrosion cracking caused by polythionic acid. Polythionic acid is formed by sulfur compounds, moisture, and air at ambient temperature. The main goal of the present work is to investigate the stress corrosion cracking susceptibility of stainless steels AISI 321 and 347 in polythionic acids using an alternative process that is to submit the samples to cooper-cooper sulfate-16% sulfuric acid test (ASTM A262 Pr.E). After the stabilization heat treatment at 900ÂC for 75 minutes, samples were heat treated at 600ÂC during 20, 40, 80, 120 and 140 hours and then exposed to boiling acidified copper sulfate solution for 72 hours. After exposure, the specimens were bent. The appearance of fissures or cracks was not observed in AISI 321 and 347 samples. The effectiveness of the solution has been made by submitting AISI 304L samples to the same environment . The AISI 304L samples with higher finishing have been cracked. The ones with fine-ground finishing have not been attacked.

[pt] Os aços inoxidáveis Duplex são materiais metálicos que tendem a aliar uma excelente resistência à corrosão em meios agressivos com elevada resistência mecânica devido à sua microestrutura bifásica. Essa microestrutura é composta por uma matriz ferrítica e ilhas de austenita, a temperatura ambiente, com frações volumétricas aproximadamente iguais dessas duas fases. Com isso, estas ligas costumam ser utilizadas em tubulações e equipamentos industriais onde se requer elevada relação resistência/peso, especialmente em empreendimentos de construção e montagem off-shore. Este trabalho apresenta uma metodologia desenvolvida com a utilização de um modelo numérico parametrizado baseado no método de elementos finitos para analisar o efeito dos ciclos térmicos de soldagem nos aços duplex e leanduplex. O modelo desenvolvido faz uso da análise térmica transiente da soldagem, em que as propriedades térmicas dos materiais envolvidos são termo dependentes, e grandes gradientes térmicos são gerados entre a região da solda e as áreas afastadas dela. Procedimentos experimentais para medição dos ciclos térmicos empregados sob determinados regimes de soldagem são utilizados para calibrar o modelo numérico. A metodologia é aplicada ao estudo do comportamento de uma solda na forma de cordão sob chapa contendo um único passe, realizada com o processo GMAW, em chapas planas de 10mm de espessura dos aços duplex UNS32205 e leanduplex UNS32304, através de um modelo de elementos finitos. Os resultados mostram uma boa correspondência entre o modelo numérico e o resultado experimental. / [en] Duplex stainless steels are metallic materials that tend to combine excellent corrosion resistance in aggressive environment with high mechanical strength due to their biphasic microstructure. This microstructure is composed of a ferritic matrix and austenite islands, at room temperature, with approximately equal volume fractions of these two phases. As a result, these alloys are often used in pipes and industrial equipment where high resistance / weight ratio is required, especially in offshore assembly and construction field. This work presents a methodology developed with the use of a parameterized numerical model based on the finite element method to analyze the effect of thermal welding cycles on duplex and leanduplex stainless steels. The developed model uses the transient thermal analysis of welding, in which the thermal properties of the materials involved are thermo-dependent, and large thermal gradients are generated between the region of the weld and the areas away from it. Experimental procedures for measuring the thermal cycles employed under certain welding conditions are used to calibrate the numerical model. The methodology is applied to the study of the behavior of a weld in the form of a strand in sheet form containing a single pass, realized with the GMAW process, in flat plates of 10mm thickness of the duplex steels UNS32205 and leanduplex UNS32304, through a finite element model. The results show a good correspondence between the numerical model and the experimental result.

A disputa por espaço no mercado automotivo tem sido intensificada a cada ano. A cobrança por componentes mais leves e de menor custo aliados à preocupação ambiental têm exigido a busca de novas alternativas de materiais e/ou processos produtivos mais eficientes. Uma das respostas a estas tendências é o aumento significativo no uso de aços de alta resistência baixa liga e dual phase nos últimos anos a fim de reduzir peso dos componentes. Entretanto, o custo destes aços no Brasil está entre 20 a 40% maior que os aços baixo carbono. Desta forma, para alguns segmentos está descartada esta hipótese, pois o mercado brasileiro exige redução de peso aliada à redução de custo. Sendo assim, a melhoria do processo produtivo ganha força nesta disputa. O processo de repuxamento (spinning) tem sido utilizado há anos para produção do componente disco de rodas para veículos comerciais e é um processo de trabalho à frio severo, o que pode resultar em aumento das propriedades mecânicas do material e redução do uso de matéria-prima em função da porcentagem da redução de espessura proposta. Sendo assim, neste trabalho foram analisadas 3 condições de repuxamento de disco, 41% de redução de espessura, 52% de redução de espessura e 64% de redução de espessura a fim de se obter o limite de redução de espessura do material S355JR por meio do processo de repuxamento do disco sem que haja perda das propriedades mecânicas do mesmo e, assim, gerar aumento da vida em fadiga do componente roda e redução de peso. Para isso, foram realizados os seguinte ensaios: análise de composição química, análise de microdureza, análise metalográfica, ensaios de tração e obtenção das curvas tensão x deformação, ensaios de fadiga por flexão alternada (R=-1,0) e obtenção das curvas S-N. A análise da composição química do aço S355JR verificou que o mesmo atende o especificado em norma DIN EN-10025-2. Por meio da análise metalográfica foi verificado que as fases presentes nos materiais analisados eram ferrita e perlita dispersa na matriz e nos contornos de grão. Através dos ensaios realizados foi observado que houve aumento das propriedades mecânicas do material para as amostras repuxadas e também aumento na vida em fadiga dos mesmos. Além disso, foi observado aumento das propriedades mecânicas e da vida em fadiga para a amostra com maior porcentagem de redução de espessura. / The battle for space in the automotive market is becoming fiercer. Calls for lighter and cheaper components, and also environmental concerns, have led to the search for alternative materials and more effective processes. One of the answers is the recent significant increase in sales of dual phase and high strength low alloy steel, which has reduced the weight of the products. However, in Brazil, the price of these steels is 20% to 40% higher than low carbon steel price and thus it is necessary to look for other options. On this way, for some segments this hypothesis is ruled out because the Brazilian market requires weight reduction combined to cost reduction. Thus, the improvement of the manufacturing process gains strength in this battle. The spinning process has long been used to make the disc of commercial vehicle wheels. It is a hard cold working process which could achieve an improvement of the material mechanical properties and a raw material reduction based on the thickness reduction during the process. Thus, three spun disc conditions were analyzed, corresponding to 41, 52% and 64% of thickness reduction, in order to find out a reasonable limit of thickness reduction with no loss of the material mechanical properties, purposing to increase the fatigue life of the wheel and reducing the wheel weight. The following tests were carried out: chemical composition analysis, metallographic analysis, tensile tests to obtain the stress v strain curves, and fatigue tests by alternated bending (R=-1.0) to obtain the S-N curves. The chemical composition analysis of the S355JR steel proved that it met the DIN EN10025-2 standard. Through metallographic analysis, it was confirmed that, for S355JR steels, whose microstructure is ferrite and perlite, the perlite was near the grain boundaries. Throughout the realized tests, it was observed that there was an increasing of the mechanical properties and the fatigue life of the spun samples. In addition, the mechanical properties and fatigue life of the sample with 64% of thickness reduction had increased more than the others spun samples had.

Grade 91 (Gr.91) is a common structural material used in boiler applications and is favored due to its high temperature creep strength and oxidation resistance. Under cyclic stresses, the material will experience creep deformation eventually causing the propagation of type IV cracks within its heat-affected-zone (HAZ) which can be a major problem under short-term and long-term applications. In this study, we aim to improve this premature failure by performing a computational thermodynamic study through the Calculation of Phase Diagram (CALPHAD) approach. Under this approach, we have provided a baseline study as well as simulations based on additional alloying elements such as manganese (Mn), nickel (Ni), and titanium (Ti). Our simulation results have concluded that high concentrations of Mn and Ni had destabilized M23C6 for short-term creep failure, while Ti had increased the beneficial MX phase, and low concentrations of nitrogen (N) had successfully destabilized Z-phase formation for long-term creep failure.

<p>The goal of this work has been to evaluate the different experimental techniques used for quantitative analysis of multi-phase materials systems. </p><p>Powder based specimens containing two-phases, austenite and ferrite , were fabricated and quantified. The volume fraction of ferrite varied from 2 Vol% to 50 Vol%. </p><p>X ray powder diffraction (XRD) measurements were based on two peak analysis. Computer based software Topas was used for quantitative analysis, which is believed to be the most advanced in this field. XRD results were found within the absolute limit of +/- 4% of given ferrite volume fraction. Volume fraction as low as 2 Vol% was successfully detected and quantified using XRD. However, high statistical error was observed in case of low volume fraction, such as 2 Vol% and 5 Vol% ferrite volume fraction. </p><p>Magnetic balance (MB) measurements were performed to determine the volume fraction of magnetic phase, ferrite. MB results were found in good agreement with given volume fractions. As low as 2 Vol% volume fraction was detected and quantified with MB. MB results were within the absolute limit of +/- 4% of given ferrite volume fraction. </p><p>Image analysis (IA) was performed after proper sample preparation as required by electron backscatter diffraction (EBSD) mode of Scanning electron microscopy (SEM). IM results were found within the absolute limit of +/- 2 % of given ferrite volume fraction. However, high statistical error was observed in case of 2 Vol% volume fraction.</p>

For ecological reasons, the current main challenge of the automotive industry is to reduce the fuel consumption of vehicles and then emissions of greenhouse gas. In this context, steelmakers and automotive manufacturers decided for some years now to join their efforts to promote the development and use of advanced high strength steels such as TRIP steels. A combination of high strength and large elongation is obtained thanks to the TRansformation Induced Plasticity (TRIP) effect. However, improvement of the mechanical properties is still possible, especially by the refinement of the matrix. In this work, two main ways were followed in order to reach improved properties. The classical way consisting of the annealing of cold-rolled samples and an innovative way consisting of obtaining the desired microstructure by direct hot rolling of the samples. In the classical way, this refinement can be obtained by acting on the chemical composition (with such alloying elements like Cu and Nb). It was observed that complete recrystallisation of the ferrite matrix is quite impossible in presence of Cu precipitates. In addition, if the ferrite recrystallisation is not completed before reaching the eutectoid temperature, the recrystallisation will be slowed down by a large way. An innovative heat treatment consisting in keeping the copper in solid solution in the high-Cu steel was developed. Therefore, ferrite recrystallises quite easily and very fine ferrite grains (~1µm) were obtained. In the innovative way, the effects of hot-rolling conditions on TRIP-assisted multiphase steels are of major importance for industrial practice and could open new dimensions for the TRIP steels (i.e. thanks to precipitation mechanisms leading to additive strengthening). Impressive mechanical properties (true stress at maximum load of 1500 MPa and true strain at uniform elongation of 0.22) were obtained with a relatively easy thermomechanical process, the role played by Nb being essential.

In this thesis 9-12 % Cr steels, used for high-temperaturecomponents in fossil-fired power plants are considered. Thecreep strength of thees steels depend on their microstructurethat consists of a matrix of tempered lath martensite withdensely distributed precipitates. The mechanical properties arestrongly influenced by precipitates present in the matrix andthe more densely distributed they are the higher is thehardening effect. These particles nucleate, grow and coarsenduring use in power plants, leading to a degradation ofmechanical properties. In this thesis the nucleation andcoarsening behaviour of the precipitates in the Cr steels aresimulated by new models and the results are compared withtransmission electron microscopy (TEM) observations of testedmaterials. A model of the nucleation of MX, which mainly isvanadium-nitrides, is presented. MX precipitates are assumed tonucleate on dislocations during annealing. The model takes intoaccount the full multicomponent thermodynamical behaviour ofthe system as well as the strain energy caused by a puredilatoric strain and the shape of the nucleus. The calculationsyield a critical size and shape represented by an oblatespheroid with a radius of a few nanometers and a thickness ofan atomic layer. This is in agreement with TEM observations ofsupercritical particles. A new coarsening model, which takes into account themulticomponent effects, is presented and it has been tested ondifferent systems to validate the model.     Four different carbides, Cr7C3, Mo6C, VC and NbC, in austenitic matrix as well asγ ' in ternary Ni-base super-alloy systems (Ni-Al-Mo)were compared with measurements from literature.     TiC-particles in austenitic stainless steel, ASTM 316Ti,were considered. The simulations were performed taking intoaccount iron and 7 alloying elements. The measurements wereperformed with TEM on samples that had been heat-treated at900° C.     MX and M23C6in a 9 % Cr steel were investigated with energyfiltering transmission electron microscopy (EFTEM) andcompared with simulations. The used samples had been heattreated for various periods of time at 600 and 650° Cfor up to 26 000 h. The agreement of the simulations with the experiments wasgood in all cases when reasonable values of the interfacialenergy, the only adjustable parameter, were chosen. Coarsening simulations were also performed to investigatethe influence of changes in composition on the coarsening rate.For MX, in a 9 % Cr steel, the coarsening rate is almostindependent of the V/Nb ratio but highly dependent on theN-content. Also the effect on the coarsening rate for M23C6by adding Co to a Cr steel was investigated bysimulation. Co is known to increase the resistance totempering. The results show that a final average radius of thecarbides after 30 000 h at 600° C decreases with 30 % witha Co addition of 10 mass %. <b>Keywords:</b>Cr steels, nucleation, coarsening, model,DICTRA, precipitates, carbides, carbo-nitrides, MX, VN, M23C6, TiC, TEM, EFTEM, Curie-temperature

This thesis contains the development of a physically-based model describing the microstructural evolution during hot deformation of microalloyed steels. The work is mainly focused on the recrystallization kinetics. During hot rolling, the repeated deformation and recrystallization provides progressively refined recrystallized grains. Also, recrystallization enables the material to be deformed more easily and knowledge of the recrystallization kinetics is important in order to predict the required roll forces. Hot strip rolling is generally conducted in a reversing roughing mill followed by a continuous finishing mill. During rolling in the roughing mill the temperature is high and complete recrystallization should occur between passes. In the finishing mill the temperature is lower which means slower recrystallization kinetics and partial or no recrystallization often occurs. If microalloying elements such as Nb, Ti or V are present, the recrystallization can be further retarded by either solute drag or particle pinning. When recrystallization is completely retarded and strain is accumulated between passes, the austenite grains will be severely deformed, i.e. pancaking occurs. Pancaking of the grains provides larger amount of nucleation sites for ferrite grains upon transformation and hence a finer ferrite grain size is achieved. In this work a physically-based model has been used to describe the microstructural evolution of austenite. The model is built-up by several sub-models describing dislocation density evolution, recrystallization, grain growth and precipitation. It is based on dislocation density theory where the generated dislocations during deformation provide the driving force for recrystallization. In the model, subgrains act as nuclei for recrystallization and the condition for recrystallization to start is that the subgrains reach a critical size and configuration. The retarding effect due to elements in solution and as precipitated particles is accounted for in the model. To verify and validate the model axisymmetric compression tests combined with relaxation were modeled and the results were compared with experimental data. The precipitation sub-model was verified by the use of literature data. In addition, rolling in the hot strip mill was modeled using process data from the hot strip mill at SSAB Strip Products Division. The materials investigated were plain C-Mn steels and Nb microalloyed steels. The results from the model show good agreement with measured data. / QC 20100706

The objective of this work was to use LEFM in order to assess the detrimental influence of surrounding chloride-containing environments for stainless steels, hardened steel as well as for a cast aluminium alloy. An additional aim was also to use LEFM to assess the influence of porosity on the fatigue properties for different commercial cast aluminium alloys and manufacturing methods. The environmental influence on fatigue performance was mainly evaluated from fatigue crack growth measurements using compact tension (CT) specimens. In addition, fatigue performance in the high cycle regime was studied using spot welded specimens and smooth specimens. Corrosion fatigue tests for stainless steels were performed in different chloride-containing aqueous solutions and compared to the behaviour in air. Variables, which have been investigated, included temperature, redox potential and fatigue test frequency. The environmental influence on fatigue performance has also been compared to localised corrosion properties. Fatigue crack propagation rates were found to be higher in 3% NaCl than in air for all stainless steels investigated. The highest alloyed austenitic steel, 654SMO, showed the least influence of the environment. For duplex stainless steels the environment enhanced fatigue crack propagation rate to a higher degree than for austenitic stainless steels. This is explained by a material-dependent corrosion fatigue mechanism. In the high cycle regime, fatigue properties for spot welded stainless steels specimens were found to be decreased between 30%-40% due to the presence of 3% NaCl. For the hardened steel 100CrMnMo8 a fracture mechanics approach was employed for prediction of corrosion fatigue properties. In this model corrosion pit growth rate and the threshold stress intensity factor for fatigue crack propagation are needed as input parameters. For the high pressure die cast aluminium alloy the environmental influence of fatigue initiation through pre-exposure of smooth specimens was studied. Depending on environment used for pre-exposure, fatigue strength was found to be reduced by up to 50 % compared to the fatigue strength in air. Fatigue strength reduction was clearly associated to corrosion pits in the aluminium material. A fracture mechanics model was further successfully used to predict the environmental influence. The influence of porosity on the fatigue strength for the cast aluminium alloys tested has been described by a Kitagawa diagram. In design, the Kitagawa diagram can be used to predict the largest allowable pore size if the load situation in the component is known. The size of the porosity could either be evaluated directly from x-ray images or from metallographic prepared cross-sections using a method of extreme value analysis / QC 20100907

The goal of this work has been to evaluate the different experimental techniques used for quantitative analysis of multi-phase materials systems. Powder based specimens containing two-phases, austenite and ferrite , were fabricated and quantified. The volume fraction of ferrite varied from 2 Vol% to 50 Vol%. X ray powder diffraction (XRD) measurements were based on two peak analysis. Computer based software Topas was used for quantitative analysis, which is believed to be the most advanced in this field. XRD results were found within the absolute limit of +/- 4% of given ferrite volume fraction. Volume fraction as low as 2 Vol% was successfully detected and quantified using XRD. However, high statistical error was observed in case of low volume fraction, such as 2 Vol% and 5 Vol% ferrite volume fraction. Magnetic balance (MB) measurements were performed to determine the volume fraction of magnetic phase, ferrite. MB results were found in good agreement with given volume fractions. As low as 2 Vol% volume fraction was detected and quantified with MB. MB results were within the absolute limit of +/- 4% of given ferrite volume fraction. Image analysis (IA) was performed after proper sample preparation as required by electron backscatter diffraction (EBSD) mode of Scanning electron microscopy (SEM). IM results were found within the absolute limit of +/- 2 % of given ferrite volume fraction. However, high statistical error was observed in case of 2 Vol% volume fraction.