Abstract not available

Abstract not available

The effects of Ca and Ce on the precipitation behaviour and microstructural characteristics of Mg-Zn based alloys are investigated by comprehensive multi-scale characterization and analysis. The elements Ca and Ce are chosen for their potential to enhance (a) precipitation hardening and (b) alloy texture and ductility, and are examined at both alloying and microalloying (< 0.5 wt%) levels. When added individually to Mg-Zn, Ca is found to enhance precipitation, but Ce produces a generally adverse effect on the hardening response. A pre-ageing strategy is proposed to alleviate this negative effect of Ce. The highlight of this work is the double microalloying addition of Ce-Ca to Mg-Zn, as this combination and quantity proves to be the most effective at increasing the age-hardening response, and enhancing microstructural characteristics for improved ductility. Transmission electron microscopy analysis reveals the hardening increase to originate from a refined precipitate microstructure, and the formation of fine-scale basal plate precipitates. These fine precipitates form during early ageing as monolayer GP zones consisting of Ca and Zn. The formation of these GP zones is facilitated by the atomic size difference between those two solutes, and their observed tendency to co-cluster. The monolayer GP zones evolve to multi-layered forms in the peak-aged condition. These precipitates are observed to be uniformly distributed, even where apparent precipitate-free zones are observed for the Mg-Zn type phases in the grain boundary regions. Notably, the size of these precipitate-free zones for the Mg-Zn phases is also reduced in the Ce-Ca microalloyed samples, compared to the binary alloy. The Ce-Ca microalloying additions also promote grain refinement and a weakening of the basal textures, typical of conventional Mg-based alloys, compared to both Mg-Zn and Mg-Zn-Ce. As a result, the tensile behaviour of the alloys with Ce-Ca is similarly enhanced. Considering both the precipitation hardening capability and microstructural characteristics, it is concluded that the double microalloying additions of Ce-Ca can be considered as a new alloy design strategy to successfully achieve improvement in both the strength and ductility of Mg-Zn alloys.

The effects of Ca and Ce on the precipitation behaviour and microstructural characteristics of Mg-Zn based alloys are investigated by comprehensive multi-scale characterization and analysis. The elements Ca and Ce are chosen for their potential to enhance (a) precipitation hardening and (b) alloy texture and ductility, and are examined at both alloying and microalloying (< 0.5 wt%) levels. When added individually to Mg-Zn, Ca is found to enhance precipitation, but Ce produces a generally adverse effect on the hardening response. A pre-ageing strategy is proposed to alleviate this negative effect of Ce. The highlight of this work is the double microalloying addition of Ce-Ca to Mg-Zn, as this combination and quantity proves to be the most effective at increasing the age-hardening response, and enhancing microstructural characteristics for improved ductility. Transmission electron microscopy analysis reveals the hardening increase to originate from a refined precipitate microstructure, and the formation of fine-scale basal plate precipitates. These fine precipitates form during early ageing as monolayer GP zones consisting of Ca and Zn. The formation of these GP zones is facilitated by the atomic size difference between those two solutes, and their observed tendency to co-cluster. The monolayer GP zones evolve to multi-layered forms in the peak-aged condition. These precipitates are observed to be uniformly distributed, even where apparent precipitate-free zones are observed for the Mg-Zn type phases in the grain boundary regions. Notably, the size of these precipitate-free zones for the Mg-Zn phases is also reduced in the Ce-Ca microalloyed samples, compared to the binary alloy. The Ce-Ca microalloying additions also promote grain refinement and a weakening of the basal textures, typical of conventional Mg-based alloys, compared to both Mg-Zn and Mg-Zn-Ce. As a result, the tensile behaviour of the alloys with Ce-Ca is similarly enhanced. Considering both the precipitation hardening capability and microstructural characteristics, it is concluded that the double microalloying additions of Ce-Ca can be considered as a new alloy design strategy to successfully achieve improvement in both the strength and ductility of Mg-Zn alloys.

Este trabalho, realizado em cooperação com a Gerdau Riograndense, tem por finalidade avaliar o comportamento do aço GG1013-M, um aço baixo teor de carbono microligado com vanádio e manganês, na laminação a quente no que tange a sua resistência à deformação, possibilitando assim a tomada de decisão em relação a modificações no processo. Foram realizados testes em simulador termomecânico Gleeble™ para determinação das temperaturas a serem usadas no teste prático no laminador, onde testou-se lotes que cobrissem toda a amplitude da faixa de composição química da qualidade do aço em estudo. No teste prático no laminador, foram retiradas amostras para os ensaios mecânicos, onde identificou-se, por intermédio do tratamento de dados em software estatístico, a influência da variação dentro da faixa da composição química sobre os limites de escoamento e resistência. Como resultado, conseguiu-se determinar a faixa de temperatura mais provável, onde a resistência a deformação a quente é menor, minimizando ou eliminando as conseqüências da redução de ductilidade a quente por conta do endurecimento da matriz por precipitação dos elementos de liga em forma de compostos. / This work was conducted in cooperation with Gerdau Riograndense aiming at the evaluation of the hot rolling behavior of a low carbon steel microalloyed with manganese and vanadium (internally GG1013-M steel).The deformation resistance was evaluated, allowing for the decision in relation to changes in the process. A thermomechanical simulator GleebleTM was used to determine the temperatures to be used in practical tests in the rolling mill, where it was tested different material batches covering the large range of chemical compositions for this kind of steel. Mechanical tests were performed on samples taken from the practical tests in the rolling mill. From this tests the influence of chemical composition variation on the yeld strength and maximum stress was studied. As a result, we were able to determine the most likely range of temperatures for a minimization of hot strentgh, therefore also minimizing or eliminating the consequences of the reduction in the hot ductility due precipitation hardening of the matrix.

Este trabalho, realizado em cooperação com a Gerdau Riograndense, tem por finalidade avaliar o comportamento do aço GG1013-M, um aço baixo teor de carbono microligado com vanádio e manganês, na laminação a quente no que tange a sua resistência à deformação, possibilitando assim a tomada de decisão em relação a modificações no processo. Foram realizados testes em simulador termomecânico Gleeble™ para determinação das temperaturas a serem usadas no teste prático no laminador, onde testou-se lotes que cobrissem toda a amplitude da faixa de composição química da qualidade do aço em estudo. No teste prático no laminador, foram retiradas amostras para os ensaios mecânicos, onde identificou-se, por intermédio do tratamento de dados em software estatístico, a influência da variação dentro da faixa da composição química sobre os limites de escoamento e resistência. Como resultado, conseguiu-se determinar a faixa de temperatura mais provável, onde a resistência a deformação a quente é menor, minimizando ou eliminando as conseqüências da redução de ductilidade a quente por conta do endurecimento da matriz por precipitação dos elementos de liga em forma de compostos. / This work was conducted in cooperation with Gerdau Riograndense aiming at the evaluation of the hot rolling behavior of a low carbon steel microalloyed with manganese and vanadium (internally GG1013-M steel).The deformation resistance was evaluated, allowing for the decision in relation to changes in the process. A thermomechanical simulator GleebleTM was used to determine the temperatures to be used in practical tests in the rolling mill, where it was tested different material batches covering the large range of chemical compositions for this kind of steel. Mechanical tests were performed on samples taken from the practical tests in the rolling mill. From this tests the influence of chemical composition variation on the yeld strength and maximum stress was studied. As a result, we were able to determine the most likely range of temperatures for a minimization of hot strentgh, therefore also minimizing or eliminating the consequences of the reduction in the hot ductility due precipitation hardening of the matrix.

Aços de alta resistência e baixa liga (ARBL) têm sido bastante utilizados na fabricação de tubulações para o transporte de petróleo e gás. Entretanto, o uso destes materiais em meios com elevadas concentrações de H2S, denominados sour, tem resultado em falhas frequentes, devido à suscetibilidade destes materiais ao desenvolvimento do fenômeno de trincamento induzido pelo hidrogênio (Hydrogen Induced Cracking - HIC), assim como devido a problemas de corrosão. O desenvolvimento de diferentes processos tecnológicos para a produção de tubos de aços ARBL, tais como a laminação controlada e resfriamento acelerado, a adição de microligantes, assim como a diminuição do teor de enxofre, fósforo, carbono e manganês, tem levado à elaboração de materiais com propriedades mecânicas otimizadas, permitindo também um melhor controle da microestrutura. As perdas de dureza e resistência mecânica devidas à redução do teor de manganês, são compensadas pela adição de elementos como cromo e nióbio. Neste trabalho estão sendo comparadas a resistência à corrosão e os parâmetros de permeabilidade do hidrogênio de dois tubos de aço API 5L X65 e uma chapa API 5L X65, todos do tipo ARBL e com baixo manganês (0,27%) e alto nióbio (0,083% a 0,090%), na solução B da norma NACE, TM-0284 (2011). Para isto, foram realizados ensaios de potencial de circuito aberto (Open Circuit Potential - OCP), espectroscopia de impedância eletroquímica (Electrochemical Impedance Spectroscopy - EIS) e curvas de polarização potenciodinâmicas no eletrólito naturalmente aerado, desaerado e saturado com H2S. Os testes de permeabilidade do hidrogênio foram realizados com base na norma ASTM INTERNATIONAL G148 - 97, porém usando a célula modificada de DEVANATHAN e STACHURSKY (1962) e com H2S como veneno catódico. Os materiais foram caracterizados por microscopia óptica (MO), microscopia eletrônica de varredura (MEV) e espectroscopia de energia dispersiva de Raios-X (X-Ray Energy Dispersive Spectroscopy - EDS) antes e depois de testes de imersão nos diferentes eletrólitos. Caracterização dos produtos de corrosão por difração de raios-X (DRX) também foi realizada após imersão em meio saturado com H2S (sour). As análises por MO e MEV mostraram matrizes ferríticas para os três aços, com a presença de baixos teores do microconstituinte martensita/austenita (M/A), de perlita e com baixo nível de inclusões uniformemente distribuídas e com composições químicas semelhantes. Os resultados dos ensaios de corrosão mostraram que, para todos os meios investigados, o aço denominado como B apresentou a melhor resistência à corrosão, enquanto aquele denominado como C se mostrou o mais suscetível em todas as condições estudadas. Para os três aços, a resistência à corrosão apresentou a seguinte ordem crescente de acordo com o meio de exposição: meio saturado com H2S < meio naturalmente aerado < meios desaerados. Ensaios de OCP e EIS no meio saturado com H2S em um período de 24h mostraram que a resistência à corrosão aumenta com o tempo em razão da formação de uma camada de sulfeto de ferro, que, no entanto, se apresentou pouco aderente. Os resultados dos ensaios de permeação de hidrogênio mostraram que o aço denominado B, que apresentou maior resistência à corrosão em todos os meios e que não apresenta perlita em sua microestrutura, teve o maior valor de difusividade efetiva de hidrogênio, menor concentração de hidrogênio atômico na sub-superfície e menor quantidade de traps por unidade de volume. Quanto aos outros dois materiais, os resultados dos testes de permeabilidade ficaram em desacordo com os resultados da caracterização microestrutural e dos testes de resistência à corrosão, indicando que fatores diferentes dos detectados neste estudo são importantes para governar essas propriedades. / High strength low alloy (HSLA) steels have been widely used in the manufacture of pipelines for the transport of oil and gas. However, the application of these steels in media with high H2S concentrations, denominated sour, has resulted in frequent failures due to the susceptibility of these materials to the development of Hydrogen Induced Cracking (HIC) phenomena, as well as due to corrosion problems. The development of different technological processes for HSLA piping production, like controlled rolling and accelerated cooling, the addition of microalloying elements, as well as the reduction of the amounts of sulphur, phosphorus, carbon and manganese, has led to the development of materials with optimized mechanical properties, also allowing a better microstructural control. Hardness and mechanical resistance reduction due to the lowering of Mn content are compensated by niobium and chromium addition. In this work, the corrosion resistance and the hydrogen permeability parameters of two API 5L X65 steel tubes and an API 5L X65 plate, all HSLA type and with low manganese (0.27%) and high niobium (0.083% to 0.090%) contents, are compared in solution B of NACE standard TM-0284 (2011). For this, open circuit potential (OCP), electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization curves were carried out in the naturally aerated, deaerated and H2S saturated electrolyte. Hydrogen permeability tests were performed based on ASTM INTERNATIONAL G148-97, but using a modified DEVANATHAN and STACHURSKY (1962) cell and with H2S as cathodic poison. The materials were characterized by means of optical microscopy (OM), scanning electron microscopy (SEM) and X-Ray Energy Dispersive Spectroscopy (EDS) prior and after immersion tests in the different electrolytes. Characterization of the corrosion products by X-ray diffraction (XRD) was also performed after immersion in the H2S-saturated (sour) medium. The OM and SEM characterization showed ferritic matrices for the three steels, with the presence of low levels of the martensite/austenite (M/A) microconstituent, perlite and with a low level of inclusions evenly distributed and with similar chemical compositions. The results of the corrosion tests showed that, for all investigated media, the steel denominated as B presented the best resistance to corrosion, whereas the one denominated as C showed to be the most susceptible in all the conditions studied. For the three steels, the corrosion resistance showed the following ascending order according to the exposure medium: H2S saturated < naturally aerated medium < deaerated media. OCP and EIS tests in the H2S-saturated medium in a period of 24 hours showed that the corrosion resistance increases over time due to the formation of an iron sulphide layer, which, however, presented little adhesion. The results of the hydrogen permeation tests showed that the steel denominated B, that presented greater corrosion resistance in all media and that does not present perlite in its microstructure, had the highest values of effective hydrogen diffusivity, the lowest concentration of atomic hydrogen in the subsurface and the smallest amount of traps per unit volume. Concerning the other two materials, the results of the permeability tests were at variance with the results of the microstructural characterization and corrosion resistance tests, indicating that factors other than those detected in this study are important to govern such properties.

The formability of Mg alloy sheet in the as-hot rolled condition depends on the microstructure developed during hot rolling. In general, the formability of Mg alloys is improved by finer grain sizes. 'Microalloying' levels of calcium (Ca), strontium (Sr), and cerium (Ce) have been found to refine the as-cast structure, but there is no information as to whether this effect will be reflected in the as-hot worked structure and formability. Thus, in this work, the effects of microalloying levels of calcium (Ca), strontium (Sr), and cerium (Ce) on the microstructures (from as-cast to as-hot rolled) and subsequent hot deformation behavior of AZ31, nominally 3% Al, 1% Zn, and 0.3%Mn, were systematically investigated. / To include the effect of solidification rate these alloys were cast in different moulds (preheated steel mould, Cu-mould, and water cooled Cu-mould). One-hit compression testing at temperatures between 250&deg;C &sim; 400 &deg;C, strain rates of 0.001, 0.01, 0.1 s-1 and strains from 0.2 up to 1.0, was performed to investigate the basic hot compression behavior, while two-hit compression testing was conducted to determine the static softening behavior. Hot rolling of the microalloyed AZ31 alloys was then carried out to study the effects of microalloying on as-hot rolled structure under two sets of rolling schedules. To investigate the formability of these microalloyed sheets, tensile tests were completed over a temperature range between ambient and 450&deg;C, at strain rates between 0.1 and 0.0003 s-1. / Results show that Ca and Sr act to refine the as cast grain size and the second phases, consistently promoting fine and uniform as-hot rolled grain structure. With regard to grain refinement, calcium has the strongest effect, whereas Ce is most effective for second phase refinement. In addition, microalloying retards grain growth during hot tensile testing. Multiple alloying presents a combined and complementary effect. / A refined and uniform grain structure combined with well dispersed and thermally stable second phases significantly improves the hot formability of AZ31 sheets by promoting dynamic recrystallization (DRX) in the matrix, resisting grain coarsening, and retarding the development of cavitation and necking. Under the superplastic condition of 450&deg;C and 0.0003 s -1, the elongation was improved by 17% with Ca only, 26% with Ca and Ce, 51% with Ca and Sr, and 59% with Ca, Sr and Ce.

No description available.

L’allégement des véhicules est l’un des objectifs prioritaires des constructeurs automobile pour répondre aux directives environnementales d’émission de CO2. Le développement des aciers multiphasés à très haute résistance mécanique est l’une des solutions communément adoptées pour réduire l’épaisseur des tôles dans les véhicules tout en conservant leur capacité à assurer la sécurité des passagers. La présente étude porte sur l’optimisation des paramètres du procédé de production industrielle de l’une des ces familles d’aciers : les aciers Dual Phase microalliés au titane et au niobium de haut grade ; c'est-à-dire possédant une résistance à la rupture supérieure à 800MPa.A partir d’une microstructure initiale bainite + martensite laminée à froid, les différents phénomènes se produisant au cours du recuit, de la chauffe jusqu’à la fin du maintien intercritique, sont caractérisés. L’influence des paramètres du recuit comme la vitesse de chauffe, la température et le temps de maintien est étudiée. Le système d’interactions triple entre la précipitation des éléments de microalliage, la recristallisation et la formation de l’austénite est au cœur du problème. Un scénario des évolutions microstructurales a été établi à partir de la caractérisation des divers phénomènes. La finesse de la microstructure étudiée (sub-micrométrique) a nécessité l’emploi combiné de techniques de caractérisation multi-échelles : MEB, MET, sonde atomique tomographique, nano-SIMS. / Lightening the weight of vehicles is one of the main challenging objectives of the automotive industry to reach the environmental regulation in term of CO2 emissions. The development of multiphase high strength steels is a common solution to reduce the thickness of sheet steel used in vehicles while keeping the same level of passenger’s safety requirements. The present study deals with the optimization of industrial process parameters applied to obtain one of these steels: the high strength microalloyed Dual Phase steels; i.e. with ultimate tensile strength superior to 800MPa.From an initial cold rolled microstructure made of bainite + martensite, the phenomena occurring during the annealing are characterized since the heating up to the end of the intercritical holding. The influence of process parameters as the heating rate, the holding temperature and the holding time are studied. The triple interactions system between the precipitation of microalloying elements, the recrystallization and the austenite formation is the core of the problem. A scenario of microstructural evolutions has been established based on the characterized phenomena. The studied fine microstructure (sub-microns) requires the combination of multiscale characterization techniques: SEM, TEM, atom probe tomography, nano-SIMS.