Thesis (Ph.D.)--University of Wollongong, 2004. / Typescript. Includes bibliographical references: leaf 192-205.

Thesis (Ph. D.)--University of Alberta, 2009. / Title from pdf file main screen (viewed on Dec. 16, 2009). "A thesis submitted to the Faculty of Graduate Studies and Research in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Materials Engineering, Department of Chemical and Materials Engineering, University of Alberta." Includes bibliographical references.

Thesis (M.Eng.). / Written for the Dept. of Mining and Materials Engineering. Title from title page of PDF (viewed 2009/06/17). Includes bibliographical references.

Low carbon bainitic steels microalloyed with Nb, Ti and V are widely used for the pipeline, construction and automobile industries because of their excellent combination of strength, toughness and weldability. Boron as another major alloying element has been also frequently used in this type of steels since the 1970s. The purpose of adding boron is to improve the hardenability of the steel by promoting bainite formation. / It has been realized that Boron can only be effective as a strengthening element when it is prevented from forming BN and/or Fe23(C, B) 6 precipitates. Therefore, Boron is always added together with other alloying elements which are stronger Nitride or Carbide formers, such as Ti and Nb. However, the formation of complex bainitic structures and the interaction with precipitates at industrial coiling temperature are not adequately understood. / In this study, the effect of boron on the microstructure and mechanical properties of a low carbon Nb-B steel was studied by a hot compression test (50% reduction at 850°C) followed by quenching samples into a salt bath. The microstructures of the tested samples were examined through optical microscopy and SEM; and the mechanical properties of these samples were investigated by micro-hardness and shear punch tests. / The results indicate that during thermo-mechanical controlled rolling (TCR), the final properties of the products not only depend on the applied deformation but also depend on the coiling temperature where phase transformation takes place. According to the investigation, two strengthening mechanisms are responsible for the strength of the steel at the coiling temperature: phase transformation and precipitation. Under optical microscopy, the microstructures of all specimens appear to be bainite in a temperature range from 350°C to 600°C without distinct differences. However, the SEM micrographs revealed that the microstructures at 550°C are very different from the microstructures transformed at the other holding temperatures. / Two strength peaks were observed at 350°C and 550°C in the temperature range studied. It is believed that the NbC precipitates are the main contributor to the peak strength observed at 550°C because the kinetics of NbC is quite rapid at this temperature. The strength peak at 350°C is mainly due to the harder bainitic phase, which formed at relatively lower temperature.

Abstract The aim of this work was to study systematically the effects of composition and processing on austenite grain growth and static recrystallization (SRX) kinetics, austenite decomposition under controlled cooling as well as microstructures, mechanical properties and weldability of hot rolled low carbon bainitic (LCB) steels. The results showed that the coarsening of austenite grain structure is influenced by the chemical composition. Steels with Nb-Ti alloying exhibited fine and uniform austenite grain size up to 1125 °C, whereas higher temperatures led to formation of the bimodal grain structures. However, with Nb-Ti-B microalloying, the abnormal grain growth was already observed at 1050 °C. SRX rate at roughing temperatures, determined by the stress relaxation method, was found to be retarded markedly by Mo, Nb and B alloying. For the test conditions investigated, the decomposition of austenite started in the temperature range from 780 °C to below 550 °C. All alloying elements with the exception of Nb (0.04–0.10 wt-%) decreased the phase transformation temperatures and increased the hardness of dilatometric specimens. Detailed microstructural examinations enabled the identification of 4 different ferrite morphologies: polygonal ferrite, quasi-polygonal ferrite (QF), granular bainitic ferrite (GB) and bainitic ferrite (BF), generally as a mixed microstructure consisting of 2–3 types morphologies. Consistent with the microstructures detected in dilatometric experiments, the microstructures of rolled plates comprise various combinations of low C ferrite morphologies. These microstructure types provided the yield strengths from 500 MPa up to 850 MPa in hot rolled condition and from 500 MPa to 950 MPa in heat-treated condition (600 °C/1h). The yield strengths from 500 MPa to 570 MPa were mainly related to QF microstructures in as-rolled condition, while the steels with the yield strength from 570 to 700 MPa had GB-QF microstructures. Steels with the yield strengths above 700 MPa consisted of BF. The most effective alloying element regarding the strength properties is B. Also C, Mn, Cr, Mo and Ni have strong influences, but Nb in the range of 0.05–0.10 wt-% is ineffective. Strengthening with B and Mo was detrimental to toughness. Alloying with Ni and Mn is beneficial to good strength and toughness combination. Mn, Mo, Nb and B contents mainly dictate CGHAZ toughness.

No description available.

No description available.

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.

Les aciers avancés à haute résistance (AHSS) de 3ème génération ont l’avantage de combiner résistance et ductilité. Ces aciers multi-phasés sont appréciés pour les applications dans l’industrie automobile pour leurs propriétés mécaniques, dues notamment à la présence d’austénite métastable permettant une transformation induite par la plasticité (effet TRIP- Transformation Induced Plasticity).L’objectif de ce travail a été d’étudier l’effet du microalliage sur les transformations de phases et la précipitation dans de tels aciers. Trois nuances ont été étudiées : une référence sans microalliage, une avec ajout de niobium et une avec ajout de vanadium. Elles ont été caractérisées au fil de la route métallurgique composée d’un recuit intermédiaire et d’un recuit final caractéristique des aciers bainitiques à effet TRIP.Des méthodes ex-situ et in-situ ont été mises en oeuvre. Les caractérisations in-situ pendant les traitements thermiques incluent une étude des transformations de phases par diffraction de rayons X à haute énergie (HEXRD) et une étude de la précipitation par diffusion de rayons X à petits angles (SAXS), utilisant le rayonnement synchrotron.La morphologie des grains a été observée par microscopie optique et diffraction d'électrons rétrodiffusés (EBSD) au Microscope Electronique à Balayage (MEB). L’imagerie des précipités a été effectuée par Microscopie Electronique en Transmission (MET) en imagerie en champ sombre, leur composition a été précisée par analyse dispersive en énergie (EDS) et leur localisation étudiée grâce à l’outil de nano-diffraction ACOM/ASTAR.L’ensemble de ces expériences a permis de mettre en évidence l’effet du traitement thermique et de la composition chimique sur la quantité d’austénite présente ainsi que sur sa teneur en carbone, qui sont les principaux paramètres contrôlant l’effet TRIP. La présence du microalliage se traduit par des variations de ces paramètres, liés à la fois à la présence de précipités contenant ces éléments et à leur présence en solution solide. / 3rd generation Advanced High Strength Steels (AHSS) have the advantage of combining strength and ductility. These multi-phase steels are appreciated for applications in the automotive industry for their mechanical properties, notably due to the presence of metastable austenite allowing Tranformation Induced Plasticity (TRIP effect).The objective of this work was to study the effect of microalloying on phase transformations and precipitation in such steels. Three grades have been studied: a reference without microalloying, one with niobium addition, and one with vanadium addition. They have been characterised through the metallurgical route composed of an intermediate annealing, following by a final annealing characteristic of TRIP-assisted bainitic steels.Both ex-situ and in-situ methods have been applied. In-situ characterisation during thermal treatments includes phase transformation study by High-Energy X-ray Diffraction (HEXRD) and precipitation study by Small Angle X-ray Scattering (SAXS), both performed with synchrotron radiation.Grain morphology has been observed by optical microscopy and Electron Back-Scatter Diffraction (EBSD) in a Scanning Electron Microscope (SEM). Imaging of precipitates has been made in Transmission Electron Microscopy (TEM) via dark-field imaging, their composition has been evauated by Energy Dispersive Spectroscopy (EDS) and their localization studied thanks to the nano-diffraction tool ACOM/ASTAR.All these experiments made it possible to highlight the effect of heat treatment and chemical composition on the amount of austenite present and on its carbon content, which are the main parameters controlling the TRIP effect. The presence of the microalloying results in variations in these parameters, related both to the presence of precipitates containing these elements and to their presence in solid solution.