The microstructure of low alloy Transformation Induced Plasticity (TRIP) assisted steels has been systematically varied through the combination of computational and experimental methodologies in order to enhance the mechanical performance and to fulfill the requirement of the next generation Advanced High Strength Steels (AHSS). The roles of microstructural parameters, such as phase constitutions, phase stability, and volume fractions on the strength-ductility combination have been revealed. Two model alloy compositions (i.e. Fe-1.5Mn-1.5Si-0.3C, and Fe-3Mn-1Si-0.3C in wt%, nominal composition) were studied. Multiphase microstructures including ferrite, bainite, retained austenite and martensite were obtained through conventional two step heat treatment (i.e. intercritical annealing-IA, and bainitic isothermal transformation-BIT). The effect of phase constitution on the mechanical properties was first characterized experimentally via systematically varying the volume fractions of these phases through computational thermodynamics. It was found that martensite was the main phase to deteriorate ductility, meanwhile the C/VA ratio (i.e. carbon content over the volume fraction of austenite) could be another indicator for the ductility of the multiphase microstructure. Following the microstructural characterization of the multiphase alloys, two microstructural design criteria (i.e. maximizing ferrite and austenite, suppressing athermal martensite) were proposed in order to optimize the corresponding mechanical performance. The volume fraction of ferrite was maximized during the IA with the help of computational thermodyanmics. On the other hand, it turned out theoretically that the martensite suppression could not be avoided on the low Mn contained alloy (i.e. Fe-1.5Mn-1.5Si-0.3C). Nevertheless, the achieved combination of strength (~1300MPa true strength) and ductility (~23% uniform elongation) on the low Mn alloy following the proposed design criteria fulfilled the requirement of the next generation AHSS. To further optimize the microstructure such that the designed criteria can be fully satisfied, further efforts have been made on two aspects: heat treatment and alloy addition. A multi-step BIT treatment was designed and successfully reduced the martensite content on the Fe-1.5Mn-1.5Si-0.3C alloy. Microstructure analysis showed a significant reduction on the volume fraction of martensite after the multi-step BIT as compared to the single BIT step. It was also found that, a slow cooling rate between the two BIT treatments resulted in a better combination of strength and ductility than rapid cooling or conventional one step BIT. Moreover, the athermal martensite formation can be fully suppressed by increasing the Mn content (Fe-3Mn-1Si-0.3C) and through carefully designed heat treatments. The athermal martensite-free alloy provided consistently better ductility than the martensite containing alloy. Finally, a microstructure based semi-empirical constitutive model has been developed to predict the monotonic tensile behavior of the multiphase TRIP assisted steels. The stress rule of mixture and isowork assumption for individual phases was presumed. Mecking-Kocks model was utilized to simulate the flow behavior of ferrite, bainitic ferrite and untransformed retained austenite. The kinetics of strain induced martensitic transformation was modeled following the Olson-Cohen method. The developed model has results in good agreements with the experimental results for both TRIP steels studied with same model parameters.

Increasing demand from flourishing construction markets led to the successful development of high strength steels (HSS). The new structural steel has exceptional high strength, high fracture toughness, long fatigue life, high corrosion resistance, and better weldability making the material attractive for structural design applications in the modern steel buildings and bridges. With their high strength, typically in the range of 500~700 MPa, and reduced weight/dimensions, it frees imaginations of modern designers and opens up new possibilities. Although HSS cost more, this is more than offset by reduced fabrication and erection costs. The advantage of the intrinsic properties of the HSS makes it possible to achieve successful applications in a cost-effective manner. At present, the Australian steel design standard, AS 4100 (SA, 1998), is limited to conventional low strength steels (LSS) with yield stress less than 450 MPa, (i.e. fy . 450 MPa). As a result steel structural members fabricated from HSS in Australia are usually designed according to overseas specifications, such as AISC-LRFD (AISC, 2003) which allows the design for structures fabricated from HSS materials. However, the design provisions of AISC-LRFD were mainly based on experimental and analytical studies on standard LSS. HSS exhibits mechanical properties that are quite different from conventional LSS. On the other hand, the design procedure and approach of the American specifications (AISC, 2003) are unfamiliar with Australian design engineers, which explains why practising engineers in Australia are reluctant to use AISC-LRFD specification in the design of HSS members. Therefore research into the behaviour of HSS members is essential to address this shortcoming. However, since the use of HSS often leads to smaller sections, hence thinner plates, the elastic and inelastic instability of these thin-walled and HSS members become highly critical. Conservatively, the local instabilities of the constituent plate element interactions in the cross-section have been ignored in the current steel practices. Increasing the slenderness of either plate elements within a cross-section leads to a significant reduction in the section capacity of the structural member. Therefore, the interactive effects between flange and web plate elements have to be considered in the strength, stability and deformation studies of HSS members. Furthermore, the current definitions and values of the plate slenderness limits also vary among major steel design codes (AS4100, 1998; AISC, 2003; EN1993, 2003; BS5950, 2000). The main aim of this research project is to investigate the structural behaviour of Ishaped HSS members subjected to local buckling effects in the elastic and inelastic ranges. For this purpose, it will use advanced numerical analyses and laboratory experiments to study the structural behaviour of these HSS members in compression and bending, respectively. The critical review has found that various inconsistencies among the major steel design specifications (AS4100, 1998; AISC, 2003; EN1993, 2003, BS5950, 2000) in the current practice produce conflicting design predictions of section capacities. The experimental measurements of residual stress distributions have confirmed that the ECCS recommendation (1984) is inappropriate for crosssections fabricated from typical HSS materials (i.e. BISPLATE80). The experimental measurements and numerical studies carried out in this project have produced a better understanding of the structural behaviour of HSS members subjected to local instabilities. The study has enabled to provide a series of proposals for proper assessment of plate slenderness limits for structural members made of HSS materials. It may also enable the inclusion of future version of the AS4100 code for HSS materials to be used in the design of steel building and bridge constructions. It is believed that the use of HSS in building and bridge constructions will increase significantly in the very near future, and to fully-facilitate this, the future versions of national and international steel design specifications must include rational and reliable design rules for members made of all steel grades by including the effects of HSS special characteristics and true interactive local buckling behaviour of HSS members. This research project has contributed towards this.

No description available.

The unique combination of high specific strength and ductility in third generation advanced high-strength steels (3G-AHSSs) has garnered significant attention from top automotive steel industries. These materials are being considered as potential options for making lighter body components due to their strength and ability to tolerate thinner material cross-sections. However, galvanizing these steels through the continuous hot-dip galvanizing process is challenging, because the main alloying elements such as Mn, Si, Al, and Cr tend to selectively oxidize on the steel surface during the annealing process before being immersed in the galvanizing bath containing Zn(Al, Fe). The presence of these oxides extensively covering the substrate surface can negatively impact reactive wetting, coating adhesion, and overall coating quality. In this study, the selective oxidation kinetics and reactive wetting of a series of Fe-(2-10)Mn-(0.00/0.01/0.03)Sb (at. pct) were determined and a model was proposed for analyzing oxide growth during intercritical annealing prior to galvanizing. Annealing heat treatments were carried out at 676, 725, 775, and 825 ˚C for 60-480s holding time in a N2-5vol pct H2 process with a dew point of –10 ˚C. MnO was formed on all samples after annealing. It was determined that the annealing conditions (temperature and isothermal holding time) affected the external oxide thickness and depth of the oxidation zone, which in turn influenced the MnO growth rate. With increasing the bulk Mn content of the alloy, the Mn elemental flux to the external surface increased, resulting in an increase in the oxidation parabolic rate constant. The average activation energy of internal oxidation for the Fe-2Mn, Fe-6Mn and Fe-10Mn alloys were determined to be 216±15 kJ/mol, 178 ± 18 kJ/mol and 152 ±10 kJ/mol, respectively, which are consistent with the activation energy of oxygen diffusion through MnO interfaces and the bulk diffusion of oxygen in austenite. Moreover, the average activation energy for external oxide growth was ~113±18 kJ/mol, which was attributed to the diffusion of Mn cations along the grain boundaries of the external Mn oxides. It was determined that micro addition of Sb to the Fe-Mn alloys led to a reduction in the oxidation rate constant, external oxide thickness, and internal oxidation zone, which was attributed to Sb segregation at both the external and internal oxide interface, resulting in the reduction of oxygen permeability. The reduction was more significant in the Fe-10Mn alloys, primarily attributable to the increased Sb segregation at the interfaces. The research showed that when the bulk Mn content increased, more antimony (Sb) segregated at both the internal and external oxide/substrate interface. As a result, the oxygen present at these interfaces decreased. This is attributed to the reduction of Sb solubility in α-Fe with increasing Mn and positive interactions between Sb and Mn. Advanced Atom Probe Tomography (APT) analysis confirmed that as more Sb segregated at the interfaces, the excess oxygen reduced due to site competition between O and Sb. Additionally, Sb surface segregation kinetics for Fe-(0.01/0.03)Sb and Fe-2Mn-(0.01/0.03)Sb at.% were determined based on the modified Darken model and linear heating followed by isothermal annealing. After the annealing, Sb segregation was detected on the surface of both the Fe-xSb and Fe-2Mn-xSb alloys, which increase with increasing temperature and holding time. The segregation rate, as determined from the Darken curves, was higher in Fe-Sb alloys compared to Fe-2Mn-Sb alloys, which can be attributed to variations in the crystal structure and the density of defects within the metal matrix. Additionally, the activation energy for Sb diffusion in both Fe-Sb and Fe-2Mn-xSb alloys were determined to be approximately 193±18 kJ/mol closely aligns with the activation energy of Sb bulk diffusion in α-Fe. Simulated galvanizing treatments were conducted on Fe-(2-10)Mn-(0.00/0.03)Sb at.% alloys. It was found that Sb segregation at the external/oxide interface resulted in a decrease in the size and thickness of the external oxide particles, which can facilitate better contact between the zinc bath and the substrate. Furthermore, it was found that Sb segregation at the interface between the external oxide and substrate led to a decrease in the stability of the interfacial region. This effect was attributed to an increase in the local atomic spacing near the interface, caused by Sb segregation. As a result, a local strain was observed near the interface. This localized strain significantly reduced the energy needed to separate the oxide from the metal matrix, contributing to decreased stability of the interfacial region. The higher bulk manganese (Mn) content led to increased segregation of antimony (Sb), resulting in a greater local strain within the interfacial region. These effects, in turn, enhanced the kinetics of the aluminothermic reduction reaction and assisted oxide lift-off. Furthermore, the closely packed Fe-Al intermetallics at the coating/steel interface increased as a result of adding Sb to the steel. In addition, no Sb segregation was observed at interfacial layer/metal interface. This absence of segregation can be attributed to the dissolution of segregated Sb into the liquid zinc. It was determined that Sb, which segregated at the external oxide/substrate interface during annealing, dissolved into the zinc bath and disrupted its bond with iron. This disruption occurred due to the higher electronegativity of Sb compared to Fe with Zinc, as well as the sufficient solubility of Sb in liquid zinc. / Thesis / Doctor of Science (PhD) / The unique combination of high specific strength and ductility exhibited by third-generation advanced high-strength steels has captured the attention of automotive industries. However, challenges arise when attempting to galvanize these steels through continuous hot-dip galvanizing processes. The selective oxidation of alloying elements during annealing can have detrimental effects on reactive wetting and coating adhesion. The objective of this research was to improve the coating quality of Mn-containing steels by introducing micro-additions of Sb. Sb segregation to the surface and interfaces began to occur during annealing. Segregated Sb resulted in a reduction of the oxidation rate. Sb segregation at oxide interfaces also contributed to decreased oxygen permeability. Upon immersion in the liquid zinc bath, both Sb and Fe dissolved into the zinc, leading to the formation of an interfacial layer on the surface, which indicates successful reactive wetting. The findings of this research provide valuable insights for improving galvanizing processes and enhancing coating quality, specifically in the context of third-generation advanced high-strength steels.

No description available.

Secondary hardening ultra-high strength (SHUHS) steels possess a unique combination of strength, fracture toughness and stress corrosion cracking resistance, which makes them candidate materials for aircraft landing gear and armour applications. There is a sustained drive to develop stronger and tougher materials for such applications. The objectives of this thesis are two-fold: first, to develop a new SHUHS alloy that is stronger than the existing SHUHS steel developed at Defence Metallurgical Research Laboratory (DMRL), Hyderabad and second, to establish processing-structure-property correlations for the new alloy. Empirical design and development of these complex steels involves enormous effort, cost, time and materials resources. To avoid this, a semi-empirical approach was espoused in this thesis wherein thermodynamic calculations using ThermoCalc were conducted to computationally design a series of alloys with varying levels of Cr and Mo. The design space was constrained by two objectives related to M2C carbides which are the primary cause of secondary hardening in these alloys. The first objective was to increase the amount of M2C to increase the peak strength, while the second objective was to lower the Cr/Mo ratio of the M2C to control its over-ageing behavior. Two new alloys C23 (with 2Cr-3Mo, wt. %) and C55 (with 5Cr-5Mo, wt. %) and a base alloy akin to the DMRL SHUHS steel, C21 were selected for experimental validation. These alloys were melted, rolled and subjected to a battery of heat treatments. Austenitization studies revealed that the new alloys required higher austenitization temperatures to dissolve primary carbides. However such a treatment also resulted in an austenite composition that was not conducive for obtaining a fully martensitic microstructure on quenching. Based on these studies, the design space was modified to include additional criteria related to the Ms and precipitate dissolution temperatures. C55 failed to clear either criteria, while C23 cleared both, and so tempering studies were limited to C23. Isochronal tempering studies revealed that C23 in the peak aged condition was >10% stronger than C21 indicating that the alloy design objective of strength enhancement was achieved successfully. Microstructural characterization revealed that the strength enhancement was due to the higher number density and volume fraction of the M2C-like solute clusters in C23, which resist shearing in the under-aged condition and strengthen by Orowan mechanism in the over-aged condition. This thesis has successfully demonstrated that the design paradigm of enhancing strength by increasing the amount of M2C is justified and that ThermoCalc can be used to as an objective-oriented alloy design tool in this class of the steels.

L’objectif de cette thèse est d’aboutir à une meilleure compréhension des mécanismes de ségrégation du bore aux joints de grains austénitiques (γGB) et de leur effet sur la décomposition de l’austénite. En effet, l’addition de très faibles quantités de bore comme élément d’alliage permet d’augmenter de manière remarquable la résistance mécanique des aciers à très haute résistance. Cet effet est lié à l’état du bore aux γGBs qui décale la cinétique de décomposition de l’austénite.Tout d’abord, la distribution du bore dans la microstructure a été identifiée de manière très précise à l’aide des analyses de la même zone par Nano-SIMS et par MEB. De plus, le couplage de la sonde atomique tomographique et du Nano-SIMS a apporté une meilleure quantification de l’état du bore dans la microstructure. Ces études ont été réalisées après différents traitements thermiques qui ont été conçus spécifiquement pour étudier séparément chaque mécanisme. L’ensemble de ces résultats permet d’écarter la contribution de la ségrégation hors équilibre et confirme la présence d’un équilibre local entre les γGBs et la solution solide dans leurs voisinages. Par conséquent, le niveau de ségrégation du bore aux γGBs est contrôlé par l’état de précipitation des borures qui définit la concentration du bore en solution solide.Par ailleurs, des mesures de DRX in situ et de dilatomètrie ont été effectuées afin de suivre les cinétiques de formation de la bainite. Les résultats montrent que la cinétique de formation de la bainite est retardée en augmentant la quantité de bore ségrégé, par contre l’augmentation de la taille de grain austénitique l’accélère. / The aim of this thesis is to lead to a better understanding of the mechanisms of boron segregation at austenite grain boundaries (γGB) and its effect on the austenite decomposition. Indeed, the small quantity of boron as alloying element remarkably improves the mechanical resistance of the advanced high strength steels. This effect is related to the boron state at γGBs, which delays the kinetics of austenite decomposition.The boron distribution in the microstructure was precisely identified thanks to the analyses of the same field by using correlative nano-SIMS and SEM. In addition, the coupling of APT and nano-SIMS provided a better quantification of the boron state in the microstructure. These studies were performed after different heat treatments, which were specifically designed to study separately each mechanism. The results excludes the contribution of non-equilibrium segregation mechanism on boron segregation at γGBs and confirm the local equilibrium between the γGBs and the solid solution at the γGBs vicinity. Consequently, the level of boron segregation at γGBs is controlled by boride precipitation, which controls the concentration of boron in solid solution.Measurements of in situ XRD and the dilatometry were performed in order to follow the kinetics of bainite formation. The specific heat treatments were applied before bainite formation in order to study the effect of boron segregated amount at γGBs and the austenite grain size. These results show that the kinetics of bainitic transformation is delayed by the increase of boron segregated amount. Whereas, the increasing of austenite grain size accelerates the kinetics of bainitic transformation.

Foram realizados ensaios de dilatometria em ligas não comerciais que apresentam microestrutura bainítica após o resfriamento contínuo. As variações de composição química foram realizadas sobre o aço destinado para construção mecânica AISI 5120 com adições de molibdênio, boro e nióbio. Os ensaios foram conduzidos no dilatômetro com atmosfera e temperatura controlada. No dilatômetro, foram aplicados resfriamentos contínuos em diferentes velocidades a partir da temperatura em que normalmente peças forjadas são reaquecidas. Tradicionalmente, a classe dos aços apresentados neste trabalho é exposta ao tratamento térmico de têmpera e revenimento e apresentam microestrutura martensítica. Com o objetivo de eliminar o tratamento térmico realizado pós conformação, foi proposto como substituição os aços bainíticos. Aços bainíticos não exigem tratamento térmico pós conformação e, apenas com a aplicação de um resfriamento controlado, é possível obter uma microestrutura que apresenta propriedades (tensão de escoamento e tenacidade) iguais ou melhoradas em relação ao material temperado e revenido. As microestruturas obtidas nas diferentes ligas resfriadas de maneira contínua foram caracterizadas de modo a estabelecer relações entre a velocidade de resfriamento e produtos formados, morfologia e fração de microconstituíntes. A caracterização microestrutural foi realizada de maneira intensiva de modo a relacionar desde propriedades magnéticas com padrões de difração de raios X das amostras para medição da fração de austenita retida. O objetivo deste trabalho foi investigar qual é a influência do molibdênio, boro e nióbio no resfriamento contínuo de aços bainíticos, bem como estabelecer o intervalo de velocidades de resfriamento em que é possível obter de maneira homogênea a estrutura bainítica. Após o resfriamento, os corpos de prova foram caracterizados por metalografia (microscopia óptica e eletrônica de varredura), dureza, saturação magnética, difração de raios x e EBSD. De fato foi verificado o efeito do molibdênio, boro e nióbio na cinética de decomposição da austenita no resfriamento contínuo e estabelecido relações entre a microestrutura obtida, velocidade de resfriamento e composição química. Foi observado também o efeito do molibdênio, boro e nióbio em evitar a transformação ferrítica para baixas velocidades de resfriamento de modo a obter uma estrutura bainítica sob um maior intervalo de resfriamento. / Dilatometry tests were carried out in a non commercial alloy that showed bainitic microstructure after continuous cooling from the austenitization temperature. The chemical composition variations were performed on a base chemical composition of a commercial steel (AISI 5120), additions were of molybdenum, boron and niobium. The tests were conducted on the dilatometer with atmosphere and temperature control. In the dilatometer, continuous cooling was carried out at different rates from the temperature in which the reheating of forged parts is usually performed. Traditionally, the steels used for this application are quenched and tempered and present a predominantly tempered martensite microstructure; bainitic steels were proposed as a substitution in order to eliminate further heat treatments after forging. The bainitic steels do not require post-conformation heat treatment: only with the application of a controlled continous cooling is possible to obtain a homogenous bainitic microstructure which has equal or improved properties (yield strength and toughness) comparing to quenched and tempered material. The microstructures obtained from the different alloys continuously cooled were characterized in order to establish relations between the cooling rate and formed products, morphology and volume fraction of phases. The microstructural characterization was carried out intensively and correlated with magnetic properties and X-ray diffraction patterns of the samples. The objectives of this work were to investigate the influence of molybdenum, boron and niobium on the continuous cooling of bainitic steels, as well as to establish the range of cooling rates needed in order to obtain an homogeneous bainitic structure. After cooling, the specimens were characterized by metallography (optical and scanning electron microscopy), hardness, magnetic saturation, x-ray diffraction and EBSD. The effect of molybdenum, boron and niobium on the kinetics of austenite decomposition in the continuous cooling was verified and relationships established between the microstructure, cooling rate and chemical composition. It was also observed the effect of molybdenum, boron and niobium in avoiding ferritic transformation at low cooling rates in order to obtain a bainitic structure under a longer cooling interval.

Os Aços Avançados de Alta Resistência ou AHSS (do inglês Advanced High Strength Steels) apresentam muitas vantagens mecânicas em relação aos aços convencionais. Seu uso crescente na indústria automotiva deve-se principalmente à sua capacidade de possibilitar a redução de peso e, ao mesmo tempo, o aumento da segurança aos ocupantes do veículo em caso de colisões. No entanto, apresentam maiores dificuldades no que se refere à conformabilidade (maiores níveis de solicitação e desgaste das ferramentas, menor deformabilidade plástica, etc). Assim, alguns testes para avaliar a conformabilidade destes materiais ganham maior importância. É o caso do Teste de Expansão de Furos, cuja propriedade medida é a Razão de Expansão de Furos (REF). Neste trabalho investiga-se o processo de expansão de furos para o aço avançado de alta resistência (AHSS) martensítico DOCOL 190M, sob as seguintes condições de processo: duas formas de obtenção do furo (jato d’água e usinagem); duas geometrias distintas de punções (cônico de 60º e elíptico); diversos diâmetros do furo inicial; com e sem o uso de lubrificante; com acabamento diferenciado da borda do furo; e expansão com deslocamento do punção em etapas. Os experimentos demonstram que a expansão de furos possui uma estreita relação com a geometria do punção utilizado para a expansão, bem como com o diâmetro do furo inicial, acabamento da borda e condições de lubrificação. A partir dos resultados experimentais de expansão de furos foi possível realizar a calibração de um software de simulação computacional em relação ao dano crítico do material no momento da fatura na borda do furo. / Advanced High Strength Steels (AHSS) offer many mechanical advantages over conventional steels. Its increasing use in the automotive industry is mainly due to its ability to reduce weight and, at the same time, increase occupant safety in the event of collisions. However, they present greater difficulties with respect to the formability (higher levels of solicitation and wear of the tools, lower plastic formability, etc). Thus, some tests to evaluate the formability of these materials come to have greater importance. This is the case of the Hole Expansion Test, whose measured property is the Hole Expansion Ratio (REF). This work investigates the hole expansion process for a martensitic advanced high-strength steel (AHSS), DOCOL 190M, under the following process conditions: two ways of obtaining the hole (water jet and machining); two different geometries of punctures (conical of 60º and elliptical); various diameters of the initial hole; with and without the use of lubricant; with differentiated finishing of the hole edge; and expansion with punch displacement in steps. The experiments demonstrate that the hole expansion has a close relationship with the geometry of the punch used for the expansion, as well as the initial hole diameter, edge finish and lubrication conditions. From the experimental hole expansion results it was possible to carry out the calibration of a computational simulation software in relation to the critical damage of the material at the moment of hole edge rupture.

This Miniature mechanical testing study is concerned with the use of miniature specimens to identify the mechanical properties of stainless steel Type 304, sensitized Type 304 and SA516 Grade 70 carbon steel as a viable replacement for the standard sized mechanical testing. The study aims at obtaining suitable specimen geometry and tensile testing proce- dure for miniature mechanical testing whose mechanical properties are comparable to that of conventional specimens of ASTM A370-10 of the same steel. All specimens are at and the gauge length cross section will be varied to obtain suitable geometry. The miniature tensile testing results are further validated by using Monte Carlo Method (MCM) for uncertainty estimation in order to know the probability distribution of mechanical properties. Miniature specimens with a cross section of 3 mm2 and 12 mm gauge length are found to produce equiva- lent mechanical properties as tested from standard-sized specimens. If a reasonable agreement is received, it will provide us with a very useful tool to evaluate mechanical properties of de- graded materials, which cannot be removed from service for standard testing, for repair and service life evaluation.