The third-generation advanced high strength steels, AHSS, represent an opportunity for today’s steel development, where lighter materials with maintained strength and toughness are in demand. The unique properties of these materials often stem from a tailored microstructure. In the continued development of these steels, without relying on expensive alloying methods, process design in the form of precise heat treatments plays an increasingly important role. This work focuses on Medium Mn AHSS with the aim of investigating one of these heat treatments, intercritical annealing, which is essential for achieving the desired material properties. Experimental testing of annealing effects is acknowledged to be a challenging process, and this study aims to present a novel approach for these types of tests. During experimental testing of intercritical annealing, the thermomechanical testing system Gleeble 3800 is a recognized tool. The mounting technique employed in the Gleeble results in an inhomogeneous heat distribution in the samples, generating a thermal gradient. This report aims to utilize this gradient as an opportunity to test the effect of several intercritical annealing temperatures on one sample, thereby increasing the efficiency of experimental work. The method is based on data retrieved from thermocouples attached to the specimen during Gleeble trials with the intent to identify the thermal gradient. This data is combined with x-ray diffraction measurements where the retained austenite fraction is measured. Thermodynamic calculations of expected retained austenite fraction following intercritical annealing are performed parallel to experimental work. The results of this work show that it is possible to utilize the thermal gradient to retrieve extensive data regarding the effect of intercritical annealing using only one sample. The results show a distinct thermal gradient and a corresponding gradient of retained austenite fraction along the specimen. The results for retained austenite fraction at room temperature can be rationalized on the basis of computational predictions. These variations potentially arise due to the material not reaching equilibrium within the annealing timeframe. This conclusion is supported by other computational results concerning austenite composition. In summary, the present work illustrates a new approach streamlining experimental work that, with some refinements, has the potential to benefit the broader scienitific community, in addition to providing a powerful new tool for rapid technological advancement in the steel industry / Tredje generationens avancerade höghållfasta stål representerar en möjlighet för dagens stålutveckling där lättare material med bibehållen styrka och seghet efterfrågas. De unika egenskaperna hos dessa material härrör ofta frän en skräddarsydd mikrostruktur. Vid fortsatt utveckling av dessa stål är det önskvärt att minimera användningen av legeringsämnen, vilket betyder att processdesign i form av korrekta värmebehandlingar blir  av  stor  betydelse.  Detta  arbete  fokuserar  på  Medium  Mn  avancerade höghållfasta stål med syftet att undersöka en av dessa värmebehandlingar, interkritisk glödgning,  vilken  har  en  avgörande  betydelse  för  att  uppnå önskad  prestanda. Experimentell  testning  av  glödgningseffekter  anses  vara  en  utmanande  process och avsikten med denna studie är att presentera ett nytt tillvägagångssätt för denna typ av test. Under experimentell utvärdering av glödgningseffekter används ofta det termomekaniska testsystemet  Gleeble  3800.  Provmonteringen  i  Gleeblen  resulterar i en  inhomogen värmefördelning i proverna vilket medför en temperaturgradient. Denna rapport syftar till att använda gradienten som en möjlighet att testa effekten av flera  glödgningstemperaturer  på  ett  enda  prov  och  därigenom  öka  effektiviteten i det  experimentella  arbetet.  Metoden  grundas  på  data  från  termoelement  fästa  på provet under Gleebleförsök, med avsikt att identifiera den termiska gradienten. Denna data kombineras sedan med XRD-mätningar där austenitfraktion efter värmebehandling utvärderas.  Termodynamiska  beräkningar  av  förväntad  austenitfraktion  efter interkritisk glödgning genomförs parallellt med experimentellt arbete. Resultaten  från  detta  arbete  påvisar  att  den  presenterade  metoden  är  genomförbar då omfattande data gällande interkritisk glödgningseffekt grundat på endast ett prov erhålls. Resultaten visar en tydlig termisk gradient och en motsvarande gradient av austenitfraktion längs provet, vilka är i överensstämmelse med tidigare experimentella resultat för samma material. Resultaten för austenitfraktion vid rumstemperatur uppvisar  betydande  likheter  med  de  termodymiska  beräkningarna, med  några  undantag. Orsaken till dessa variationer ¨ar troligen en otillräcklig glödgningstid, vilket gör att  materialet  inte  når  jämvikt.  Denna  hypotes  stöds  av andra  beräkningsresultat gällande austenitens sammansättning. Sammanfattningsvis presenterar denna rapport ett nytt tillvägagångssätt för att effektivisera experimentellt arbete, som med vissa förbättringar har potential att gynna det bredare forskarsamhället.

[pt] A demanda por veículos mais seguros e com baixo consumo de combustível vem levando a indústria automotiva a buscar novos materiais. A indústria do aço, ameaçada pela competitividade da indústria do alumínio, reagiu com uma série de novos aços de alta resistência. Dentre estes aços, os Aços Avançados de Alta Resistencia (AHSS) podem ser destacados. Esses aços podem ser divididos em 3 gerações, cada uma delas com suas vantagens e desafios. A primeira geração tem os aços mais baratos, geralmente com microestrutura ferritica/martensitica. A segunda geração possui os aços inoxidáveis austeníticos/ferríticos, com composição mais cara devido ao maior teor de liga, muitos deles apresentando efeito de plasticidade induzida por maclagem (TWIP). Entre essas duas gerações, uma terceira vem se sobressaindo, baseada em aços de composição mais barata, porém com processamento mais complexo, como os aços de tempera e partição (Quenching and Partitioning - Q and P). Como não existe apenas um único caminho para o sucesso, todas as três gerações vêm recebendo bastante atenção e pesquisa. Buscando atender parte da demanda do setor, a Companhia Siderúrgica Nacional (CSN), vem aprimorando seu portfólio de aços AHSS de primeira geração. Entre os aços de primeira geração, os mais utilizados hoje são os Dual-Phase (DP). No entanto, os aços DP apresentam alguns problemas, como a nucleação de vazios durante a deformação, o que é um fator limitante para suas propriedades mecânicas. Sua substituição por aços Complex-Phase (CP), com maiores quantidades de bainita e menos propensos a nucleação de vazio, vem sendo proposta. O processamento de aços de fase complexa envolve uma sequência de etapas de laminação a quente e a frio, seguidas de um tratamento térmico. Na presente tese, foi estudada a produção de um aço CP1200 em uma linha industrial de galvanização por imersão a quente. O ponto de partida foi um aço CP1100. Amostras deste aço laminado a frio foram analisadas por dilatometria de forma a se obter a curva CCT. Utilizando os dados dilatométricos, um novo tratamento térmico foi proposto e realizado nas instalações da CSN, produzindo com sucesso um aço CP 1200. Ensaios de tração, dureza, dobramento e expansão de buraco foram realizados para medir as propriedades mecânicas do novo aço. A caracterização microestrutural foi realizada por meio de microscopia óptica (MO), microscopia eletrônica de varredura (MEV), microscopia de força atômica (MFA), difração de elétrons retroespalhados (EBSD) e microscopia eletrônica de transmissão (MET); a quantificação das micrografias foi realizada usando processamento digital de imagem e redes neurais. O aumento da propriedade mecânica foi atribuído ao aumento na fração de bainita, bem como de interfaces bainita-ferrita e bainita-martensita, que são menos suscetíveis a nucleação de vazios. / [en] The demand for safer and fuel-efficient vehicles leads the automotive industry to seek new and stronger materials. The steel industry, threatened by the aluminum competition, reacted with new and higher strength steels. Among the possible steels, the Advanced High Strength Steels (AHSS) can be highlighted. These steels can be divided into 3 generations, each one possessing advantages and challenges. The first generation includes more economical alloying and processing strategies, usually with a ferritic/martensitic microstructure. The second generation contains the more expensive, higher alloyed ferritic/austenitic stainless steels, using TWinning Induced Plasticity (TWIP). Between these two classes, a third generation is growing, based on more inexpensive compositions but with more complex processing, such as Quenching and Partitioning (Q and P). There is not only a single path to success, because of that, all three generations receive their fair amount of attention and research. Trying to fulfill part of the industry demand, the Companhia Siderúrgica Nacional (CSN) is conducting research on the first generation of AHSS steels. Among the first generation steels, Dual-Phase (DP) are the most used. However, DP steels present some problems, such as void nucleation during deformation, which is a limiting factor on their mechanical properties. Therefore, their replacement by Complex-Phase (CP) steels, with higher bainite amounts, and less prone to void nucleation, is welcome. The complex phase steels processing involves a sequence of hot-rolling and cold rolling steps, followed by a heat treatment. In the present thesis, the production of a CP1200 steel in an industrial hot dip galvanizing line was studied. The starting point was an industrial CP1100 steel. Samples of this cold rolled steel were analyzed by quenching dilatometry to obtain the CCT curve. Using the dilatometric data, a new heat treatment was proposed and done at CSN facilities, successfully producing a CP 1200 steel. Tension, hardness, bending and hole expansion tests were performed to measure the mechanical properties of the new steel. The microstructural characterization was done using light optical microscopy (LOM), scanning electron microscopy (SEM), atomic force microscopy (AFM), electron backscattering diffraction (EBSD) and transmission electron microscopy (TEM); neural networks and digital image processing were used to quantify the obtained micrographs. The increase in tension and yielding strengths was explained based on the higher amounts of bainite as well as of bainite-ferrite and bainite-martensite interfaces, found to be less prone to void nucleation.

Automotive companies are actively pursuing to increase the use of high-strength-lightweight alloys such as aluminum, magnesium, and advanced/ultra high-strength steels (A/UHSS) in body panel and structural part applications to achieve fuel efficiency while satisfying several environmental and safety concerns. A/UHSS sheet materials with higher strength and crashworthiness capabilities, in comparison to mild steel alloys, are considered as a near-term (i.e., ~5 years) choice of material for body and structural components due to their relatively low cost when compared with other lightweight materials such as aluminum and magnesium. However, A/UHSS materials present an increased level of die wear and springback in stamping operations when compared to the currently used mild steel alloys due to their higher surface hardness and high yield strength levels. In order to prevent the excessive wear effect in stamping dies, various countermeasures have been proposed such as alternative coatings, modified surface enhancements in addition to the use of newer die materials including cast, cold work tool, and powder metallurgical tool steels. In this study, a new die wear test method was developed and tested to provide a cost-effective solution for evaluating various combinations of newly developed die materials, coatings and surfaces accurately and rapidly. A new slider type of test system was developed to replicate the actual stamping conditions including the contact pressure state, sliding velocity level and continuous and fresh contact pairs (blank-die surfaces). Several alternative die materials in coated or uncoated conditions were tested against different AHSS sheet blanks under varying load, sliding velocity circumstances. Prior to and after wear tests, several measurements and tribological examinations were performed to obtain a quantified performance evaluation using commonly adapted wear models. Analyses showed that (1) the rapid wear method is feasible and results in reasonable wear assessments, (2) uncoated die materials are prone to expose severe form wear (galling, scoring, etc.) problems; (3) coated samples are unlikely to experience such excessive wear problems, as expected; (4) almost all of the the recently developed die materials (DC 53, Vancron 40, Vanadis 4) performed better when compared to conventional tool steel material AISI D2, and (5) in terms of coating type, die materials coated with thermal diffusion (TD) and chemical vapor deposition (CVD) coatings performed relatively better compared to other tested coating types; (6) It was seen that wear resistance correlated with substrate hardness.

Advanced high strength steels (AHSS) have high susceptibility to hydrogen embrittlement, and are often exposed to hydrogen environments in processing. In order to study the embrittlement and recovery of steel, tensile tests were conducted on two different types of AHSS over time after hydrogen charging. Concentration measurements and hydrogen microprinting were carried out at the same time steps to visualize the hydrogen behavior during recovery. The diffusible hydrogen concentration was found to decay exponentially, and equations were found for the two types of steel. Hydrogen concentration decay rates were calculated to be -0.355 /hr in TBF steel, and -0.225 /hr in DP. Hydrogen concentration thresholds for embrittlement were found to be 1.04 mL/100 g for TBF steel, and 0.87 mL/100g for DP steel. TBF steel is predicted to recover from embrittlement within 4.1 hours, compared to 7.2 hours in DP steel. A two-factor method of evaluating recovery from embrittlement, requiring hydrogen concentration threshold and decay rate, is explained for use in predicting recovery after exposure to hydrogen. Anisotropic hydrogen diffusion rates were also observed on the surface of both steels for a short time after charging, as hydrogen left the surface through <001> and <101> grains faster than grains with <111> orientations. This could be explained by differences in surface energies between the different orientations.

The ductility of Q&P 1180 steel was studied with regard to retained austenite transformation under different strain paths. Specimens were tested in uniaxial tension in a standard test frame as well as in situ in the scanning electron microscope (SEM). Then digital image correlation (DIC) was used to compute the effective strain at the level of the individual phases in the microstructure. Stretching experiments were also performed using limiting dome height (LDH) tooling, where specimens were strained in both biaxial and plane strain tension. The experiments were done incrementally, for each strain path, and the retained austenite at each level of strain was measured using electron backscatter diffraction (EBSD). Retained austenite levels in the uniaxial tension case dropped from an initial measured level of about 8% to about 2% during an initial strain increment of 0.02, but then stabilized as the specimen was strained to 0.1. In the plane strain and biaxial tension cases retained austenite also dropped significantly during an initial strain increment of about 0.04, but then continued to decrease as the specimens were strained to failure. Biaxial tension, in particular, was the most effective strain path for transforming retained austenite to martensite, resulting in a final volume fraction of 0.3% at an effective strain of 0.3. Retained austenite in the plane-strain tension case dropped at a faster rate than in the biaxial tension case, but finished at about 1% at a strain of 0.1. The greatest limit strains were seen in the biaxial tension case, which may be partly explained by the more effective conversion of retained austenite than was seen in the uniaxial tension case.

The Latin American steel making company Ternium S.A. aims to develop and produce a new type of advanced high strength steel (AHSS) in which the main alloying elements are carbon, aluminium, manganese, and silicon. The present work is the first phase of the development project and it involves casting and characterization of four steel compositions with varying amounts of the aforementioned elements. The results revealed that the Mn-content had a large impact on the development of hard phases during solidification. A steel with a Mn-content of 2 %wt. had almost completely transformed to pearlite during cooling, while a steel with a 4 %wt. Mn-content consisted of primarily martensite and retained austenite. Only the impact of the Mn-content is evaluated. The columnar grain size for two of the four steel compositions were in the range of 20-30 mm, which is similar to those observed from continuous casting. This indicate that the heat transfer rate was slow enough to allow these grains to grow. Measurements during casting showed an initial cooling rate of 10-20°C/min at a distance of 10 mm inside the ingot, which is much slower than the surface cooling rate during continuous casting (100-150°C/min). It was assumed that the cooling rate was similar for all castings since the methodology was identical. However, the steel used for cooling rate measurements was not characterized, why a correlation between cooling rate and composition could not be obtained. A heat transfer model was developed to gain further knowledge of the solidification process. As a reference to the heat transfer model, a eutectic Bi-42Sn alloy was cast with temperaturemonitoring using a casting setup identical to that of the steel castings. A similar cooling rate tothe Bi-42Sn reference casting was obtained where the cooling was faster from above of the ingot than below. Thus, the last part of the metal to solidify during the simulation was situated in the lower half of the ingot. This provides a model for testing future steel compositions.

When developing an electric vehicle, it is essential to evaluate the deformation in and around the battery box for different crash scenarios, and it is necessary to develop a more advanced model that would take into account all the stress modes. Thanks to the excellent properties of Advanced High Strength Steel (AHSS) combine with high strength for more safety and weight reduction for less exhaust emission, AHSS is more and more commonly used in automobile industry. The material employed in this project is DOCOL 900M and it is a martensitic steel with yield strength higher than 700MPa.  The focus of the current work is to describe the experimental setup for the GISSMO model used in LS-DYNA. A number of experimental methods and theories have been reviewed. Different geometries of the test specimens under different stress triaxialities have been discussed. The study also compares the accuracy and robustness of each of the testing methods and setups. The effect of anisotropy of materials on the mechanical properties was studied. Some summaries about how to reduce errors in the experiment under the conditions of low costing and high efficiency have been discussed. According to the stress-strain response of ductile materials, the parameters of plasticity model can be calibrated. The material can be implemented in finite element software to calibrate the parameters of damage and the prediction of material failure can be achieved. The experiment and simulation are always good to be used together in the research.

TBF 1180 steel was studied under various conditions focusing on the correlation of ductility and amount of retained austenite. Samples were prepared from sheet stock and then strained using limiting dome height tooling (LDH), a standard uniaxial test frame, and a tensile stage for use in an electron microscope. The steel was observed in plane, biaxial, and uniaxial strain to determine its effect on retained austenite transformation and ultimately, ductility. Retained austenite was observed using a scanning electron microscope (SEM) equipped with an electron backscatter detector (EBSD) to distinguish the different phases present. Initial austenite levels were around 5% by volume and was quickly reduced as the sample was strained. The biaxial samples were the slowest to transform, having about 2.5% austenite at .05 effective strain, which allowed the specimen to reach an effective strain of .3 with 1.1% austenite remaining. In contrast, the plane strain samples had the fastest rate of transformation having only 1.2% austenite at .05 effective strain and .7% austenite at a final effective strain of .18. Both forms of uniaxial, (in-situ and ex-situ), were near identical, as expected, and exhibited an austenite transformation curve between that of the plane and biaxial curves. The uniaxial austenite level at .05 strain was 2.1% and was able to reach about .15 strain with a final austenite percentage around 1%. It was concluded that the biaxial strain path had the greatest ductility due in part to its slower austenite transformation rate while plane and uniaxial strain paths were not as ductile with their faster austenite transformation rates.

Multiple strain path changes during forming lead to complex geometrically necessary dislocation (GND) development in strain gradient fields, inducing internal stresses that contribute to the Bauschinger effect, residual stresses, and springback which alters the final geometrical shape of the part. In order to analyze and design improved processing routes, models must capture the evolution of these internal stresses. However, most models capture the effects of these stresses via phenomenological approaches that require calibration to each new material and strain path. The development of models that capture the underlying physics at the sub-grain level is underway but requires in-depth studies of dislocation behavior (at the relevant meso length scale) in order to guide and validate them. The novel experimental campaign central to this thesis aims to tackle this problem by capturing unprecedented data of dislocation activity for several sheet metals during multiple strain path deformation. The resultant insights provide a new window into multi-path forming of metals, while also aiding the development and validation of two crystal plasticity (CP) models by collaborators at the University of New Hampshire (UNH). The models incorporate internal stresses at the grain and sub-grain levels, respectively. The hardening response due to strain path change during forming of AA6016-T4 was studied at the macro- and micro-level via combined experiments and an elasto-plastic self-consistent (EPSC) model. The experiments demonstrated that possible recombination and/or redirection of dislocations onto different slip systems under strain path change allowed for a gradual elasto-plastic transition, in comparison to a much sharper response upon continued deformation under the same strain path due to buildup and immediate activation of backstresses. The phenomenological backstress law of the EPSC model underpredicted the yield stress response for the strain path change deformations, possibly due to missing sub-grain GND development and an accurate description of associated backstresses. A more detailed experimental study of multi-path deformation for the AA6016-T4 was required in order to guide development of a strain gradient elasto-visco plasticity self-consistent model (SG-EVPSC); the model includes sub-grain strain gradient fields, and related internal stress fields. Total dislocation and GND density were tracked at various points of the deformation, and a complete 3D statistical volume element was characterized, to enable accurate modeling of the microstructure. The tests revealed a relatively lower yield stress response following strain path change, presumably aided by lower latent hardening than self hardening; the tests then showed a rapid accumulation of dislocations on the newly activated slip systems resulting in much higher final dislocation density without affecting the ductility of the pre-strained material. Interestingly, GND development was dominated by the precipitates instead of grain boundaries. These observations are vital for an accurate forming prediction from CPFEA models. Finally, optimized forming conditions of continuous bending under tension produced a ratcheting strain path resulting in a gradual GND development and a more complete retained austenite transformation in quenched-&-partitioned- and TRIP-assisted bainitic ferritic-1180 steels increasing their ductility by at least 360%.

Third-generation advanced high-strength steels (3G AHSS) are being developed to assist in vehicle light weighting so that fuel efficiency may be improved without sacrificing passenger safety. 3G-AHSS have received significant interest from the automotive industry as a critical candidate for their unique combination of high strength and ductility. However, due to selective oxidation of the principal alloying elements such as Mn, Si, Al, and Cr at the steel surface during the annealing stage prior to immersion in the galvanizing Zn(Al, Fe) bath, the process of continuous hot-dip galvanizing of these steel is challenging. This thesis determined the influence of annealing process parameters such as oxygen partial pressure and annealing time, on the selective oxidation and reactive wetting of an Fe-0.15C-5.56Mn-1.17Si-1Al (wt%) prototype 3G AHSS during intercritical annealing as well as continuous galvanizing. Simulated annealing and galvanizing were conducted on the prototype Fe-0.15C-5.56Mn-0117Si-1Al (wt%) 3G steel; Intercritical annealing heat treatments were carried out at 690˚C in a N2-5 vol pct H2 process atmosphere under dew points of 223 K (–50 °C), 243 (–30 °C) and 268 K (–5 °C). MnO was the major oxide formed at the outmost layer of the external oxides on all annealed samples. The experimental parameters, on the other hand, had a substantial impact on the morphology, distribution, thickness, and surface oxide coverage. The greatest Mn surface concentration as well as maximum surface oxide coverage and thickness was obtained by annealing the panels under the 223 K (–50 °C) and 243 (–30 °C) dp process atmospheres. The oxides formed under these process atmospheres largely comprised coarse, compact, and continuous film nodules. In contrast, MnO nodules formed under the 268 K (–5 °C) dewpoint process, exhibited wider spacing between finer and thinner nodules, which was consistent with the internal oxidation mode, while under 223 K (–50 °C) dp process atmosphere, generally external oxidation took place. Poor reactive wetting was obtained for the panels annealed under the 223 K (–50 °C) dp process atmosphere for both the 60 s and 120 s holding times as well as the 243 K (–30 °C) dp process atmosphere for 120 s. This was attributed to the formation of a thick, compact oxide layer on the steel surface, which acted as a barrier between the substrate and Zn bath, preventing Fe dissolution from the substrate surface for the formation of the desired Fe2Al5Znx interfacial layer. However, a well-developed interfacial Fe-Al intermetallic layer was formed under the 268 K (–5 °C) and 243 (–30 °C) dp process atmospheres for intercritical annealing times of 60 s, which is indicative of a good reactive wetting since the thinner and nodule-like oxides on the steel surface after annealing encourage the reactive wetting. External oxides morphology plays a dominant role in facilitating the contact between Zn-alloy bath and the substrate via different mechanisms such as aluminothermic reduction which occurred for the sample annealed under the 268 K (–5 °C) dp process atmosphere. / Thesis / Master of Applied Science (MASc)