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.

The present study focuses on developing a relationship between process variables, mechanical properties and post weld microstructure in Friction Stir Welded HSLA 65 steel. Fully consolidated welds can be produced in HSLA 65 steel by PCBN Convex-Scrolled-Shoulder-Step-Spiral (CS4) tool over a wide range of parameters. Microstructures in the nugget center (NC) are dominated by lath bainite and a few polygonal/allotriomorphic grain boundary ferrites. FSW dependent variables are related to FSW independent variables by non-linear relationship. Heat input is identified to be the best parameter index to correlate with microstructures. With increasing heat input, the volume of bainite is reduced, the shape of bainite is more curved and grain/lath size become coarser. A linear relationship was established between heat input and semi-quantitative post-weld microstructures based on the optical microstructures. Further analysis has been applied on the NC to obtain more fundamental understanding of FSW. The new approach via Orientation Imaging Microscopy (OIM) was developed to acquire quantitative microstructural data including bainite lath/packet and prior austenite grain size (PAG). A linear relationship between heat input and quantitative microstructural features in the NC have been established. Mechanical properties exhibits linear relationship with heat input. These correlations can be utilized to determine FSW weld parameter to get desired mechanical properties welds.

Polycrystalline NiTi shape memory alloys have the ability to recover their original, pre-deformed shape in the presence of external loads when heated through a solid-solid phase transformation from a lower-symmetry B19' martensite phase to a higher-symmetry B2 austenite phase. The strain associated with a shape memory alloy in an actuator application typically has thermal, elastic and inelastic contributions. The objective of this work was to investigate the aforementioned strains by recourse to in situ neutron diffraction experiments during selected combinations of heating, cooling and/or mechanical loading. The primary studies were conducted on polycrystalline Ni49.9Ti50.1 specimens on the Spectrometer for MAterials Research at Temperature and Stress (SMARTS) at Los Alamos National Laboratory. Quantitative information on the phase-specific strain, texture and phase fraction evolution was obtained from the neutron data using Rietveld refinement and single-peak analyses, and compared with macroscopic data from extensometry. First, the lattice strain evolution during heating and cooling in an unloaded sample (i.e., free-recovery experiment) was studied. The lattice strain evolution remained linear with temperature and was not influenced by intergranular stresses, enabling the determination of a thermal expansion tensor that quantified the associated anisotropy due to the symmetry of B19' NiTi. The tensor thus determined was subsequently used to obtain an average coefficient of thermal expansion that was consistent with macroscopic dilatometric measurements and a 30,000 grain polycrystalline self-consistent model. The accommodative nature of B19' NiTi was found to account for macroscopic shape changes lagging (with temperature) the start and finish of the transformation. Second, the elastic response of B19' martensitic NiTi variants during monotonic loading was studied. Emphasis was placed on capturing and quantifying the strain anisotropy which arises from the symmetry of monoclinic martensite and internal stresses resulting from intergranular constraints between individual variants and load re-distribution among variants as the texture evolved during variant reorientation and detwinning. The methodology adopted took into account both tensile and compressive loading given the asymmetric response in the texture evolution. Plane specific elastic moduli were determined from neutron measurements and compared with those determined using a self-consistent polycrystalline deformation model and from recently reported elastic stiffness constants determined via ab initio calculations. The comparison among the three approaches further helped understand the influence of elastic anisotropy, intergranular constraint, and texture evolution on the deformation behavior of polycrystalline B19' NiTi. Connections were additionally made between the assessed elastic properties of martensitic NiTi single crystals (i.e., the single crystal stiffness tensor) and the overall macroscopic response in bulk polycrystalline form. Lastly, the role of upper-cycle temperature, i.e., the maximum temperature reached during thermal cycling, was investigated during load-biased thermal cycling of NiTi shape memory alloys at selected combinations of stress and temperature. Results showed that the upper-cycle temperature, under isobaric conditions, significantly affected the amount of transformation strain and thus the work output available for actuation. With the objective of investigating the underlying microstructural and micromechanical changes due to the influence of the upper-cycle temperature, the texture evolution was systematically analyzed. While the changes in transformation strain were closely related to the evolution in texture of the room temperature martensite, retained martensite in the austenite state could additionally affect the transformation strain. Additionally, multiple thermal cycles were performed under load-biased conditions in both NiTi and NiTiPd alloys, to further assess and understand the role of retained martensite. Dimensional and thermal stabilities of these alloys were correlated with the volume fraction and texture of retained martensite, and the internal strain evolution in these alloys. The role of symmetry, i.e., B19' monoclinic martensite vs. B19 orthorhombic martensite in these alloys was also assessed. This work not only established a methodology to study the thermal and elastic properties of the low symmetry B19' monoclinic martensite, but also provided valuable insight into quantitative micromechanical and microstructural changes responsible for the thermomechanical response of NiTi shape memory alloys. It has immediate implications for optimizing shape memory behavior in the alloys investigated, with extension to high temperature shape memory alloys with ternary and quaternary elemental additions, such as Pd, Pt and Hf. This work was supported by funding from NASAÂ s Fundamental Aeronautics Program, Supersonics Project (NNX08AB51A) and NSF (CAREER DMR-0239512). It benefited additionally from the use of the Lujan Neutron Scattering Center at Los Alamos National Laboratory, which is funded by the Office of Basic Energy Sciences (Department of Energy) and is operated by Los Alamos National Security LLC under DOE Contract DE-AC52-06NA25396.

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<p>Molecular dynamics (MD) simulations performed on two-phase simulation cells were used to compute the Austenite (FCC) / Ferrite (BCC) boundary mobility in pure iron (Fe) over the temperature range of 600K - 1400K. An embedded atom method interatomic potential was used to model Fe and the driving force for interface motion is the free energy difference between the two phases, which was computed as a function of temperature using a thermodynamic integration technique. For low index FCC/BCC crystallographic orientations, no interface motion was observed. But for slight misorientations steps were introduced at the interphase and sufficient mobility was observed over MD time scales. A new interphase mechanism was found that instead of the moving of structure disconnection by diffusion control, growing of misfit dislocations in each steps were observed (interphase control). The interphase velocity could reach 2 m/s and the mobility at 1000K was approximately 0.001 mol-m/J-s. In agreement with previous MD studies of grain boundary mobility, we found that the activation energy for the austenite-ferrite boundary mobility was much lower than the values found from previous experiments.</p> / Master of Applied Science (MASc)

O aço maraging é conhecido pela sua alta resistência mecânica proveniente da formação de precipitados intermetálicos como Ni3Ti e Fe2Mo durante o envelhecimento, porém com subsequente perda de tenacidade à fratura. Existe uma vasta literatura sobre este tipo de aço, o qual é submetido a diversos tratamentos térmicos. Normalmente dois tratamentos térmicos são aplicados: uma homogeneização inicial para solubilização dos precipitados, sendo a recomendação geral 820 °C/1 h, e posteriormente o tratamento de envelhecimento, variando a temperatura de 455 °C a 510 °C e o tempo de 3 a 12 h. No entanto, pode haver variações no tratamento, como aquecimento após homogeneização numa faixa de temperatura intercrítica ou abaixo da Ac1 visando a reversão da martensita em austenita e o refino de grão. Até o presente momento, não está bem definida a influência da temperatura/tempo em tratamentos de temperaturas inter ou subcríticas que visam o refinamento da estrutura e o aumento da austenita retida/reversa. A literatura mostra tratamentos na liga maraging 300 por meio de estudos mais antigos, da década de 70 e 80, utilizando aquecimentos curtos e cíclicos para reversão e estabilização da austenita reversa. Estudos mais recentes de outras ligas utilizaram tratamentos isotérmicos para difusão e reversão da martensita em austenita. Nesta proposta serão pesquisadas as duas rotas de tratamento, cíclica e isotérmica, para avaliar a reversão martensita-austenita. Os tratamentos cíclicos foram caracterizados por EBSD, MEV e difração de raio-X ex-situ. Os tratamentos isotérmicos foram caracterizados por EBSD e difração de raio-X de fonte sincrotron in-situ, ou seja, medida em tempo real durante o tratamento. Ambas as condições foram avaliadas mecanicamente por meio de ensaios de flexão de 3 pontos. / Maraging steel is known for its high mechanical strength resulting from the formation of intermetallic precipitates such as Ni3Ti and Fe2Mo during aging heat treatment, with subsequent loss of fracture toughness. There is a vast literature on this type of steel, which is subjected to various thermal treatments. Normally two heat treatments are applied: an initial homogenization for solubilization of the precipitates, the general recommendation being 820 ° C/1 h, and later the aging treatment, varying temperature from 455 ° C to 510 ° C and time of treatment from 3 to 12 hours. However, there may be applied other heat treatments, such as heating after homogenization in an intercritical temperature range or below Ac1 for the reversion of martensite-to-austenite and grain refinement. To date, the influence of temperature and time on inter- or subcritical temperature treatments aiming at grain refinement and martensite-to-austenite reversion is not well defined. The literature shows treatments in the maraging 300 alloy, from the 70s and 80s, using short and cyclic heat treatment for reversion and stabilization of austenite. Recent studies of other alloys have used isothermal treatments for diffusion and martensite-to-austenite revresion. In this study, two heat treatment routes, cyclical and isothermal, were investigated to evaluate the martensite-to-austenite reversion. Cyclic treatments were characterized by EBSD, SEM and ex-situ X-ray diffraction. The isothermal treatments were characterized by EBSD and X-ray diffraction of synchrotron source in-situ, that is, measured in real time during the treatment. Both conditions were mechanically evaluated by 3-point-bending tests.

This thesis concerns the mathematical modelling of phase transformations with a special emphasis on martensitic phase transformations and their application to the modelling of steels. In Chapter 1, we develop a framework that determines the optimal transformation strain between any two Bravais lattices and use it to give a rigorous proof of a conjecture by E.C. Bain in 1924 on the optimality of the so-called Bain strain. In Chapter 2, we review the Ball-James model and related concepts. We present some simplification of existing results. In Chapter 3, we pose a conjecture for the explicit form of the quasiconvex hull of the three tetragonal wells, known as the three-well problem. We present a new approach to finding inner and outer bounds. In Chapter 4, we focus on highly compatible, so called self-accommodating, martensitic structures and present new results on their fine properties such as estimates on their minimum complexity and bounds on the relative proportion of each martensitic variant in them. In Chapter 5, we investigate the contrary situation when self-accommodating microstructures do not exist. We determine, whether in this situation, it is still energetically favourable to nucleate martensite within austenite. By constructing different types of inclusions, we find that the optimal shape of an inclusion is flat and thin which is in agreement with experimental observation. In Chapter 6, we introduce a mechanism that identifies transformation strains with orientation relationships. This mechanism allows us to develop a simpler, strain-based approach to phase transformation models in steels. One novelty of this approach is the derivation of an explicit dependence of the orientation relationships on the ratio of tetragonality of the product phase. In Chapter 7, we establish a correspondence between common phenomenological models for steels and the Ball-James model. This correspondence is then used to develop a new theory for the (5 5 7) lath transformation in low-carbon steels. Compared to existing theories, this new approach requires a significantly smaller number of input parameters. Furthermore, it predicts a microstructure morphology which differs from what is conventionally believed.

O presente trabalho avaliou o efeito de tratamentos térmicos ou diferentes graus de deformação plástica na transformação da austenita do microconstituinte AM de uma chapa de aço alta resistência baixa liga (ARBL) classe API 5L X80 usada para gasodutos. A chapa tem espessura de 19 mm e passaria pelo processo de conformação UOE, mas a deformação foi realizada por laminação a frio, a temperatura ambiente, com reduções de 5 a 20%. O propósito foi compreender melhor o microconstituinte AM, explorar a transformação martensítica induzida por deformação (SIMT) e a decomposição austenítica por tratamento térmico, com ênfase em seu comportamento magnético. A transformação da austenita foi acompanhada através de medidas de polarização magnética, comparada com a densidade de massa e difração de raios X. A deformação plástica e os tratamentos térmicos alteraram a polarização magnética de saturação e a densidade de massa da amostra de aço de forma compatível com a eliminação da austenita retida metaestável. O método de densidade hidrostática foi considerado sensível para mensurar transformações de fase. Os dados obtidos revelam expansão volumétrica de aproximadamente 0,13%, correspondendo a 3,2% a quantidade de austenita retida original do material, enquanto os valores obtidos por polarização magnética de saturação são 2,8% pelo histeresígrafo e 2,1% por MAV. A difração de raios X nas amostras sob deformação ou tratamentos térmicos resultaram em queda nos primeiros picos da austenita quando comparadas com a amostra como recebida. / This study evaluated the effect of different degrees of plastic deformation or heat treatment on the transformation of austenite into martensite of an HSLA steel plate API 5L X80 for pipelines. A 19 mm thickness plate would be submitted to UOE forming process, but the cold work instead occurred by cold rolling at room temperature, with reductions of 5 up to 20%. The purpose was to better understand the MA constituent, explore the strain-induced martensitic transformation (SIMT) and austenitic decomposition by heat treatment with emphasis on its magnetic behavior. The transformation was accompanied by saturation magnetization measurements, compared with the mass density and X-ray diffraction. The plastic deformation or the heat treatment altered the saturation magnetization and the mass density in a manner consistent with the elimination of metastable retained austenite. The density method is sensible to measure phase transformations induced by strain. The data obtained shows a volumetric expansion of about 0.13%, corresponding to an amount of retained austenite of the original material of 3.2%, while the values obtained by magnetization saturation are 2.8% by hysteresigraph and 2.1% by VSM. By X-ray diffraction there is a clear drop in first peaks of austenite of the samples under deformation or heat treatment compared with the sample as-received.