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Serious issues including solidification porosity, columnar grains, and large grain sizes are common during fusion-based metal additive manufacturing due to the inherent melting and solidification that occurs during printing. In recent years, a high-temperature, rapid plastic deformation technique called additive friction stir deposition (AFSD) has shown great promise in overcoming these issues. Because the deposited material stays in the solid state during printing, there are no melting and solidification events and the process can result in as-printed material that is fully-dense with equiaxed, fine grains. As AFSD is an emerging process, developing an understanding of the synergy between material deformation and the resultant microstructure evolution, especially the strain magnitude, its influence on dynamic microstructure evolution, and material flow details, is imperative for the full implementation of AFSD. Therefore, the purpose of this work is to investigate the severe plastic deformation in AFSD through complementary studies on the concurrent evolution of shape and microstructure during the deposition of dissimilar aluminum alloys. In this work, we systematically study (1) the entire deposition via dissimilar cladding along with (2) specific volumes within the deposited layer via embedded tracers printed at varied processing parameters. X-ray computed tomography and electron backscatter diffraction are employed to visualize the complex shape of the deposits and understand the microstructure progression. Investigation of dissimilar cladding of homogeneous AA2024 feed-rods onto an AA6061 substrate establishes a working understanding of the mechanisms related to material flow and microstructure evolution across the whole deposit (macroscopic shape evolution) as well as at the interface between the deposit and the substrate. Variations in tooling and rotation rate affect the interfacial features, average grain size, and depth of microstructural influence. The non-planar and asymmetric nature of AFSD on the macro-scale is revealed and a maximum boundary of deposited material is established which gives a frame of reference for the next material flow study within the deposition zone. An understanding of the mesoscopic morphological evolution and concurrent dynamic microstructure evolution of representative volumes within the deposition zone is determined by comparing depositions of hybrid feed-rods (AA6061 matrix containing an embedded tracer of AA2024). Samples were printed with and without an in-plane velocity to compare initial material feeding to steady-state deposition. Variations in initial tracer location and tool rotation rate/in-plane velocity pairs affect the final morphology, intensity of mixing, and microstructure of the deposited tracer material. The tracer material undergoes drastic mesoscopic shape evolution from millimeter-scale cylinders to long, curved micro-ribbons. There is simultaneous grain refinement in AA2024 via geometric dynamic recrystallization during initial material feeding, after which the grain size remains relatively constant at a steady-state size. The lower bound of strain is estimated based on extrusion, torsion, and shear-thinning factors. The step-by-step mesoscopic deformation and microstructure evolution is further elucidated by characterizing depositions of hybrid feed-rods with a series of embedded tracers. The AFSD tooling is stopped quickly at the end of the deposition with a quench applied to "freeze" the sample. X-ray computed tomography reveals multiple intermediate morphologies including the progression from a cylinder to a tight spiral, to a flattened spiral shape, and to a thin disc. EBSD mapping shows that a refined microstructure is formed soon after the material leaves to tool head with areas off the centerline reaching a fully recrystallized state more quickly. The findings from this work summarize the current understanding of the link between material deformation and microstructure evolution in AFSD. Hopefully these first fundamental studies on the co-evolution of material flow and grain structure during AFSD can inspire future work, especially in the area of heterogeneous multi-material printing. / Doctor of Philosophy / Additive friction stir deposition (AFSD) is a new metal 3D printing process that uses friction to heat up and deposit materials rather than using a laser to melt the material into place. This is beneficial since it avoids problems that come from melting and solidification (e.g., porosity, hot cracking, residual stresses, columnar grains). Since AFSD is such a new technology, an understanding of some of the fundamental processing science is needed in order to predict and control the performance of the resultant parts. This is because the processing of a material affects its structure (at multiple scales, for example macro-, micro-, atomic) which then affects the properties a material will exhibit which, finally, dictates the performance of the overall part. Therefore, the purpose of this work is to explore how the feed material is transformed and deposited into the final layer after printing and to link the original processing conditions to the resultant structure. To investigate the interface between the deposited layer and the substrate, we use a simple feed-rod of one aluminum alloy (AA2024) and deposit it onto a substrate of another aluminum alloy (AA6061). To look at just one small volume within the deposited layer, we use a hybrid feed-rod that is mostly AA6061 except for small cylinders of AA2024 that are placed either in the center or on the edge of the feed-rod so that we can track the AA2024. Printing these feed-rods under different processing conditions will help us understand the connection between processing and structure. Using a characterization technique called X-ray computed tomography we can visualize a 3D representation of the final position for the AA2024 material. In order to evaluate the structure on the micro-scale, a characterization technique called electron backscatter diffraction is used to show the individual grains of our metal. The main contributions of this work are as follows: 1) a lower bound of strain is estimated for AFSD, 2) various intermediate deformation steps are captured for the tracer cylinders including a progression from cylinder to multiple spiral shapes to a thin disc to long ribbons, 3) these deformation steps are linked to different microstructures, and 4) changing the tool geometry and other processing parameters significantly alters the range of shapes and microstructures developed in the deposited material. These findings bring us closer to a fully controllable system as well as sparking some interesting areas for future research because of the complex shapes we observed. These results could lead to the customization and optimization of 3D spirals, ribbons, etc. designed for a certain application.

Aluminum alloys have increasing applications in construction and transportation industries. Both 5xxx-series (Al-Mg) and 6xxx-series (Al-Mg) alloys are frequently used in marine construction because of their light weight, high strength, and corrosion resistance. One of the major concerns regarding the marine application of aluminum alloys is their mechanical performance in fire scenarios. The material strength may be degraded due to both thermal and mechanical damage during fire exposure. This work emphasizes the stress-induced mechanical (physical) damage and its impact on the residual (post-fire) performance of 5083-H116 and 6061-T651 aluminum alloy. Thermo-mechanical tests were performed at various temperatures and stresses to study the stress-induced damage at induced plastic creep strain levels. Unstressed thermally exposed and thermo-mechanically damaged samples were examined to separate the stress-induced microstructural damage. The stress-induced microstructural damage primarily manifests itself as dynamic recovery at low creep temperatures, while cavitation, dynamic recrystallization and dynamic precipitation (in Al6061) are the types of damage developed in the high creep strains at high exposure temperatures. Different creep mechanisms are also studied for both Al5083 and Al6061. The post-fire mechanical response at room temperature after thermo-mechanical damage was investigated with reference to the damaged microstructure present in the material. Residual material strengths based on deformed cross sectional area after the creep test were calculated to provide insight into how microstructural damage affects the post-fire material performance. The competing effects of strength degradation caused by cavitation and strengthening due to grain elongation and subgrain refinement were investigated. Engineering residual material strengths calculated based on the original cross sectional area prior to creep tests were also studied to provide guidance for structural design. / Ph. D.

Mg-alloys, despite being the lightest structural metallic materials, find limited applications due to their poor workability, which is due to the hcp structure that does not provide sufficient number of independent slip systems for compatible deformation. Workability improves with the increase in the deformation temperature, when non-basal slip starts playing a larger role in deformation. Efforts were made to improve the workability through control of texture, grain refinement and alloying. Alloying activates non-basal slip by decreasing the critical resolved shear stress (CRSS) on non-basal planes or by promoting cross slip through an increase in the stacking fault energy (SFE) on basal planes. In this thesis, the effect of Li addition to the most widely used wrought Mg-alloy AZ31 on its workability is examined. Plastic deformation behaviour of a series of AZ31-Li alloys with temperature, T, and strain rates, ε , as variables was studied, so as to identify the optimum Li content that results in highly workable alloy. The T and ε combinations that are best suited for hot deformation of these alloys were also identified through processing maps and microstructural analysis. First, deformation behaviour of the base AZ31 is examined in detail. Compression tests were carried out, with T ranging between 150 and 400 °C and at ranging from 10-3 to 102 s-1, covering entire hot working range of the alloy. The results suggest that the deformation behaviour of AZ31 could be partitioned into three temperature regimes. In low T regime, twinning played an important role. It changes the orientation and increases hardening rate, θ (given by dσ/dε where σ and ε are true stress and strain respectively); material exhibits macroscopic flow localization and cracking along twin boundaries. The onset of twinning was examined in detail by examining the local maxima before ϵpeak strain in plot between d2σ/dε2 vs. ε. Twinning was found to occur at all the deformation conditions. Dynamic recrystallization (DRX) was observed at temperatures above 250 °C whereas deformation at low T (< 250 °C) led to extensive twinning at all . ε . At intermediate T of 250-300 °C, plastic strains tend to localize near grain/twin boundaries, confining DRX only to these regions. Increase in T promotes non-basal slip, which, in turn, leads to uniform deformation; DRX too becomes uniform. The dependence of critical stress (σc) for the onset of DRX and peak flow stress (σp) on Zener-Hollomon parameter (Z) indicates that these stresses increase with Z. Activation energy (Q) for the deformation of AZ31 was estimated at peak stress and steady state conditions. High values of Q (150-200 kJ/mol) indicate cross slip as the rate controlling mechanism, at the peak, in the stress-strain responses. For steady state, Q corresponds to lattice/grain boundary diffusion (90-150 kJ/mol). Next, the effect of Li on deformation behaviour of AZ31 was examined. In addition to AZ31 without any Li (0Li), three alloys 1 (1Li), 3 (3Li) and 5 (5Li) wt% Li were prepared with the aid of a specially designed set-up for melting and casting of Li containing alloys. Experimental results on homogenized alloys show that 1Li alloy’s overall response is similar to that of 0Li alloy, but 3Li and 5Li alloys exhibit distinctly different deformation behaviour. Li addition facilitates cross slip by increasing SFE on basal planes, thus leading to change in the deformation mechanism of the alloy. Increased softening due to cross slip decreases θ and also the twin density at low ϵ (<10-2 s-1). During deformation at low ϵ and low T, high Li alloys reveal cavities along the grain boundaries in contrast to cracking along twin boundaries that was observed in AZ31. In the intermediate T range, high Li alloys reveal the presence of a small mantle, which can be attributed to the increased cross slip with increasing Li. In fact, Li addition was found to restrict DRX and promote dynamic recovery (DRY). As ϵ increases in this T regime deformation becomes more homogeneous and twinning occurs extensively in high Li alloys. This results in remarkable increase in dσ/dε (θ) in these alloys and DRX was predominantly seen at twinned regions. At high ϵ -T regime, where non-basal slip and twinning occur uniformly, DRX is observed throughout the samples. On the basis of d2σ/dε2 – ε plots, it was found that twinning occurs at almost all -T combinations examined in present study for 0Li and 1Li alloys. In high Li alloys, twinning activity was found to be insignificant at low ε , resulting in low twin density than low Li alloys. Twinning occurs at very early stages of deformation. In the low T and high ε regime, extensive twinning in high Li alloys is noted. In high T regime, presence of twins was not prominent due to the preferential occurrence of DRX at twin boundaries. Estimated values of Q in high Li alloys were found to be very low and correspond to lattice/grain boundary diffusion of Li in Mg, indicating that cross slip is no longer the rate controlling mechanism. Instead, unpinning of kinks from Li atoms appears to control the deformation. Cross slip is promoted by Li through increase in SFE at basal planes. Onset of the DRX was predicted and it was observed that high Li alloys posses lower σc at low ε , but at high ε , σc was either comparable to or higher than low Li alloys. Processing maps were generated for all the alloys using Prasad's as well as Murty's models. Instability predictions of Prasad’s and Murty’s models are similar, except that isoefficiency contours in the latter are slightly shifted to higher ε . These maps indicate to an increase in the workability with the addition of Li to AZ31. Instability predicted by processing maps in the low ε regime in high Li alloys is attributed to underestimation of stress values due to spline interpolation. High sensitivity observed for high Li alloy at intermediate ε (10-1 – 100 s-1) is attributed to the change in the deformation mode i.e. from slip to twinning. Deformation at high T leads to dissolution of Li containing precipitates, which in turn increases the solid solution strengthening in the alloy. Hence, increase in flow stress is observed with increase in T in high Li alloys. This structural change too causes instability predictions in the high -T regime. The 0 Li alloy exhibits peak efficiency of 45% in T = 250-400 °C and ε = 10-1.25 - 100.25 s-1 regime. DRX is observed in this regime and optimum conditions for deformation predicted for this alloys are T = 350 °C and ε = 10-1 s-1. These alloys can be worked at low ε regime too (T = 250-400 °C and ε = 10-2.5 – 10-1 s-1) where the softening mechanism is DRY. Accordingly, it is concluded that the intrinsic workability of AZ31Mg-alloy increases with the addition of 3% and 5% Li.

Au cours de leur mise en forme, les alliages de titane destinés à la fabrication de pièces tournantes pour moteurs d'avions suivent un schéma thermomécanique complexe constitué généralement de plusieurs opérations de forgeage. L'étape de forgeage dans le domaine monophasé β joue un rôle important, car elle conditionne la transformation de phases qui s'opère au cours du refroidissement ou du traitement thermique consécutif dans le domaine biphasé α-β, et donc les propriétés mécaniques finales de la pièce. La maîtrise de l'évolution de la microstructure et de la texture cristallographique au cours du forgeage dans le domaine β est donc indispensable pour optimiser l'ensemble du procédé de mise en forme. Pour cela, il est important de bien comprendre les mécanismes de recristallisation dynamique (continue et géométrique) se produisant dans ce type de matériau.Dans cette étude, les effets de la température, de la déformation et de la vitesse de déformation ont été étudiés au moyen d'essais de compression uniaxiale et de torsion à chaud. Les microstructures et textures de déformation ont été caractérisées par diffraction des électrons rétrodiffusés (EBSD). Ces approches expérimentales sont associées à un travail de modélisation, pour lequel le schéma de recristallisation dynamique "continue" (ou CDRX), consistant en une fragmentation progressive des grains β initiaux par la formation de nouveaux joints de grains, a été adapté à partir d'études antérieures. Les paramètres caractérisant les mécanismes élémentaires de la CDRX (écrouissage, restauration dynamique, migration des joints) ont été déterminés par ajustement sur les données expérimentales.Ces travaux ont pour objectif l'élaboration d'un post-processeur métallurgique dédié au forgeage des alliages de titane en phase β. / Titanium alloys used for the manufacture of rotating parts of aircraft engines undergo complex thermomechanical processing schedules, involving usually several forging operations. The forging step in the single -phase domain plays an important role, because it governs the phase transformation that occurs during cooling or subsequent heat treatment in the two-phase α+β range, and therefore the final mechanical properties of the workpiece. Controlling the microstructural evolutions during forging in the β-domain is of prime interest to optimize the entire process of disks manufacture. A full understanding of the (continuous and geometric) dynamic recrystallization mechanisms occurring in this type of material is therefore required.In this study, the effects of temperature, strain and strain rate were investigated by hot uniaxial compression and torsion tests. The microstructures and textures were characterized using backscattering electron diffraction (EBSD). These experimental approaches were associated with the development of a physical model. In the latter, the mechanism of "continuous" dynamic recrystallization (CDRX), consisting of a progressive initial fragmentation of the grains leading to the formation of new grain boundaries, was adapted from former studies. The parameters characterizing the elementary mechanisms of CDRX (strain hardening, dynamic recovery, grain boundary migration) were determined by fitting the experimental data.The final objective of this work is to develop a metallurgical post-processor dedicated to forging operations of titanium alloys in the -phase range.

This thesis contains the development of a physically-based model describing the microstructural evolution during hot deformation of microalloyed steels. The work is mainly focused on the recrystallization kinetics. During hot rolling, the repeated deformation and recrystallization provides progressively refined recrystallized grains. Also, recrystallization enables the material to be deformed more easily and knowledge of the recrystallization kinetics is important in order to predict the required roll forces. Hot strip rolling is generally conducted in a reversing roughing mill followed by a continuous finishing mill. During rolling in the roughing mill the temperature is high and complete recrystallization should occur between passes. In the finishing mill the temperature is lower which means slower recrystallization kinetics and partial or no recrystallization often occurs. If microalloying elements such as Nb, Ti or V are present, the recrystallization can be further retarded by either solute drag or particle pinning. When recrystallization is completely retarded and strain is accumulated between passes, the austenite grains will be severely deformed, i.e. pancaking occurs. Pancaking of the grains provides larger amount of nucleation sites for ferrite grains upon transformation and hence a finer ferrite grain size is achieved. In this work a physically-based model has been used to describe the microstructural evolution of austenite. The model is built-up by several sub-models describing dislocation density evolution, recrystallization, grain growth and precipitation. It is based on dislocation density theory where the generated dislocations during deformation provide the driving force for recrystallization. In the model, subgrains act as nuclei for recrystallization and the condition for recrystallization to start is that the subgrains reach a critical size and configuration. The retarding effect due to elements in solution and as precipitated particles is accounted for in the model. To verify and validate the model axisymmetric compression tests combined with relaxation were modeled and the results were compared with experimental data. The precipitation sub-model was verified by the use of literature data. In addition, rolling in the hot strip mill was modeled using process data from the hot strip mill at SSAB Strip Products Division. The materials investigated were plain C-Mn steels and Nb microalloyed steels. The results from the model show good agreement with measured data. / QC 20100706

<p>Recrystallization kinetics, during and after hot deformation, has been investigated for decades. From these investigations several equations have been derived for describing it. The equations are often empirical or semi-empirical, i.e. they are derived for certain steel grades and are consequently only applicable to steel grades similar to these. To be able to describe the recrystallization kinetics for a variety of steel grades, more physically based models are necessary.</p><p>During rolling in hot strip mills, recrystallization enables the material to be deformed more easily and knowledge of the recrystallization kinetics is important in order to predict the required roll forces. SSAB Tunnplåt in Borlänge is a producer of low-carbon steel strips. In SSAB’s hot strip mill, rolling is conducted in a reversing roughing mill followed by a continuous finishing mill. In the reversing roughing mill the temperature is high and the inter-pass times are long. This allows for full recrystallization to occur during the inter-pass times. Due to the high temperature, the rather low strain rates and the large strains there is also a possibility for dynamic recrystallization to occur during deformation, which in turn leads to metadynamic recrystallization after deformation. In the finishing mill the temperature is lower and the inter-pass times are shorter. The lower temperature means slower recrystallization kinetics and the shorter inter-pass times could mean that there is not enough time for full recrystallization to occur. Hence, partial or no recrystallization occurs in the finishing mill, but the accumulated strain from pass to pass could lead to dynamic recrystallization and subsequently to metadynamic recrystallization.</p><p>In this work a newly developed physically based model has been used to describe the microstructural evolution of austenite. The model is based on dislocation theory where the generated dislocations during deformation provide the driving force for recrystallization. The model is built up by several submodels where the recrystallization model is one of them. The recrystallization model is based on the unified theory of continuous and discontinuous recovery, recrystallization and grain growth by Humphreys.</p><p>To verify and validate the model, rolling in the hot strip mill was modeled using process data from SSAB’s hot strip mill. In addition axisymmetric compression tests combined with relaxation was modeled using experimental results from tests conducted on a Gleeble 1500 thermomechanical simulator at Oulu University, Finland. The results show good agreement with measured data.</p>

Made available in DSpace on 2014-06-11T19:32:21Z (GMT). No. of bitstreams: 0 Previous issue date: 2003-08-15Bitstream added on 2014-06-13T20:23:37Z : No. of bitstreams: 1 almeida_hl_dr_rcla.pdf: 806140 bytes, checksum: 7940276ecd62a931d89c15464ccc97db (MD5) / Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) / A zona de cisalhamento Itapetim (ZCI) desenvolveu foliação e lineação nos diferentes tipos de rochas, milonitos a ultramilonitos. Muitos dos tipos de microestruturas observadas na ZCI preservam evidências de condições metamórficas de alto grau e baixo grau de temperatura. O padrão das orientações preferenciais dos eixos [c] de quartzo, obtida a partir de agregados policristalinos deformados, mostra dois diferentes tipos de simetrias, guirlandas do tipo I e simples. A análise da textura sugere partição da deformação com cisalhamento coaxial e não coaxial na ZCI. Um veio de quartzo mineralizado em ouro encaixado em rocha ultramilonítica, constitui a zona de precipitação hidrotermal. O veio é bandado por segmentos de turmalina, o qual inclui agregados de grãos de quartzo maciço entre as bandas. Os grãos de quartzo mostram contatos poligonais e restritos limites intumescentes. O último sugere recristalização dinâmica por migração de limite de grão e os grãos poligonais (microestrutra em espuma) são melhor explicados por annealing. Os padrões de eixos [c] de quartzo obtido no veio aurífero é idêntico ao observado nos ultramilonitos da ZCI. Este padrão é interpretado como uma textura preservada formada durante o cisalhamento não coaxial. A estrutura bandada é interpretada como o resultado de variações da pressão de fluidos e a formação microfraturas, associadas a eventos de crack-seal. Mecanismos de crack-seal foram ativos antes ou durante a deformação da ZCI. As feições microestruturais suportam evidências para a última possibilidade. / The Itapetim shear zone(ISZ) developed both foliation and lineation in the different rock types, from mylonites to ultramylonites. Most of the microstructure types observed in the ISZ preserve evidence of high temperature metamorphic conditions. The quartz [c]-axis, of deformed polycrystalline aggregates, show two distinct symmetries, type I crossed girdles and single girdles. The geometrical analysis of texture, suggest non-coaxial shear for deformation in ISZ. A gold mineralized quartz vein hosted in ultramylonitic rocks, constitutes the hydrothermal precipitation zone. The vein is banded by tourmiline segments, which include massive quartz grains aggregates between the bands. The quartz grains show polygonal contacts and minor intumescent limits. These latter suggest grain boundary migration recrystallization and the polygonal grains seem to be best explained by the annealing after stopping the shear deformation. The quartz [c]-axis obtained in the auriferous vein shows the same single girdle pattern observed in the ultramylonites of the ISZ. This pattern is interpreted as a preserved texture formed during the shear deformation. The banded structure is interpreted as the result of variations of the fluid pressure and the formation of microfractures, associated the crack-seal events. Crack-seal mechanisms can have been active previous or during the deformation of the IZS. The microstructurals features supports evidences for the last possibility.

京都大学 / 0048 / 新制・課程博士 / 博士(工学) / 甲第21767号 / 工博第4584号 / 新制||工||1714(附属図書館) / 京都大学大学院工学研究科材料工学専攻 / (主査)教授 辻 伸泰, 教授 乾 晴行, 教授 安田 秀幸 / 学位規則第4条第1項該当 / Doctor of Philosophy (Engineering) / Kyoto University / DFAM

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