none

The present work aims to reveal the microstructural evolution and post-processing mechanical behavior of difficult-to-work alloys upon severe plastic deformation. Severe plastic deformation is applied using equal channel angular extrusion (ECAE) where billets are pressed through a 90o corner die achieving simple shear deformation. Three different materials are studied in this research, namely Ti-6Al-4V, Ti-6Al-4V reinforced with 10% TiC and AISI 316L stainless steel. Microstructure and mechanical properties of successfully extruded billets were reported using light microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), tension and compression experiments and microhardness measurements. The effects of extrusion conditions (temperature and processing route) on the microstructure and mechanical properties are investigated. The underlying mechanisms responsible for observed mechanical behaviors are explored. It is seen that ECAE shear deformation leads to refinement in α plates and elimination of prior β boundaries in Ti-6Al-4V. Decreasing extrusion temperature and increasing number of passes decreases α plate size and grain size. Refined α grain size leads to a significant increase in tensile and compressive flow stresses at room temperature. Texture produced by ECAE has a pronounced effect on mechanical properties. Specifically it leads to tension/compression asymmetry in flow strengths and strain hardening coefficients may be described by the activation of differing slip systems under tension and compression loading. ECAE of Ti-6Al-4V+10%TiC samples also improved mechanical properties due to α plate size refinement. Nevertheless, further extrusion passes should be carried out for tailoring reinforcement size and distribution providing optimum strength and ductility. ECAE deformation of AISI 316L stainless steel at high homologous temperatures (0.55 to 0.60 Tm) results in deformation twinning as an effective deformation mechanism which is attributed to the effect of the high stress levels on the partial dislocation separation. Deformation twinning gives rise to high stress levels during post-processing room temperature tension and compression experiments by providing additional barriers to dislocation motion and decreasing the mean free path of dislocations. The highest tensile flow stress observed in the sample processed at 700 oC following one pass route A was on the order of 1200 MPa which is very high for 316L stainless steel. The ultimate goal of this study is to produce stabilized end microstructures with improved mechanical properties and demonstrate the applicability of ECAE on difficult-to-work alloys.

NiTiHf alloys have attracted considerable attention as potential high temperature Shape Memory Alloy (SMA) but the instability in transformation temperatures and significant irrecoverable strain during thermal cycling under constant stress remains a major concern. The main reason for irrecoverable strain and change in transformation temperatures as a function of thermal cycling can be attributed to dislocation formation due to relatively large volume change during transformation from austenite to martensite. The formation of dislocations decreases the elastic stored energy, and during back transformation a reduced amount of strain is recovered. All these observations can be attributed to relatively soft lattice that cannot accommodate volume change by other means. We have used Equal Channel Angular Extrusion (ECAE), hot rolling and marforming to strengthen the 49.8Ni-42.2Ti-8Hf (in at. %) material and to introduce desired texture to overcome these problems in NiTiHf alloys. ECAE offers the advantage of preserving billet cross-section and the application of various routes, which give us the possibility to introduce various texture components and grain morphologies. ECAE was performed using a die of 90º tool angle and was performed at high temperatures from 500ºC up to 650ºC. All extrusions went well at these temperatures. Minor surface cracks were observed only in the material extruded at 500 °C, possibly due to the non-isothermal nature of the extrusion. It is believed that these surface cracks can be eliminated during isothermal extrusion at this temperature. This result of improved formability of NiTiHf alloy using ECAE is significant because an earlier review of the formability of NiTiHf using 50% rolling reduction concluded that the minimum temperature for rolling NiTi12%Hf alloy without cracks is 700°C. The strain level imposed during one 90° ECAE pass is equivalent to 69% rolling reduction. Subsequent to ECAE processing, a reduction in irrecoverable strain from 0.6% to 0.21% and an increase in transformation strain from 1.25% to 2.18% were observed at a load of 100 MPa as compared to the homogenized material. The present results show that the ECAE process permits the strengthening of the material by work hardening, grain size reduction, homogeneous distribution of fine precipitates, and the introduction of texture in the material. These four factors contribute in the increase of stability of the material. In this thesis I will be discussing the improvement of mechanical behavior and stability of the material achieved after various passes of ECAE.

Hexagonal closed packed (hcp) materials, in contrast to cubic materials, possess several processing challenges due to their anisotropic structural response, the wide variety of deformation textures they exhibit, and limited ductility at room temperature. The aim of this work is to investigate, both experimentally and theoretically, the effect os severe plastic deformation, ultrafine grain sizes, crystallographic textures and number of phases on the flow stress anisotropy and tension compression asymmetry, and the mechanisms responsible for these phenomena in two hcp materials: AZ31B Mg alloy consisting of one phase and Zn-8wt.% Al that has an hcp matrix with a secondary facecentered cubic (fcc) phase. Mg and its alloys have high specific strength that can potentially meet the high demand for light weight structural materials and low fuelconsumption in transportation. Zn-Al alloys, on the other hand, can be potential substitutes for several ferrous and non-ferrous materials because of their good mechanical and tribological properties. Both alloys have been successfully processed using equal channel angular extrusion (ECAE) following different processing routes in order to produce samples with a wide variety of microstructures and crystallographic textures for revealing the relationship between microstructural parameters, crystallographic texture and resulting flow stress anisotropy at room temperature. For AZ31B Mg alloy, the texture evolution during ECAE following conventional and hybrid ECAE routes was successfully predicted using visco-plastic self-consistent (VPSC) crystal plasticity model. The flow stress anisotropy and tension-compression (T/C) asymmetry of the as received and processed samples at room temperature were measured and predicted using the same VPSC model coupled with a dislocation-based hardening scheme. The governing mechanisms behind these phenomena are revealed as functions of grains size and crystallographic texture. It was found that the variation in flow stress anisotropy and T/C asymmetry among samples can be explained based on the texture that is generated after each processing path. Therefore, it is possible to control the flow anisotropy and T/C asymmetry in this alloy and similar Mg alloys by controlling the processing route and number of passes, and the selection of processing conditions can be optimized using VPSC simulations. In Zn-8wt.% Al alloy, the hard phase size, morphology, and distribution were found to control the anisotropy in the flow strength and elongation to failure of the ECAE processed samples.

TiNiPd high-temperature shape memory alloys (HTSMAs) have attracted considerable attention as potential solid-state actuators capable of operating at temperatures up to 500 °C, exhibiting excellent corrosion resistance, adequate ductility levels and significant strain recovery under both constrained and unconstrained thermomechanical conditions. During operation, these actuators may be subjected to multiple cycles and from an application point of view, the functional stability, i.e. conservation of original actuator dimensions and transformation temperatures during repeated employment, is of considerable importance. This study addresses the issue of functional stability in a model HTSMA, Ti50.5Ni24.5Pd25, for its use as a compact solid-state actuator. Since the primary reason for functional instability is the creation of lattice defects (dislocations, vacancies, etc.) during repeated transformation cycles, several methods were successfully undertaken to improve the functional stability through inhibiting the generation of these defects. Solid-solution strengthening through Sc microalloying and thermomechanical treatments via severe plastic deformation were the two approaches used to strengthen the HTSMA against defect generation. Thermal cycling the HTSMA under stress was the third method to voluntarily introduce defects into the microstructure such that further defect generation during application would be impeded. Overall, severe plastic deformation was found to be more efficient than other strengthening methods in improving the functional stability of TiNiPd HTSMA, yet it brought about disadvantages such as reduction in transformation strain and transformation temperatures. While functional instability is due to the creation of lattice defects, the generation of these defects is mainly controlled by the crystallographic incompatibility between martensitically transforming phases and the strength levels for plastic deformation. It was shown that TiNiPd HTSMAs, which exhibited martensitic transformation from a cubic (B2) to orthorhombic (B19) symmetry, illustrated better compatibility and thus better functional stability levels compared to TiNi SMAs, which had a B2 to monoclinic (B19’) transition. Although crystallographic incompatibility seems to be the governing factor for the functional stability of the TiNiPd HTSMA, the strength differential between the onset of plastic deformation and local constraint due to the martensitic transformation was also found to be an influential factor determining the overall stable behavior. Functional stability was also investigated for the two-way shape memory effect (TWSME) in TiNiPd HTSMAs. Better strength and compatibility levels compared to TiNi SMAs were also reflected in the TWSME characteristics in the form of enhanced stability under stress-free thermal cycling. The stability during constrained thermal cycling was not as good and TWSME degraded rapidly while doing work against an opposing stress. Nevertheless, work output levels were much higher as compared to those obtained from conventional TiNi and Cu-based SMAs.

In this work, ultrafine-grained (UFG) Al-5wt%Zn alloy was produced by equal channel angular extrusion (ECAE). The microstructure evolution during ECAE and the mechanical properties of the UFG Al-Zn alloy were investigated. In order to identify the effect of Zn in the Al-Zn alloy, pure aluminum (4N, 99.99%) was also studied for comparison. The grains of the Al-Zn alloy could be refined effectively by increasing the ECAE passes. However, as the ECAE passes increased, the microhardness increased initially but maintained constant after 4 ECAE passes. The dislocation density within grain interior was decreased gradually with increasing ECAE passes. After being processed to twelve ECAE passes, the UFG Al-Zn alloy exhibited 53.7% of the grain boundaries being high angle grain boundaries (HAGBs). The UFG Al-5wt%Zn alloy exhibits superior tensile strength and elongation as compared with pure aluminum fabricated by the same ECAE process. Experimental results indicated that adding Zn in aluminum alloy could provide solid-solution strengthening and considerable enhancement in tensile ductility which might be related to an improved post-uniform elongation (PUE). The strain rate sensitivity (SRS) of the UFG Al-Zn alloy also increased with increasing the ECAE passes, which might be related to the fine grain size and the contribution of grain boundary sliding. The activation volume of the UFG Al-Zn alloy was in the range of 32b3~76b3, and the pure aluminum was in the range of 57b3~122b3. Because of the small value of the activation volume, it is suggested that the controlling mechanism for dislocation glide in the UFG Al-Zn alloy might be related to the generation and absorption of dislocations in grain boundary, as well as the interaction between dislocations and solute Zn atoms in the grain boundary.

Severe plastic deformation methods are of great interest in industrial forming applications, as they give rise to significant refinement in microstructures and improvements in mechanical and physical properties. In the &ldquo / Equal Channel Angular Extrusion (ECAE)&rdquo / , which is the most common method for production of ultrafine grained bulk samples, very high plastic strains are introduced into the bulk material without any change in cross section. This study is composed of two main parts. Part I focuses on the plastic deformation behavior of Al alloys by modeling ECAE with Msc. Marc finite element software. A series of numerical experiments were carried out for the die angles of 90&deg / , 120&deg / , and 150&deg / , different friction conditions, and different round corners. Besides, the effects of strain hardening characteristics of the material, strain hardening coefficient (K) and exponent (n) of Hollomon&rsquo / s law, on corner gap formation and strain homogeneity in equal channel angular pressing process were investigated quantitatively. The results were compared and verified with those of the upper bound analysis. The numerical results showed that the process performance can be improved by modifying the die corner curvature accordingly, without running time consuming simulations. On the other hand, the aim of Part 3 is to investigate the texture evolution, mechanical response and the corresponding mechanisms, in terms of the flow stress anisotropy and tension-compression asymmetry in the ZK60 Mg alloy. The alloy was processed using ECAE, with different processing routes and temperatures, in order to produce samples with a wider variety of microstructures and crystallographic textures. Several mechanical tests and microstructure examinations were carried out / and the flow stress anisotropy and tension-compression asymmetry of the as-received and processed samples were measured. It was found that the initial texture has a strong effect on the resulting textures / and the textures, combined with the microstructure effect, define the mechanical properties of processed samples. Thus, the tension-compression asymmetry and the flow stress anisotropy variations in the processed samples are attributed to the generated textures and it is possible to control these properties by controlling the processing route and temperature.

Aufgrund ihrer herausragenden Eigenschaften haben ultrafeinkörnige Werkstoffe, die aus konventionellen normalkörnigen Halbzeugen über eine extrem große Kaltverformung hergestellt wurden, in den letzten zwei Jahrzehnten zunehmend an Bedeutung erlangt. In der vorliegenden Arbeit wird das Fließspannungsverhalten eines Reinaluminiumwerkstoffes (EN AW-1070 – Al99,7) und einer ausscheidungshärtbaren Aluminiumlegierung (EN AW-6060 – AlMgSi) mit Korngrößen von bis zu 660 nm und 310 nm in einem weiten Bereich von Dehnungen und Dehnraten analysiert und mit den zzt. existierenden Modellvorstellungen zu den mikrostrukturellen Abläufen in Verbindung gebracht. Um die Voraussetzung zur Herstellung von ultrafeinkörnigen Werkstoffen zu schaffen, wurden mehrere Werkzeugprototypen für die ECAP-Umformung im Labormaßstab entwickelt und erprobt. Die Untersuchungen zum Fließspannungsverhalten erfolgten anhand von Zug- und Druckversuchen über insgesamt sieben Dekaden der Dehnrate bis in den Bereich der hochdynamischen Belastung von 10^3 s^-1. Die Tests zeigen, dass das Fließspannungsverhalten ultrafeinkörniger Aluminiumwerkstoffe vollständig mithilfe der thermisch aktivierbaren Mechanismen erklärbar ist, wobei Ausscheidungen eine wichtige Rolle spielen. / Because of their exceptional properties ultrafine-grained materials, processed from conventional polycrystalline materials by severe plastic deformation, have gained increasing scientific and industrial interest during the last two decades. Based on the concept of work-hardening for f.c.c. metals the commercially pure aluminium AA1070 (Al99,7 – soft annealed) and the aluminium alloy AA6060 (AlMgSi – peak aged) were investigated. ECAP was used to introduce very high strains and an ultrafine-grained microstructure with grain sizes down to 660 nm and 310 nm. Subsequently compression and tensile tests were performed in a wide range of strain rates over seven decades up to the range of impact loading of 10^3 s^-1. The results indicate that strain path and the corresponding dislocation structure is important for the post-ECAP yielding and the following hardening response. Furthermore the precipitates of the AA6060 clearly constrain the interactions of dislocations in work-hardening stage III – causing lower strain rate sensitivity. If compared to the AA1070 they avoid hardening in stage V where an additional rate and temperature depending effect contributes – caused by the interaction of deformation induced vacancies and dislocations. The results indicate that the strain-hardening behavior can be described by thermal activated mechanisms.

Made available in DSpace on 2016-06-02T19:19:59Z (GMT). No. of bitstreams: 1 VEGA_Marcelo_2014.pdf: 9141409 bytes, checksum: fd60293925ed2e6a9d8df71ece7c06f5 (MD5) Previous issue date: 2014-08-18 / Financiadora de Estudos e Projetos / It is known that the formability of aluminum alloy AA1050 is not favored when sheets are produced by conventional rolling due to the appearance of intense cube texture {100} <100> after recrystallization heat treatment. The objective of this study was to investigate whether components of shear processes can improve this property. For this work two processes of plastic deformation introducing shear stresses were selected: Equal channel angular extrusion (ECAE) and asymmetric rolling; these processes were compared to conventional rolling. In conventional rolling deformation results mainly compressive stresses. In the ECAE process shear is induced in the intersection of two channels of the same geometry that intersect by an angle &#61542; In the asymmetric rolling the shear stress is basically increased due to the speed variation between the rolls. An AA1050 aluminum sheet produced by the twin roll casting process was used in this study. The deformations were performed basically in 4 paths: i) conventional rolling, 70% reduction, ii) ECAE 1-8 passes, iii) ECAE 1-4 passes followed by conventional rolling with reduction of 70% and iv) Asymetric Rolling with reductions 30-50%. The mechanical and microstructural characterization of the deformed state was performed and the formability after annealing heat treatment was studied. ECAE deformation reduced the grain size, which measured by EBSD and transmission electron microscopy yield 1 micrometer. The evolution of equivalent strain compared with the increase of the hardness indicated a grain size stabilization of the grain/cell after four ECAE extrusion passes. After 8 passes the fraction of high angle boundaries exceeded the low-angle boundaries, ie dynamic recrystallization occurred during deformation. The texture after one pass ECAE approached the ideal texture for a 120 ° ECAE die. For deformations with 4 - 8 ECAE passes, the texture evolved into scattering the orientations having the {111} plane parallel to the surface (&#61543; fiber), and into the formation of rotated cube {100} <110> and rotated Goss {110} <110> orientations. The conventional rolling after ECAE returned the orientations to typical rolling textures: brass, copper and Goss. Deformation by asymmetric rolling with a difference of tangential velocity of 1.2 imposed shear stress, but it was necessary to decrease the reduction rate from 10% to 5% per pass in order to appreciably modify the texture. Comparing the formability of the deformed material, it was observed that ECAE increased the penetration depth in the Erichsen test, while rolling decreased the Erichsen index. Asymmetric rolling reduced the intensity of texture and destroyed the symmetry of the crystallographic orientations. The asymmetric rolled sample presented better formability than the rolled samples. After annealing, the samples of conventional rolling, with or without ECAE pre - strain, showed typical textures of annealed laminated material with high cube texture type. The &#61543; fiber was not stable in the ECAE annealed samples. Although the overall texture intensity remained low, increasing ECAE deformation before heat treatment strengthened the Goss {110} <001> orientation. For the asymmetric rolling the fiber orientations <100>// ND was scattered and both rotated cube and cube orientations were present. The lowest index of planar anisotropy was obtained in the sample annealed after four ECAE passes, representing a lower tendency to fail, This sample also presented an index of penetration in Erichsen testing of the same order of conventionally rolled sheets. It has been shown that both ECA as the asymmetric rolling deformation can significantly modify the texture of deformation and annealing, and improve the characteristics of formability of aluminum alloy 1050. This processing step should be located at the end of mechanical forming process before final annealing. / Sabe-se que a estampabilidade em ligas de alumínio AA1050 não é favorecida quando as chapas são produzidas por laminação convencional devido ao surgimento de uma textura do tipo cubo {100}<100> de forte intensidade após tratamentos térmicos de recristalização. O objetivo do trabalho foi investigar se processos com componentes de cisalhamento podem melhorar esta propriedade. Para este trabalho foram selecionados dois processos de deformação plástica que introduzem tensões de cisalhamento: Extrusão em canal angular (ECA) e Laminação assimétrica (LA); esses processos foram comparados à laminação convencional. Na laminação convencional a deformação resulta principalmente de esforços de compressão. No processo ECA o cisalhamento é imposto na intersecção de dois canais de mesma geometria que se interceptam formado um ângulo &#61542;. Na laminação assimétrica o esforço de cisalhamento é introduzido devido à variação de velocidade entre os cilindros de laminação. Partiu-se de chapas de alumínio AA1050 produzidas pelo processo Caster. As deformações foram executadas basicamente em 4 esquemas: i) Laminação convencional com 70% de redução; ii) ECA rota A de 1 a 8 passes; iii) ECA rota A de 1 a 4 passes seguido por laminação convencional com redução de 70% e iv) LA com reduções variando de 30 a 50%. Foi realizada a caracterização mecânica e microestrutural do estado deformado e foi estudada a conformabilidade após tratamento térmico de recozimento. Na deformação por ECA foi observado a redução do tamanho de grão, que medido por EBSD e por microscopia eletrônica de transmissão foi de cerca de 1 &#956;m. A evolução da deformação equivalente comparada com o aumento da dureza indicou uma estabilização do tamanho de grão/célula a partir de 4 passes. Após 8 passes a fração de contornos de alto ângulo ultrapassou a de contornos de baixo ângulo, ou seja, ocorreu recristalização dinâmica durante a deformação. A textura após um passe de ECA se aproximou da textura ideal para matriz ECA de 120°. Mas para deformações com quatro e oito passes, a textura evoluiu para uma dispersão das orientações contendo os {111} paralelos à superfície da chapa (fibra &#61543;), o aparecimento de orientações do tipo cubo rodado (100)<011> e de Goss rodado {110} <110>. A laminação convencional após ECA provocou o retorno às orientações típicas de laminação: latão, cobre e Goss. A deformação por laminação assimétrica com uma diferença de velocidade tangencial de 1,2 impôs esforços de cisalhamento, porém foi necessário diminuir a redução por passes de 10% para 5% para que o cisalhamento adicional modificasse sensivelmente a textura. Comparando a estampabilidade dos materiais deformados, observou-se que a deformação ECA aumentou a profundidade da penetração no ensaio Erichsen, enquanto que a laminação diminuiu o índice Erichsen. A laminação assimétrica reduziu a intensidade de textura e destruiu a simetria das orientações cristalográficas. Esta amostra encruada apresentou estampabilidade superior à das amostras laminadas. Após o recozimento, as amostras de laminação convencional, com ou sem pré-deformação ECA apresentaram texturas típicas de material laminado recozido com alto índice de textura tipo cubo. Nas amostras ECA a fibra &#61543; não ficou estável e teve sua intensidade reduzida. Embora a intensidade de textura total tenha permanecido baixa, o aumento de deformação ECA antes do tratamento térmico reforçou a orientação Goss {110}<001>. Já a amostra de laminação assimétrica houve dispersão das orientações na fibra <100>//ND e tanto orientações cubo como cubo rodado estavam presentes. O menor índice de anisotropia planar foi obtido na amostra de 4 passes ECA recozida (representando uma menor tendência ao orelhamento) e um índice de penetração no ensaio Erichsen da mesma ordem de chapas laminadas convencionalmente. Demostrou-se que tanto a deformação ECA quanto a laminação assimétrica podem modificar significantemente a textura de deformação e de recozimento e melhorar as características de conformabilidade da liga de alumínio 1050. Esta etapa de processamento deve estar localizada no final do processo de conformação mecânica, antes do recozimento final.

Aufgrund ihrer herausragenden Eigenschaften haben ultrafeinkörnige Werkstoffe, die aus konventionellen normalkörnigen Halbzeugen über eine extrem große Kaltverformung hergestellt wurden, in den letzten zwei Jahrzehnten zunehmend an Bedeutung erlangt. In der vorliegenden Arbeit wird das Fließspannungsverhalten eines Reinaluminiumwerkstoffes (EN AW-1070 – Al99,7) und einer ausscheidungshärtbaren Aluminiumlegierung (EN AW-6060 – AlMgSi) mit Korngrößen von bis zu 660 nm und 310 nm in einem weiten Bereich von Dehnungen und Dehnraten analysiert und mit den zzt. existierenden Modellvorstellungen zu den mikrostrukturellen Abläufen in Verbindung gebracht. Um die Voraussetzung zur Herstellung von ultrafeinkörnigen Werkstoffen zu schaffen, wurden mehrere Werkzeugprototypen für die ECAP-Umformung im Labormaßstab entwickelt und erprobt. Die Untersuchungen zum Fließspannungsverhalten erfolgten anhand von Zug- und Druckversuchen über insgesamt sieben Dekaden der Dehnrate bis in den Bereich der hochdynamischen Belastung von 10^3 s^-1. Die Tests zeigen, dass das Fließspannungsverhalten ultrafeinkörniger Aluminiumwerkstoffe vollständig mithilfe der thermisch aktivierbaren Mechanismen erklärbar ist, wobei Ausscheidungen eine wichtige Rolle spielen. / Because of their exceptional properties ultrafine-grained materials, processed from conventional polycrystalline materials by severe plastic deformation, have gained increasing scientific and industrial interest during the last two decades. Based on the concept of work-hardening for f.c.c. metals the commercially pure aluminium AA1070 (Al99,7 – soft annealed) and the aluminium alloy AA6060 (AlMgSi – peak aged) were investigated. ECAP was used to introduce very high strains and an ultrafine-grained microstructure with grain sizes down to 660 nm and 310 nm. Subsequently compression and tensile tests were performed in a wide range of strain rates over seven decades up to the range of impact loading of 10^3 s^-1. The results indicate that strain path and the corresponding dislocation structure is important for the post-ECAP yielding and the following hardening response. Furthermore the precipitates of the AA6060 clearly constrain the interactions of dislocations in work-hardening stage III – causing lower strain rate sensitivity. If compared to the AA1070 they avoid hardening in stage V where an additional rate and temperature depending effect contributes – caused by the interaction of deformation induced vacancies and dislocations. The results indicate that the strain-hardening behavior can be described by thermal activated mechanisms.