Ultra-fine grained (UFG) materials have attracted considerable interest due to the possibility of achieving simultaneous increase in strength and ductility. Effective use of these materials in engineering applications requires investigating the processing-microstructure-property inter-relations leading to a comprehensive understanding of the material behavior. Research efforts on producing UFG hexagonal close packed (hcp) materials have been limited in spite of their envisaged utilization in various technologies. The present study explores multiple UFG hcp materials to identify the general trends in their deformation behaviors, microstructural features, crystallographic texture evolutions and mechanical responses under strain path changes. UFG hcp materials, including commercial purity Ti, Ti-6Al-4V alloy and high purity Zr, were fabricated using equal channel angular extrusion (ECAE) as a severe plastic deformation (SPD) technique following various processing schedules. Several characterization methods and a polycrystal plasticity model were utilized in synergy to impart the relationships between the UFG microstructure, the texture and the post-ECAE flow behavior. Pure UFG hcp materials exhibited enhanced strength properties, making them potential substitutes for coarse-grained high strength expensive alloys. Incorporation of post-ECAE thermo-mechanical treatments was effective in further improvement of the strength and ductility levels. Strong anisotropy of the post-ECAE flow response was evident in all the materials studied. The underlying mechanisms for anisotropy were identified as texture and processing-induced microstructure. Depending on the ECAE route, the applied strain level and the specific material, the relative importance of these two mechanisms on plastic flow anisotropy varied. A viscoplastic self-consistent approach is presented as a reliable model for predicting the texture evolutions and flow behaviors of UFG hcp materials in cases where texture governs the plastic anisotropy. Regardless of the material, the initial billet texture and the extrusion conditions, ECAE of all hcp materials revealed similar texture evolutions. Accurate texture and flow behavior predictions showed that basal slip is the responsible mechanism for such texture evolution in all hcp materials independent of their axial ratio. High strength of the UFG microstructure was presented as a triggering mechanism for the activation of unexpected deformation systems, such as high temperature deformation twinning in Ti-6Al-4V and room temperature basal slip in pure Zr.

This thesis describes the effect of dislocation slip on superplastic deformation of AZ31 magnesium alloy. Through two different routes of ECAE (equal channel angular extrusion), two types of specimens having the same grain size but different texture were obtained. One is favorable for basal slip and the other is not. Under the same condition of deformation, the strain rate sensitivity and contribution of grain boundary sliding to total elongation in these two different specimens are almost the same. As for elongation, not much difference was found. The present results demonstrate that the relationship between dislocation slip and grain boundary sliding in superplastic AZ31 magnesium alloy is non-obvious.

Ultrafine-grained(UFG) AZ31 Mg alloy was obtained by equal-channel angular extrusion(ECAE) and subsequent annealing at elevated temperatures. The basal texture component for ECAEed material is located on the Z plane of the ECAEed billets. Tensile tests were performed at temperatures between room temperature and 125¢J, and strain rates used ranging from 3*10-5 to 6*10-2 s-1. The experimental results showed that a high tensile yield stress of 394 MPa was obtained at room temperature under a strain rate of 3*10-3 s-1. Strengths of UFG AZ31 specimens were greatly improved due to grain refinement. It was found that strain rate sensitivity of UFG AZ31 alloy increased significantly from 0.024 to 0.321 with increasing temperature. The constant k of Hall-Petch equation, £m=£m0 +kd-1/2, decreased with increasing temperature, and decreasing strain rate. Negative k values were ontained at 75¢J and 100¢J under a strain rate 3*10-5 s-1. When compressed along X, Y and X45Z billet orientations, strain localization within shear bands was found in UFG AZ31 specimens. Shear bands are formed inclined near 45 to the compression axis. The smaller the grain size, the thinner the shear band. Different Hall-Petch constant k were found in specimens deformed along different orientations, which is caused by different deformation mechanisms. The formation of tension twins is the primary deformation mechanism for compressed X and Y samples, and basal slip is responsible for the deformation of X45Z sample. tension twins were found in 0.46 £gm grain size specimens.

Ultra-fine grained (UFG) materials have attracted considerable interest due to the possibility of achieving simultaneous increase in strength and ductility. Effective use of these materials in engineering applications requires investigating the processing-microstructure-property inter-relations leading to a comprehensive understanding of the material behavior. Research efforts on producing UFG hexagonal close packed (hcp) materials have been limited in spite of their envisaged utilization in various technologies. The present study explores multiple UFG hcp materials to identify the general trends in their deformation behaviors, microstructural features, crystallographic texture evolutions and mechanical responses under strain path changes. UFG hcp materials, including commercial purity Ti, Ti-6Al-4V alloy and high purity Zr, were fabricated using equal channel angular extrusion (ECAE) as a severe plastic deformation (SPD) technique following various processing schedules. Several characterization methods and a polycrystal plasticity model were utilized in synergy to impart the relationships between the UFG microstructure, the texture and the post-ECAE flow behavior. Pure UFG hcp materials exhibited enhanced strength properties, making them potential substitutes for coarse-grained high strength expensive alloys. Incorporation of post-ECAE thermo-mechanical treatments was effective in further improvement of the strength and ductility levels. Strong anisotropy of the post-ECAE flow response was evident in all the materials studied. The underlying mechanisms for anisotropy were identified as texture and processing-induced microstructure. Depending on the ECAE route, the applied strain level and the specific material, the relative importance of these two mechanisms on plastic flow anisotropy varied. A viscoplastic self-consistent approach is presented as a reliable model for predicting the texture evolutions and flow behaviors of UFG hcp materials in cases where texture governs the plastic anisotropy. Regardless of the material, the initial billet texture and the extrusion conditions, ECAE of all hcp materials revealed similar texture evolutions. Accurate texture and flow behavior predictions showed that basal slip is the responsible mechanism for such texture evolution in all hcp materials independent of their axial ratio. High strength of the UFG microstructure was presented as a triggering mechanism for the activation of unexpected deformation systems, such as high temperature deformation twinning in Ti-6Al-4V and room temperature basal slip in pure Zr.

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.

The primary objectives of this study were: (1) to verify the effectiveness of ECAE to induce equal amounts of strain and grain refinement in bars of different cross-sectional areas, (2) to determine the effectiveness of ECAE in breaking down the as-cast macrostructure in CDA 101 Cu and in producing a homogeneous material containing micron-scale grains upon recrystallization, and (3) to determine a thermomechanical processing (TMP) schedule (from the ones examined) that produces the best microstructure in terms of grain size and uniformity. The effects of extrus ion route, levels of strain and intermediate heat treatment were investigated. To achieve the first objective, bars having square cross-sections of three different sizes, 19 mm, 25 mm and 50 mm, were processed up to eight ECAE passes through routes A, B, C and E. To achieve the second and third objectives, bars were processed up to eight ECAE passes with and without intermediate heat treatments through routes Bc, C, E and F. ECAE processing was carried out in a 90o extrusion die with sliding walls at an extrusion speed of 2.5 mm/s. Recrystallization studies were carried out on the processed material to evaluate the recrystallization behavior and thermal stability of the material. The as-worked and recrystallized materials were characterized by Vickers microhardness, optical microscopy (OM) and transmission electron microscopy (TEM). Results indicate that similar hardness values, sub-grain morphology and recrystallized grain size are generated in the three bars having different cross-sectional sizes processed through ECAE. ECAE is shown to induce uniform strain in all three billet sizes. ECAE is therefore shown to be effective in scale-up to a size of at least 50 mm, with larger billets giving better load efficiency. Results from the later parts of this study indicate that eight extrusion passes via route Bc produces the best microstructure in terms of grain size and microstructural uniformity. The routes can be arranged in the sequence Bc> E, F> C for their ability to produce a uniform recrystallized microstructure with small average grain size. Macroscopic shear bands are sometimes generated during extrusion depending upon the initial grain morphology and texture of the material.

Bulk metallic glasses (BMGs) have displayed impressive mechanical properties, but the use and dimensions of material have been limited due to critical cooling rate requirements and low ductility. The application of severe plastic deformation by equal channel angular extrusion (ECAE) for consolidation of bulk amorphous metals (BAM) and amorphous metal matrix composites (AMMC) is investigated in this dissertation. The objectives of this research are a) to better understand processing parameters which promote bonding between particles and b) to determine by what mechanisms the plasticity is enhanced in bulk amorphous metal matrix composites consolidated by ECAE. To accomplish the objectives BAM and AMMCs were produced via ECAE consolidation of Vitreloy 106a (Zr58.5Nb2.8Cu15.6Ni12.8Al10.3-wt%), ARLloy #1 (Hf71.3Cu16.2Ni7.6Ti2.2Al2.6 -wt%), and both of these amorphous alloys blended with crystalline phases of W, Cu and Ni. Novel instrumented extrusions and a host of postprocessing material characterizations were used to evaluate processing conditions and material properties. The results show that ECAE consolidation at temperatures within the supercooled liquid region gives near fully dense (>99%) and well bonded millimeter scale BAM and AMMCs. The mechanical properties of the ECAE processed BMG are comparable to cast material: σf = 1640 MPa, εf = 2.3%, E = 80 GPa for consolidated Vitreloy 106a as compared to σf = 1800 MPa, εf = 2.5%, E = 85 GPa for cast Vitreloy 106, and σf = 1660 MPa, εf = 2.0%, E = 97 GPa for ARLloy #1 as compared to σf = 2150 MPa, εf < 2.5%, E = 102 GPa for Hf52Cu17.9Ni14.6Ti5Al10. The mechanical properties of AMMCs are substandard compared to those obtained from melt-infiltrated composites due to non-ideal particle bonding conditions such as surface oxides and crystalline phase morphology and chemistry. It is demonstrated that the addition of a dispersed crystalline phase to an amorphous matrix by ECAE powder consolidation increases the plasticity of the amorphous matrix by providing locations for generation and/or arrest of adiabatic shear bands. The ability of ECAE to consolidated BAM and AMMCs with improved plasticity opens the possibility of overcoming the size and plasticity limitations of the monolithic bulk metallic glasses.

Bulk nanocrystalline 304L and 316L austenitic stainless steels (SS) were produced by equal channel angular pressing(ECAP) at elevated temperature. The average grain size achieved in 316L and 304 L SS is ~ 100 nm, and grain refinement occurs more rapid in 316 L SS than that in 304L. Also the structures are shown to retain a predominant austenite phase. Hardness increases by a factor of about 2.5 in both steels due largely to grain refinement and an introduction of a high density of dislocations. Tensile strength of nanocrystalline steels exceeds 1 GPa with good ductility in both systems. Mechanical properties of ECAPed 316L are also shown to have less dependence on strain rate than ECAPed 304L. ECAPed steels were shown to exhibit thermal stability up to 600oC as indicated by retention of high hardness in annealed specimens. Furthermore, there is an increased tolerance to radiation-induced hardening in the nanocrystalline equiaxed materials subjected to 100 keV He ions at an average dose of 3-4 displacement-per-atom level at room temperature. The large volume fraction of high angle grain boundaries may be vital for enhanced radiation tolerance. These nanocrystalline SSs show promise for further research in radiation resistant structural materials for next-generation nuclear reactor systems.

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.

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.