Abstract Equal channel angular extrusion (ECAE) has been used to investigate the formation of submicron grain structures in copper deformed to ultra-high plastic strains by different die angles, deformation routes, and deformation temperatures. The result was characterized by the use of transmission election microscopy (TEM), and the evolution of the deformed Cu depended on several parameters such as die angle, deformation route, and deformation temperature. It has been demonstrated that the most effective method of forming high angle boundaries and recrystallized grains by severe plastic deformation is to rotate billets with a constant clockwise 90o between each pass (route BC) via a 90o die angle. Besides, the temperature effect on the microstructural evolution is studied. With increasing deformation temperature, the microstructure becomes more homogeneous because the climb and the cross-slip of dislocations are easier at higher temperatures, and the fraction of high angle boundaries, recrystallized grains and size of them are increased significantly with the deformation temperature. In addition, the thermomechanical process was also investigated in the present work. It is suggested that a uniform submicron grained structure could be obtained by increasing the deformation temperature and decreasing the intermediate annealing temperature to promote dynamic recovery and to inhibit discontinuous recrystallization.

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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 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.

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.

The deformation mechanism of an ultrafine grained (UFG) Al-Zn alloy has been studied. In this work, Al-15wt%Zn alloy was processed by equal channel angular extrusion (ECAE) route A at 100oC to achieve UFG structure. The deformation mechanism was studied by performing tensile test with various strain rates. Scanning electron microscopy and transmission electron microscopy were used to investigate the microstructure evolution in Al-15wt%Zn alloy with increasing ECAE passes. The observation indicated that the super saturated Al-Zn alloy would decompose and precipitate Zn particles during ECAE process. Increasing ECAE passes, the aluminum grain size was reduced, but the size of Zn particles was increased. However, the net effect of increasing ECAE passes is softening of this Al-Zn alloy. The tensile properties of the UFG Al-Zn alloy can be summarized as follows. (1)The UFG Al-Zn alloy possesses higher tensile strength and elongation as compared to commercial purity Al (AA1050). (2)The strain rate sensitivity of the UFG Al-Zn alloy increases significantly with increasing number of ECAE pass, which might be related to the refined aluminum grain size. After processed by 4-16 ECAE passes, the activation volume of the UFG Al-Zn alloy falls in the range of 25 b3~40 b3, which remains nearly constant value with increasing tensile strain. It is suggested that the controlling mechanism responsible for the tensile deformation of the UFG Al-Zn alloy might be related to a grain boundary mediated mechanism. (3)With increasing ECAE passes, the total tensile elongation of the UFG Al-Zn alloy increases but the uniform elongation show little change. This indicates that the increase in total elongation is mainly due to the contribution from an enhanced post-uniform elongation (PUE). It is suggested that the enhanced PUE might be related to the increase in strain rate sensitivity, which is resulted from the refinement of grain size. More detailed studies are needed to understand the deformation mechanism.

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.