Understanding the plastic deformation mechanisms in polycrystals is a long-standing fundamental problem and its improvement has significant potential impact on the increase in materials resistance to typical failure modes such as fatigue cracking and stress corrosion cracking and hence the increase in the materials strength. However many deformation models are yet to be validated as quantitative experimental results at mesoscale to correlate dislocations and microstructure features are limited. This thesis furthers the High Resolution EBSD (HR-EBSD) technique in Geometrically Necessary Dislocation (GND) density measurement from qualitative analysis with a typical map size of 100 μm x100 μm to quantitative analysis with a map of 500 μm x500 μm by determining the optimised scanning step size (0.5 μm) and detector binning level (4x4 binning). This allows a statistically large number of grains to be sampled. Combining with obtained crystallographical information from a conventional EBSD system, systematic studies on GNDs behaviours with respect to a range of microstructure features such as grain boundaries and triple junctions were conducted on monotonically deformed polycrystal copper samples under tension. Relatively high GND density points were found near triple junctions and some grain boundaries whereas the low GND density points tend to appear near the grains’ interiors. These tendencies are particularly profound in low and moderately deformed samples. Hence more detailed analyses were performed to investigate the relations of GND density and the properties of grain boundaries and triple junctions. These quantitative analyses were complemented with direct visual assessment. The visual inspection provides interesting findings such as the strong GND structure dependence on grain orientations and GND structure development through increasing deformation; grain-grain interaction influences on GND structure development and GND structures near triple junctions. These GND density studies provide experimental results to validate some of the existing plastic deformation models for instance Ashby’s model of hardening and Hall-Petch relation. However, some of the new observations on GND structures at mesoscale cannot be fully rationalised by existing proposed mechanisms. Hence new models have been proposed that these GND structures might be generated from the intersections of different slip systems which occurred in various parts of a grain, or by the dislocation piling-up at some microstructural features e.g. triple junctions and twin boundaries.

Further understanding of dislocation-GB interactions is critical to increasing the performance of polycrystalline metals. The research contained within this dissertation aims to further dislocation-GB interaction understanding through three research studies. First, the effect of noise in EBSPs on GND calculations was evaluated in order to improve dislocation characterization via HR-EBSD. Second, the evolution of GNDs and their effects on back stress was studied through experimental and computational methods applied to tantalum oligo specimens. Third, statistical analysis was used to evaluate grain parameters and current GB transmission parameters on their correlation with dislocation accumulation.

This thesis apply High Resolution Electron Back Scatter Diffraction (HR-EBSD) technique to a variety of microstructure features and their interactions in pure h.c.p polycrystals. By correlating high quality Kikuchi patterns with a reference pattern, the relative state and distribution of strain, stress, and geometrically necessary dislocation (GND) density can be obtained with high strain sensitivity (10^-4) and angular resolution (10<sup-4</sup> radian). This technique is companied by a further investigation of subsurface features using Differential Aperture X-ray Micro-diffraction (DAXM) technique. The two technique have shown excellent agreement in capturing the magnitude and distribution of stress and GND. Stress field and GND distribution induced by slip band and grain boundary interactions, including blocked slip band with no observable slip transfer in SEM and slip transfer, were characterised. It was found that some blocked slip bands lead to high and localised stress concentration in the neighbouring grain while others did not, and no stress concentration were correlated with transferred slip bands. These three categories of interactions were rationalised using a slip transfer criteria (called LRB criteria) by investigating the geometric alignments between the impinging slip system and all possible slip systems in the neighbouring grain. The level of stress concentration were quantified into a stress intensity factor K, following the Frank, Eshelby, and Nabarro (FEN) model. It was found that the level of stress intensity correlates well with the number of dislocations within the pile up plane. The slip band and grain boundary interaction case that led to the highest magnitude of stress intensity factor was further investigated using DAXM experiments. The 3D data set informed us additional information hidden below the sample surface. The distribution of stress concentration in 3D is a ribbon conforming to the line of intersection between slip plane and grain boundary. Stress intensity factor calculation along this ribbon have shown large variations which led to a concern that sometimes 2D results might not be conclusive. For example, if damage is observed in sample surface, there is a possibility that large populations of damage already exist below sample surface as a result of the stress fluctuations. The level of stress concentration and distribution measured by both HR-EBSD and DAXM agree with each other and 3D lattice rotation gradient used in DAXM GND calculation was found to affect the range of GND distribution and how fast it decays away from grain boundary. Twinning is a deformation mechanism in HCP metal that is equally important as dislocation slip. The stress concentrations associated with twin propagation, approaching grain boundary, and thickening were characterised using HR-EBSD, from which the calculated stress tensor were used to generate a local Schmid factor (LSF) map. It was found that during twin propagation, local positive shear provides a favourable LSF condition that promote twin tip extension while supress it from thicken. When twin tip is approaching the grain boundary, the positive shear stress field no longer favour twin propagation, a narrow positive LSF field still exist at the tip of twin, promoting it to grow thick. During propagation and thickening process, the LSF seem to only affect the tip of twins and therefore these processes are possibly tip controlled.

Electron backscatter diffraction is a method that is well described and commonly used for orientation image mapping, including grain size estimation. The use of this method for measuring elastic deformation and rotations caused by plastic deformations is not so well decribed. This diploma thesis first describes the typical EBSD system. The information regarding the standard coordinate systems, grain orientation notation and system calibration is then used to create an open-source software for mapping elastic deformations and rotations inside a single grain or a monocrystal. This software uses data acquired during standard EBSD mapping on a commercial system.