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Changes in stress applied to mantle rocks, such as those imposed by earthquakes, induce a period of evolution in viscosity and microstructure. This transient creep is often modelled based on stress transfer among slip systems due to grain interactions. However, recent experiments have demonstrated that the intragranular accumulation of stresses among dislocations is the dominant cause of strain hardening in olivine at low temperatures, raising the question of whether the same process contributes to transient creep at higher temperatures. Here, we demonstrate that olivine samples deformed at 25{\deg}C or 1150 to 1250{\deg}C both contain stress heterogeneities of ~1 GPa that are imparted by dislocations and have correlation lengths of ~1 micrometre. The similar stress distributions formed in both temperature regimes indicate that accumulation of stresses among dislocations also provides a contribution to transient creep at high temperatures. The results motivate a new generation of models that capture these intragranular processes and may refine predictions of evolving mantle viscosity over the earthquake cycle., Comment: 17 pages, 5 figures, 2 tables

A method is presented for the registration and correlation of intrinsic property maps of materials, including data from nanoindentation hardness, Electron Back-Scattered Diffraction (EBSD), Electron Micro-Probe Analysis (EPMA). This highly spatially resolved method allows for the study of micron-scale microstructural features, and has the capability to rapidly extract correlations between multiple features of interest from datasets containing thousands of datapoints. Two case studies are presented in commercially pure (CP) titanium: in the first instance, the effect of crystal anisotropy on measured hardness and, in the second instance, the effect of an oxygen diffusion layer on hardness. The independently collected property maps are registered us-ing affine geometric transformations and are interpolated to allow for direct correlation. The results show strong agreement with trends observed in the literature, as well as providing a large dataset to facilitate future statistical analysis of microstructure-dependent mechanisms., 33 pages, 15 figures (9 main body) + graphical abstract, code on Github @XPCorrelate

Measurements of the local tetragonality in Fe-C martensite at microstructural length-scale through pattern matching of electron backscatter diffraction patterns (EBSPs) and careful calibration of detector geometry are presented. It is found that the local tetragonality varies within the complex microstructure by several per cent at largest and that the scatter in the axial ratio is increased at higher nominal carbon content. At some analysis points the local crystal structure can be regarded as lower symmetry than simple body centred tetragonal. A linear relation between the nominal carbon content and averaged local tetragonality measured by EBSD is also obtained, although the averaged axial ratio is slightly below that obtained from more classical X-ray diffraction measurements., 33 pages, 12 figures, 2 Tables

It is well-known that steels always oxidize faster in the environments containing water vapour than in dry oxygen. Due to the difficulties in obtaining necessary experimental scale of observations, the mechanisms responsible for the steam-accelerated oxidation are still unclear. Through a combination of multiscale characterization techniques, the surface oxide film formed on an Fe-17Cr-9Ni stainless steel after exposure to high-temperature steam has been studied in detail. The characterization results obtained in this study reveal that the inner oxide layer actually consists of two phases Fe-Ni austenite and FeCr2O4 oxide, which formed due to internal oxidation. The classic internal oxidation model underestimates the thickness of the inner oxide layer by one order of magnitude. This difference can be explained by the existence of fast diffusion channels in the inner oxide layer. This study provides direct evidence of a high density of nanopores in the oxide phase of the internal oxide layer, which can act as fast-diffusion channels if interconnected, and proposes their mechanisms of formation, a consequence of water dissociation-induced protons promoting the formation, migration, and clustering of both cation and anion vacancies.

Microcantilevers with triangular cross-sections were machined using a focused ion beam from an α Ti–6Al alloy. Plasticity was predominantly in the lower part of the cantilever, allowing tension–compression asymmetry to be investigated by bending the cantilever up or down. Both ⟨a⟩ prismatic slip and 〈 c + a 〉 pyramidal slip were investigated. The critical resolved shear stress was determined by calibrating a crystal plasticity model and found to be 329 MPa for ⟨a⟩ prismatic slip in both tension and compression. However significant tension–compression asymmetry was observed for 〈 c + a 〉 pyramidal slip; increasing to 820 MPa under compression and decreasing to 558 MPa in tension.

The evolution of dislocation density with creep strain in single-crystal superalloys is studied quantitatively using high-resolution electron backscatter diffraction (HR-EBSD) and electron channelling contrast imaging under controlled diffraction conditions (cECCI). Data regarding dislocation density/structure is measured for deformation at 900 °C and 450 MPa up to ≈ 1% plastic strain. Effects of chemical composition are elucidated via three purpose-designed superalloys of differing rhenium and ruthenium contents. The evidence indicates that dislocation avalanching is already prevalent at plastic strains of ≈ 0.1%; thereafter, an exponential decay in the dislocation multiplication rate is indicative of self-hardening due to dislocation constriction within the matrix channels, as confirmed by the imaging. The results are rationalised using discrete dislocation dynamics modelling: a universal dislocation evolution law emerges, which will be useful for alloy design efforts.

Resonance assignment and structural studies of larger proteins by nuclear magnetic resonance (NMR) can be challenging when exchange broadening, multiple stable conformations, and 1H back-exchange of the fully deuterated chain pose problems. These difficulties arise for the SARS-CoV-2 Main Protease, a homodimer of 2 × 306 residues. We demonstrate that the combination of four-dimensional (4D) TROSY-NOESY-TROSY spectroscopy and 4D NOESY-NOESY-TROSY spectroscopy provides an effective tool for delineating the 1H–1H dipolar relaxation network. In combination with detailed structural information obtained from prior X-ray crystallography work, such data are particularly useful for extending and validating resonance assignments as well as for probing structural features.

Cross correlation based high angular resolution EBSD (or HR-EBSD) has been developed for measurement of elastic strains, lattice rotations (and estimating GND density). Recent advances in Transmission Kikuchi diffraction (TKD), especially the on-axis geometry allows the possibility of acquiring patterns at higher spatial resolution. However, some controversy remains as to whether stresses/strains measured after the sample thinning process are still representative of the bulk sample. In this paper, we explore a way of applying the HR-EBSD method to study strains and lattice rotations in an initially bulk sample, that is then progressively thinned down until a similar analysis can be performed on thin (and electron transparent) samples. Thus, HR-TKD will be compared as a possible alternative to HR-EBSD, in scenarios when it is not always possible to perform EBSD on the surface of the sample. An estimate of strain relaxation in the sample as a result of sample thinning is presented.

The mechanics of olivine deformation play a key role in large-scale, long-term planetary processes, such as the response of the lithosphere to tectonic loading or the response of the solid Earth to tidal forces, and in short-term processes, such as the evolution of roughness on oceanic fault surfaces or postseismic creep within the upper mantle. Many previous studies have emphasized the importance of grain-size effects in the deformation of olivine. However, most of our understanding of the role of grain boundaries in deformation of olivine is inferred from comparison of experiments on single crystals to experiments on polycrystalline samples.To directly observe and quantify the mechanical properties of olivine grain boundaries, we use high-precision mechanical testing of synthetic forsterite bicrystals with well characterised interfaces. We conduct nanoindentation tests at room temperature on low-angle (13o tilt about [100] on (015)) and high-angle (60o tilt about [100] on (011)) grain boundaries. We observe that plasticity is easier to initiate if the grain boundary is within the volume tested. This observation agrees with the interpretation that certain grain-boundary configurations can act as sites for initiating microplasticity.As part of continuing efforts, we are also conducting in-situ micropillar compression tests at high-temperature (above 600o C) within similar bicrystals. In these experiments, the boundary is contained within the micropillar and oriented at 45o to the loading direction to promote shear along the boundary. In these in-situ tests, our hypothesis is that the low-angle grain boundary displays a higher viscosity relative to the high-angle interface. Key advantages of performing in-situ experiments are the direct observation of grain-boundary migration or sliding, simplified kinematics of a single boundary segment, and potentially changes in style of deformation with different grain-boundary character.These small deformation volume experiments allow us to qualitatively explore the differences between the crystal interior and regions containing grain boundaries. Overall, the variation in strain and temperature in our small scale experiments allows the fundamental investigation of the response of well characterised forsterite grain boundaries to deformation.

Digital image correlation (DIC) and crystal plasticity simulation were utilised to study cold dwell behaviour in a coarse grain Ti-6Al alloy at 3 different temperatures up to 230 °C. Strains extracted from large volume grains were measured during creep by DIC and were used to calibrate the crystal plasticity model. The values of critical resolved shear stresses (CRSS) of the two main slip systems (basal and prismatic) were determined as a function of temperature. Stress along paths across the boundaries of two grain pairs, (1) a `rogue' grain pair and (2) a `non-rogue' grain pair, were determined at different temperatures. Load shedding was observed in the `rogue' grain pair, where a stress increment during the creep period was found in the `hard' grain. At elevated temperatures, 120 °C was found to be the worst case scenario as the stress difference at the grain boundaries of these two grain pairs were found to be the largest among the three temperatures. This can be attributed to the fact that the strain rate sensitivity of both prismatic and basal slip systems is at its greatest in this worst case scenario temperature.

In this paper, we investigate the residual deformation field in the vicinity of nanoscratch tests using two orientations of a Berkovich tip on an (001) Cu single crystal. We compare the deformation with that from indentation, in an attempt to understand the mechanisms of deformation in tangential sliding. The lattice rotation fields are mapped experimentally using high-resolution electron backscatter diffraction (HR-EBSD) on cross-sections prepared using focused ion beam (FIB). A physically-based crystal plasticity finite element model (CPFEM) is used to simulate the lattice rotation fields, and provide insight into the 3D rotation field surrounding a nano-scratch experiment, as it transitions from an initial static indentation to a steady-state scratch. The CPFEM simulations capture the experimental rotation fields with good fidelity, and show how the rotations about the scratch direction are reversed as the indenter moves away from the initial indentation.

The serration of grain boundaries in Inconel 600 caused by heat treatment is studied systematically. A new method based on Fourier transforms is used to analyse the multiple wave-like character of the serrated grain boundaries. A new metric – the serration index – is devised and utilised to quantify the degree of serration and more generally to distinguish objectively between serrated and non-serrated boundaries. By considering the variation of the serration index with processing parameters, a causal relationship between degree of serration and solution treatment/cooling rate is elucidated. Processing maps for the degree of serration are presented. Two distinct formation mechanisms arise which rely upon grain boundary interaction with carbides: (i) Zener-type dragging which hinders grain boundary migration and (ii) a faceted carbide growth-induced serration.

Displacive transformations have been widely reported in metals, alloys and ceramics, but rarely reported to be important in the aqueous corrosion of alloys. We report here our analysis of the formation of the hexagonal-ZrO suboxide during the aqueous corrosion of α-Zr alloys and propose this to be a paraequilibrium displacive transformation with the rate controlled by oxygen diffusion. Two orientation relationships were identified between α-Zr and hexagonal-ZrO, ( 0002 ) α − Z r ∥ ( 1 ¯ 011 ) h − Z r O and [ 2 ¯ 110 ] α − Z r ∥ [ 10 1 ¯ 2 ] h − Z r O or ( 0002 ) α − Z r ∥ ( 22 4 ¯ 1 ¯ ) h − Z r O and [ 2 ¯ 110 ] α − Z r ∥ [ 1 1 ¯ 01 ] h − Z r O , with the first one more commonly observed. No specific orientation relationships between either hexagonal-ZrO and monoclinic-ZrO2 or α-Zr and monoclinic-ZrO2 were identified, which suggests that the formation of often-reported bulk oxide texture during aqueous corrosion is not related directly to the texture of the metallic substrate. These results provide a guideline for understanding the mechanisms of crystallographic evolution during oxide growth on commercial zirconium alloys, and also demonstrate the capability of transmission Kikuchi diffraction to investigate orientation relationships in nano-scale materials.

It is well known that titanium and some titanium alloys creep at ambient temperature, resulting in a significant fatigue life reduction when a stress dwell is included in the fatigue cycle. It is thought that localised time dependent plasticity in 'soft' grains oriented for easy plastic slip leads to load shedding and an increase in stress within a neighbouring 'hard' grain poorly oriented for easy slip. Quantifying this time dependent plasticity process is key to successfully predicting the complex cold dwell fatigue problem. In this work, synchrotron X-ray diffraction during stress relaxation experiments was used to characterise the time dependent plastic behaviour of commercially pure titanium (grade 4). Lattice strains were measured by tracking the diffraction peak shift from multiple plane families (21 diffraction rings) as a function of their orientation with respect to the loading direction. Critical resolved shear stress, activation energy and activation volume were established for both prismatic and basal slips modes by fitting a crystal plasticity finite element model to the lattice strain relaxation responses measured along the loading axis for three strong reflections. Prismatic slip was the easier mode having both a lower critical resolved shear stress (τc basal=252MPa and τcprism=154MPa) and activation energy (∆F basal=10.5×1020 J=0.65eV and ∆F prism=9.0×1020 J=0.56eV). The prism slip parameters correspond to stronger strain rate sensitivity compared to basal slip. This slip system dependence on strain rate will have a significant effect on stress redistribution to hard grain orientations during cold dwell fatigue.

The fracture properties of as-cast TiVNbTa, a refractory high-entropy alloy (RHEA), were investigated using four-point bending tests from −139 °C to 20 °C under a strain-rate of 10−3 s−1. From those tests and fractography, the conditional fracture toughness values and the brittle-to-ductile transition temperature were obtained. The brittle-to-ductile transition temperature was between −47 °C to −27 °C, which gives an estimated activation energy value of 0.52±0.09 eV for the alloy. This study provides a preliminary understanding of the nature of dislocation motion in a relatively ductile RHEA.

In this work, we report the feasibility of the silver nanowire (AgNW) foils as highly-sensitive, reproducible and facile detection tools for surface-enhanced Raman spectroscopy (SERS) applications. These flexible and free-standing AgNW foils, fabricated by vacuum filtration method following a modified polyol synthesis of AgNWs, are adequately structured for both biological specimen filtering and trace amount of molecule detection simultaneously. The compatibility of AgNW foil in SERS is investigated by using a Raman active molecule of different steric volumes across the filter cross-section. We have shown that AgNW foils exhibit extremely strong SERS activity with detection limit up to 10-9 M of crystal violet (CV) molecule with 20% variation over ∼cm2 , revealing reliable homogeneity of the acquired signal. While naturally occurring polyvinylpyrrolidone (PVP) layer during polyol synthesis contribute to controlled aggregation, oxidation prevention, and size - shape control purposes, it also creates a major challenge for obtaining enormous enhancement factors. However, controlled thickness of aluminum oxide (Al2O3) coating on PVP@AgNW foils affords to achieve higher enhancement factors than the uncoated ones. What is interesting is that the maximum intensity is achieved from two cycles of Al2O3 deposited on AgNW foils. This is attributed to the two different origins: first, a higher adsorption affinity of CV molecules to Al2O3 layer than PVP layer; second, tunneling barrier formation against quantum tunneling effects.

It is well known that titanium and some titanium alloys creep at ambient temperature, resulting in a significant fatigue life reduction when a stress dwell is included in the fatigue cycle. It is thought that localised time dependent plasticity in ‘soft’ grains oriented for easy plastic slip leads to load shedding and an increase in stress within a neighbouring ‘hard’ grain that is poorly oriented for easy slip. Quantifying this time dependent plasticity process is key to successfully predicting the complex cold dwell fatigue problem. In this work, synchrotron X-ray diffraction during stress relaxation experiments was performed to characterise the time dependent plastic behaviour of commercially pure titanium (grade 4). Lattice strains were measured by tracking the diffraction peak shifts from multiple plane families (21 diffraction rings) as a function of their orientation with respect to the loading direction. The critical resolved shear stress, activation energy and activation volume were established for both prismatic and basal slip modes by fitting a crystal plasticity finite element model to the lattice strain relaxation responses measured along the loading axis for three strong reflections. Prismatic slip was the easier mode having both a lower critical resolved shear stress ( τ c basal = 252 MPa and τ c prism = 154 MPa) and activation energy (ΔFbasal= 10.5×10−20J = 0.65 eV andΔFprism = 9.0×10−20J = 0.56 eV). The prism slip parameters correspond to a stronger strain rate sensitivity compared to basal slip. This slip system dependence on strain rate has a significant effect on stress redistribution to ‘hard’ grain orientations during cold dwell fatigue.

The strain fields of deformation twins in the ferrite matrix of an age-hardened duplex stainless-steel (Zeron 100: 25%Cr, 7%Ni) have been studied in situ under load, and ex situ (unloaded), using high-resolution electron backscatter diffraction (HR-EBSD). The local two-dimensional (2D) elastic strain field acting on the twin tip was parameterised for the first time using the strain energy release rate (J-integral) and then decomposed into the mode I and mode II stress intensity factors (KI and KII). An improved method to select the strain reference was used, based on the relationship between the HR-EBSD cross-correlation peak height and mean angular error. The elastic field described by KI increased with twin thickness. The in-plane shear field, described by KII, relaxed when the load was removed. Some current limitations of the 2D analysis are discussed, which aims to provide an experimental methodology to quantify the fields that describe the local boundary conditions for twin thickening and propagation.

There is a long-standing technological problem in which a stress dwell during cyclic loading at room temperature in Ti causes a drastic fatigue life reduction. To better understand the material characteristics that control or exacerbate this behaviour, evaluation of the time dependent plasticity of the main prismatic and basal slip systems is critical. Incorporating the influence of operating temperatures and common alloying elements on cold dwell fatigue will be beneficial for future alloy design to address this problem. In this work, characterisation of the time dependent plastic behaviour of two commercially pure titanium samples (grade 1 and grade 4) with different oxygen content at 4 different temperatures (room temperature, 75 ° C , 145 ° C and 250 ° C ) was performed during stress relaxation using synchrotron X-ray diffraction. Key parameters that govern the dislocation motion were determined for the major prismatic and basal slip systems as a function of temperature and oxygen content by calibrating a crystal plasticity finite element model with the measured lattice strain relaxation responses. From the temperatures assessed, 75 ° C was found to be the worst-case scenario, where the macroscopic plastic strain accumulation was significant during a relaxation cycle due to the greatest activity of both prism and basal slip systems. As the temperature increases, the contribution of thermal energy becomes greater than mechanical energy for dislocation glide. Oxygen was found to have a stronger strengthening effect on prism slip over basal slip, through a significant change in their respective critical resolved shear stresses. This effect becomes more significant in high oxygen content commercially pure Ti.

Interactions between dislocations potentially provide a control on strain rates produced by dislocation motion during creep of rocks at high temperatures. However, it has been difficult to establish the dominant types of interactions and their influence on the rheological properties of creeping rocks due to a lack of suitable observational techniques. We apply high-angular resolution electron backscatter diffraction (HR-EBSD) to map geometrically necessary dislocation (GND) density, elastic strain, and residual stress in experimentally deformed single crystals of olivine. Short-range interactions are revealed by cross-correlation of GND density maps. Spatial correlations between dislocation types indicate that non-collinear interactions may impede motion of proximal dislocations at temperatures of 1000°C and 1200°C. Long-range interactions are revealed by autocorrelation of GND density maps. These analyses reveal periodic variations in GND density and sign, with characteristic length-scales on the order of 1–10 μm. These structures are spatially associated with variations in elastic strain and residual stress on the order of 10-3 and 100 MPa, respectively. Therefore, short-range interactions generate local accumulations of dislocations, leading to heterogeneous internal stress fields that influence dislocation motion over longer length-scales. The impacts of these short- and/or long-range interactions on dislocation velocities may therefore influence the strain rate of the bulk material, and are an important consideration for future models of dislocation-mediated deformation mechanisms in olivine. Establishing the types and impacts of dislocation interactions that occur across a range of laboratory and natural deformation conditions will help to establish the reliability of extrapolating laboratory-derived flow laws to real Earth conditions.

In this work we combine experiments and simulations to study the residual deformation state near twins in titanium at different stages of the complete twin growth process, including the twin tip: (i) far from a grain boundary, (ii) approaching a grain boundary, and (iii) intersecting with a grain boundary. High resolution electron backscatter diffraction (HR-EBSD) was used to characterise the local residual stress state and dislocation density distributions. Schmid factors were calculated from both the global deformation state (i.e. remote loading) and local deformation state (i.e. from high angular resolution EBSD). Crystal plasticity finite element modelling was used to simulate the stress field close to twins during loading and unloading. These simulations indicate that while the magnitudes of the localized stress fields close to twin boundaries are reduced upon removing the far field load, the major features of the stress fields in these regions are dominated by accommodation of the twin and thus persist from the peak load state to the unloaded state. We find a good correlation between the active twin variant and the maximum local Schmid factor, while the external loading (i.e. global Schmid factor) plays a less important role. These findings are useful in determining which twins will grow when a sample is deformed, and this has important implications for in service performance as well as texture evolution during mechanical processing.

The angular resolution of electron backscatter diffraction (EBSD) measurements can be significantly improved using an analysis based on determination of small shifts in features from one pattern to the next using cross-correlation functions. Using pattern shift measurements at many regions of the pattern, errors in the best fit strain and rotation tensors can be reduced. The authors show that elements of the strain tensor and small misorientations can be measured to ±10 -4 and ±0.006° for rotations. We apply the technique to two quite different materials systems. First, we determine the elastic strain distribution near the interface in a cross-sectioned SiGe epilayer, Si substrate semiconductor heterostructure. The plane stress boundary conditions at the sample surface are used to separate every term in the strain tensor. Second, the applicability to structural materials is illustrated by determining the lattice curvature caused by dislocations within the plastic zone associated with the wake and tip of a fatigue crack in a Ni based superalloy. The lattice curvatures are used to calculate the geometrically necessary dislocation content in the plastic zone. © 2006 Institute of Materials, Minerals and Mining.

We study the mechanisms of slip transfer at a grain boundary, in titanium, using Differential Aperture X-ray Laue Micro-diffraction (DAXM). This 3D characterization tool enables measurement of the full (9-component) Nye lattice curvature tensor and calculation of the density of geometrically necessary dislocations (GNDs). We observe dislocation pile-ups at a grain boundary, as the neighbor grain prohibits easy passage for dislocation transmission. This incompatibility results in local micro-plasticity within the slipping grain, near to where the slip planes intersect the grain boundary, and we observe bands of GNDs lying near the grain boundary. We observe that the distribution of GNDs can be significantly influenced by the formation of grain boundary ledges that serve as secondary dislocation sources. This observation highlights the non-continuum nature of polycrystal deformation and helps us understand the higher order complexity of grain boundary characteristics., 30 pages, 9 figures, 2 tables

Two new, low activation high entropy alloys (HEAs) TiVZrTa and TiVCrTa are studied for use as in-core, structural nuclear materials for in-core nuclear applications. Low-activation is a desirable property for nuclear reactors, in an attempt to reduce the amount of high level radioactive waste upon decommissioning, and for consideration in fusion applications. The alloy TiVNbTa is used as a starting composition to develop two new HEAs; TiVZrTa and TiVCrTa. The new alloys exhibit comparable indentation hardness and modulus, to the TiVNbTa alloy in the as-cast state. After heavy ion implantation the new alloys show an increased irradiation resistance.

Analysis of distortions of the crystal lattice within individual mineral grains is central to the investigation of microscale processes that control and record tectonic events. These distortions are generally combinations of lattice rotations and elastic strains, but a lack of suitable observational techniques has prevented these components being mapped simultaneously and routinely in earth science laboratories. However, the technique of high-angular resolution electron backscatter diffraction (HR-EBSD) provides the opportunity to simultaneously map lattice rotations and elastic strains with exceptional precision, on the order of 0.01 degree for rotations and 10-4 in strain, using a scanning electron microscope. Importantly, these rotations and lattice strains relate to densities of geometrically necessary dislocations and residual stresses. Recent works have begun to apply and adapt HR-EBSD to geological minerals, highlighting the potential of the technique to provide new insights into the microphysics of rock deformation. Therefore, the purpose of this overview is to provide a summary of the technique, to identify caveats and targets for further development, and to suggest areas where it offers potential for major advances. In particular, HREBSD is well suited to characterising the roles of different dislocation types during crystal plastic deformation and to mapping heterogeneous internal stress fields associated with specific deformation mechanisms/microstructures or changes in temperature, confining pressure, or applied deviatoric stress. These capabilities make HR-EBSD a particularly powerful new technique for analysing the microstructures of deformed geological materials., resubmitted article

Silicon wafers for photovoltaics could be produced without kerf loss by rolling, provided sufficient control of defects such as dislocations can be achieved. Here we report a study using mainly high resolution electron backscatter diffraction (HR-EBSD) of the microstructural evolution of Siemens polycrystalline silicon feedstock during a series of processes designed to mimic high temperature rolling. The starting material is heavily textured and annealing at 1400 ˚C results in 90% recrystallization and a reduction in average geometrically necessary dislocation (GND) density from >1014 m-2 to 1013 m-2. Subsequent compression at 1150 ˚C – analogous to rolling – produces subgrain boundaries seen as continuous curved high GND content linear features spanning grain interiors. Post-deformation annealing at 1400 ˚C facilitates a secondary recrystallization process, resulting in large grains typically of 100 µm diameter. HR-EBSD gives the final average GND density in as 3.2  1012 m-2 . This value is considerably higher than the dislocation density of 5  1010 m-2 from etch pit counting, so the discrepancy was investigated by direct comparison of GND maps and etch pit patterns. The GND map from HR-EBSD gives erroneously high values at the method’s noise floor (~1012 m-2) in regions with low dislocation densities.

Pattern matching between target electron backscatter patterns (EBSPs) and dynamically simulated EBSPs was used to determine the pattern centre (PC) and crystal orientation, using a global optimisation algorithm. Systematic analysis of error and precision with this approach was carried out using dynamically simulated target EBSPs with known PC positions and orientations. Results showed that the error in determining the PC and orientation was < 10$^{-5}$ of pattern width and < 0.01�� respectively for the undistorted full resolution images (956x956 pixels). The introduction of noise, optical distortion and image binning was shown to have some influence on the error although better angular resolution was achieved with the pattern matching than using conventional Hough transform-based analysis. The accuracy of PC determination for the experimental case was explored using the High Resolution (HR-) EBSD method but using dynamically simulated EBSP as the reference pattern. This was demonstrated through a sample rotation experiment and strain analysis around an indent in interstitial free steel.

In this paper, we have analysed the depth resolution that can be achieved by on-axis transmission Kikuchi diffraction (TKD) using a Zr-Nb alloy. The results indicate that the signals contributing to detectable Kikuchi bands originate from a depth of approximately the mean free path of thermal diffuse scattering (lambdaTDS) from the bottom surface of a thin foil sample. This existing surface sensitivity can thus lead to the observation of different grain structures when opposite sides of a nano-crystalline foil are facing the incident electron beam. These results also provide a guideline for the ideal sample thickness for TKD analysis of 6lambdaTDS, or 21 times the elastic scattering mean free path (lambdaMFP) for samples of high crystal symmetry. For samples of lower symmetry, a smaller thickness 3lambdaTDS, or 10lambdaMFP is suggested.

© 2016 The Authors. Published by Elsevier Inc. Electron backscatter diffraction (EBSD) is an automated technique that can measure the orientation of crystals in a sample very rapidly. There are many sophisticated software packages that present measured data. Unfortunately, due to crystal symmetry and differences in the set-up of microscope and EBSD software, there may be accuracy issues when linking the crystal orientation to a particular microstructural feature. In this paper we outline a series of conventions used to describe crystal orientations and coordinate systems. These conventions have been used to successfully demonstrate that a consistent frame of reference is used in the sample, unit cell, pole figure and diffraction pattern frames of reference. We establish a coordinate system rooted in measurement of the diffraction pattern and subsequently link this to all other coordinate systems. A fundamental outcome of this analysis is to note that the beamshift coordinate system needs to be precisely defined for consistent 3D microstructure analysis. This is supported through a series of case studies examining particular features of the microscope settings and/or unambiguous crystallographic features. These case studies can be generated easily in most laboratories and represent an opportunity to demonstrate confidence in use of recorded orientation data. Finally, we include a simple software tool, written in both MATLAB® and Python, which the reader can use to compare consistency with their own microscope set-up and which may act as a springboard for further offline analysis.

The performance of dynamic seals and hence the overall efficiency of the gas turbine is strongly dependent on the wear of individual seal elements and their ability to provide continuous sealing. Dynamic seals such as brush seals contact the rotating ‘rotor’ during operation, either transiently or continuously depending on factors such as thermal expansions, axial/radial displacements and eccentricities of the rotating components. This intermittent or continuous contact results in sliding wear of the seal tips and dictates the seal degradation and hence its efficiency. The present work examines the effect of sliding speeds between 6 m s −1 and 150 m s -1 on the wear-oxidation of Haynes 25 brush seal ‘tufts’ sliding against nitrided steel and thermal sprayed chrome oxide coating.

Among the electrodes for Li‐ion batteries, Li4Ti5O12 (LTO) stands out as anode owing to its stability and safety, in part ascribed to its low surface reactivity. However, the overlayer formation on the LTO surface upon electrochemical cycling is reported in recent years; a rough surface layer of electrochemically inactive α‐Li2TiO3 on top of the LTO (111) surface is suggested on the grounds of scanning probe techniques and theoretical ab initio calculations which would negatively strike on the battery performance. Hence the investigation of the LTO surface evolution is key to achieve more stable and safer Li‐ion batteries. LTO (111) thin film electrodes are used as model system where a variety of surface specific characterization techniques are applied to unveil the surface behavior of LTO in Li‐ion batteries. In contrast with previous studies, with the help of high‐resolution transmission electron microscopy and synchrotron‐based surface X‐ray diffraction, α‐Li2TiO3 is found to be a surface preparation product. Of special importance is the use of high‐resolution electron backscatter diffraction to report an increase on the LTO surface strain upon electrochemical cycling which can have a critical effect in long cycling performance of LTO that is always considered a zero‐strain material.

Electron backscatter diffraction (EBSD) is a well-established method of characterisation for crystalline materials. This technique can rapidly acquire and index diffraction patterns to provide phase and orientation information about the crystals on the material surface. The conventional analysis method uses signal processing based on a Hough/Radon transform to index each diffraction pattern. This method is limited to the analysis of simple geometric features and ignores subtle characteristics of diffraction patterns, such as variations in relative band intensities. A second method, developed to address the shortcomings of the Hough/Radon transform, is based on template matching of a test experimental pattern with a large library of potential patterns. In the present work, the template matching approach has been refined with a new cross correlation function that allows for a smaller library and enables a dramatic speed up in pattern indexing. Refinement of the indexed orientation is performed with a follow-up step to allow for small alterations to the best match from the library search. The orientation is further refined with rapid measurement of misorientation using whole pattern matching. The refined template matching approach is shown to be comparable in accuracy, precision and sensitivity to the Hough based method, even exceeding it in some cases, via the use of simulations and experimental data collected from a silicon single crystal and a deformed {\alpha}-iron sample. The drastic speed up and pattern refinement approaches should increase the widespread utility of pattern matching approaches., Comment: Article resubmitted for peer review, changes highlighted in red

The effect of Nb/Ti ratio on environmentally-assisted crack growth of three prototype Ni-based superalloys is studied. For these alloys, the yield strength is unaltered with increasing Nb/Ti ratio due to an increase in grain size. This situation has allowed the rationalization of the factors influencing damage tolerance at 700 °C. Primary intergranular cracks have been investigated using energy-dispersive X-ray spectroscopy in a scanning transmission electron microscope and the analysis of electron back-scatter diffraction patterns. Any possible detrimental effect of Nb on the observed crack tip damage due to Nb-rich oxide formation is not observed. Instead, evidence is presented to indicate that the tertiary γ′-precipitates are dissolving ahead of the crack consistent with the formation of oxides such as alumina and rutile. Our results have implications for alloy design efforts; at any given strength level, both more and less damage-tolerant variants of these alloys can be designed.

Grain boundary serration in the superalloy Inconel 600 was studied. Two microstructural variants, one with nonserrated and the other with serrated grain boundaries were generated by altering the heat-treatment conditions, while keeping other aspects of the microstructure unchanged. The effect on the creep response between 700 °C and 900 °C was measured, and the different failure modes and accumulated damage were quantified using high-angular resolution electron backscatter diffraction analysis in the scanning electron microscope and also by X-ray computed tomography. It is found that serration plays a more crucial role in the high-temperature/low-stress regime when an intergranular cracking mechanism involving cavitation is operative; here it plays a role in improving both creep life and creep ductility. Any effect of serration is less prevalent at low temperatures where transgranular failure is dominant.

The influence of statistics on calculated lattice strains has been studied by comparing crystal plasticity finite element (CPFE) calculations with strains measured experimentally. Experimentally, when Bragg's law is obeyed, a plane normal must lie within a narrow orientation range (∼ 0.02° for synchrotron diffraction), or Bragg tolerance. However, CPFE models consider only a small number of grains compared to experiments, necessitating a justification of the statistically representative volume. It also becomes necessary to assess the threshold of Bragg tolerance allowable for the determined statistically representative volume. In this study, an 8 × 8 × 8 model was deemed as statistically representative such that only small benefits are obtained in terms of lattice strain calculations by adopting larger models such as 10 × 10 × 10. Based on the selected model, an allowable Bragg tolerance of approximately 5° was calculated. Also highlighted was the coupling between lattice strain, texture, hardening and applied boundary condition which are discriminators that will affect the choice of model size and Bragg tolerance threshold. Keywords: Lattice strain, Statistics, Crystal plasticity, X-ray diffraction, Texture, Hardening

Micro s li p activation and localization in Ti - 6Al - 4V deformed in tension have been examined quantitatively using high - resolution (HR) digital image correlation (DIC) , HR - e lectron backscatter diffraction (EBSD) and crystal plasticity finite element modelling . The measured polycrystal slip, strain, lattice rotation and g eometrically necessary d islocation (GND ) density distributions are generally well captured by the a priori crystal plasticity model based on the rate - sensitive properties of α - titanium. An overall slip t race analysis showed over 80% agreement between HR - DIC and crystal plasticity modelling of th e primary slip activation . The texture beneath the characterised free - surface has been found to affect the local slip, stress distribution , lattice curvature and GND density and three texture variations have been considered . Grain - level slip trace analysis shows that the crystal plasticity modelling can capture single ( straight ) slip, multiple slip activation and complex wavy slip . The latter has been found to result from the interaction of independently activated basal and prismatic slip systems with common slip direction . I nitial inter - granular misorientations greater than about 5 o have been shown to influence the subsequent micromechanical grain behaviour including slip, lattice rotation and GND density. This work contrib utes to the understanding of slip localization and load shedding in dwell fatigue in polycrystalline hexagonal materials .

The deformation of polycrystalline zirconium is analysed at the individual grain level using three-dimensional Synchrotron X-ray Diffraction (3D-XRD) in combination with a Crystal Plasticity Finite Element (CPFE) model. The effects of elastic strains and lattice rotations on the shape and position of diffracted peaks are studied in detail. For this purpose, the three dimensional measured microstructure of a commercially pure zirconium (CPZr) sample was imported into a crystal plasticity finite element (CPFE) model to simulate the deformation of measured grains. The calculated lattice rotations and strains of the selected most active grains were subsequently used to forward simulate diffracted peaks. The simulated peaks are then compared to the 3D-XRD measured ones. It is shown that although the sample was deformed to 1.2% strain, soft grains exhibit significant peak smearing. Peak broadening is mostly affected by the deformation induced lattice rotation and less affected by the elastic strains. Further, the comparison of CPFE modelling and 3D-XRD results confirms that prism and basal slip are the most active systems and pyramidal is present but only slightly active. A method is developed to determine the activity of possible slip systems. As an example, by comparing the simulated and measured peak positions as well as the rotations of the most affected diffraction peaks, it is shown that pyramidal slip system is not active significantly at room temperature.

We used a range of advanced microscopy techniques to study the microstructure, nanoscale chemistry, and porosity in zirconium alloys at different stages of oxidation. Samples from both autoclave and in-reactor conditions were available, including ZIRLO™, Zr-1.0Nb, and Zr-2.5Nb samples with different heat treatments. Scanning transmission electron microscopy (STEM), transmission Kikuchi diffraction (TKD), and automated crystal orientation mapping with TEM were used to study the grain structure and phase distribution. Significant differences in grain morphology were observed between samples oxidized in the autoclave and in-reactor, with shorter, less well-aligned monoclinic grains and more tetragonal grains in the neutron-irradiated samples. A combination of energy-dispersive X-ray mapping in STEM and atom probe tomography analysis of second-phase particles (SPPs) can reveal the main and minor element distributions respectively. Neutron irradiation seems to have little effect on promoting fast oxidation or dissolution of β-niobium precipitates but encourages the dissolution of iron from Laves-phase precipitates. An electron energy-loss spectroscopy (EELS) analysis of the oxidation state of niobium in β-niobium SPPs in the oxide revealed the fully oxidized Nb5+ state in SPPs deep into the oxide but Nb2+ in crystalline SPPs near the metal-oxide interface. EELS analysis and automated crystal orientation mapping with TEM revealed Widmanstatten-type suboxide layers in some samples with the hexagonal ZrO structure predicted by ab initio modeling. The combined thickness of the ZrO suboxide and oxygen-saturated layers at the metal-oxide interface correlated well to the instantaneous oxidation rate, suggesting that this oxygen-rich zone is part of the protective oxide that is rate limiting in the transport processes involved in oxidation. Porosity in the oxide had a major influence on the overall rate of oxidation, and there was more porosity in the rapidly oxidizing annealed Zr-1.0Nb alloy than in either the recrystallized alloy or the similar alloy exposed to neutron irradiation.

We have used the cross-correlation based high resolution electron backscattering diffraction (HR-EBSD) technique to evaluate at high spatial resolution the spatial patterning of the type III intragranular residual stresses and geometrically necessary dislocation (GND) density within polycrystalline Cu after cyclic deformation. Oxygen free high conductivity (OFHC) polycrystalline copper samples were cyclically deformed under stress-control at a load ratio of 0.1 and EBSD measurements were made at points throughout the early stages of fatigue when strain amplitudes and cyclic creep rates are changing most significantly, namely at 0 cycles, 2 cycles, 200 cycles and 2000 cycles. Statistical analysis is presented showing that moderate correlations exist between stored GND density, residual intragranular stress and distance from the nearest grain boundaries and/or triple junctions.

The cross-correlation based HR-EBSD technique was used to derive stored geometrically necessary dislocation (GND) density in the OFHC copper samples deformed under uniaxial tension to true strain of 0%, 6%, 10%, 22.5% and 40%. Large maps (500 μm × 500 μm with 0.5 μm step size) with 1 million points and ∼1600 grains were acquired at each deformation level. Detailed studies on dislocation structure and evolution using the HR-EBSD were conducted. Distinct types of dislocation arrangements were revealed in grains with various orientations. For example, dislocation cells were formed in grains of orientation and dislocation bands were generally found in grains of and orientations. The complicated dislocation networks provide vital evidence to understand the deformation mechanisms in polycrystals at mesoscale. Quantitative analyses were also carried out to study this GND density orientation dependence in which Taylor factor was used as an indicator to quantify the grain resistance to deformation. It was found that points with high GND content preferentially accumulated in grains with high Taylor factor (‘hard’ grains) in deformed samples. This relation becomes stronger with increasing deformation.

Single α–β colony micro-cantilevers with an equilateral triangular cross-section and an apex at the bottom were machined from a polycrystalline commercial Ti–6Al–4V sample using a focused ion beam (FIB). Each cantilever contained several α lamellae separated by thin fillets of β. A nano-indenter was used to perform micro-bending tests (Ding et al., 2012) [1]. 〈c + a〉 Slip systems were selectively activated in the cantilevers by controlling the crystal direction along the micro-cantilever to be [0 0 0 1]. Specimens for transmission electron microscopy were prepared from the deformed micro-cantilevers using a dual-beam FIB. Bright field scanning transmission electron microscopy was used to investigate the processes of slip nucleation, propagation and transmission through the α/β interface. Dislocations initiate first near the bottom of the cantilever and subsequently from the top. Both sets of dislocations move inward toward the neutral axis. Planar pyramidal { 1 0 1 ¯ 1 } slip was observed at the top (tension) but cross-slip was observed at the bottom (compression). All the 〈c + a〉 slip systems are equally stressed, but only a limited number is activated. This is tentatively interpreted in terms of dislocation transmission through the β fillets.

In this study, we have used a Zr-Nb alloy containing well-defined nano-precipitates as a model material in which to study imaging contrast inversions (atomic number or diffraction contrast) observed with the forescattered electron imaging system, ARGUS™, in a scanning electron microscope (SEM) when imaging a thin foil in a transmission geometry. The study is based on Monte Carlo simulations and analysis of micrographs experimentally acquired under different imaging conditions. Based on the results, imaging conditions that enhance atomic number or diffraction contrast have been proposed. Data acquired from the ARGUS™ imaging system in an SEM has also been compared with results from standard transmission electron microscopy and scanning transmission electron microscopy imaging of the same material. These results demonstrate the capability of the ARGUS™ system to investigate microstructures in nano-scale materials.

We analyse the link between precision of pattern shift measurements and the resolution of the measurement of elastic strain and lattice rotation using high resolution electron backscatter diffraction (HR-EBSD). This study combines analysis of high quality experimentally obtained diffraction patterns from single crystal silicon; high quality dynamical simulations using Bloch wave theory; quantitative measurements of the detector Modulation Transfer Function (MTF) and a numerical model. We have found that increases in exposure time, when 1×1 binning is selected, are the primary reason for the observed increase in sensitivity at greater than 2×2 binning and therefore use of software integration and high bit depth images enables a significant increase in strain resolution. This has been confirmed using simulated diffraction patterns which provide evidence that the ultimate theoretical resolution of the cross correlation based EBSD strain measurement technique with a 1000×1000 pixel image could be as low as 4.2×10-7 in strain based on a shift precision of 0.001 pixels. © 2013 Elsevier B.V.

A discrete dislocation model was used to simulate residual stress fields close to deformation twins in stainless steels. Dislocation pairs were distributed along an initially elliptical twin boundary and an iterative scheme used to allow the dislocations to relax towards positions where the internal shear stresses were below a friction stress. The relaxed twin shape was close to elliptical but the flanks were flatter and the twin tips where the grain boundaries are situated were somewhat blunted compared to an ellipse. A dislocation-based boundary element model was then used to assess the interaction between the stress field from such twins and a crack. The stress field near the tip of the crack was characterized in terms of mode I and mode II stress intensity factors. The effects of twin width, length, orientation and distance from the crack tip on the strength of the interaction were studied. Wider, shorter twins were found to induce the largest stress intensity at the crack tip when close to the crack tip and aligned perpendicular to the crack plane. The influence of a pair of deformation twins does not significantly exceed the influence of a single deformation twin. © 2014 Elsevier B.V. All rights reserved.

A method is presented for the determination of elastic strains from electron back scatter diffraction patterns, which are obtained at high spatial resolution, from bulk specimens in a scanning electron microscope. It is estimated that the method is sensitive to strains of the order of 0.02%. Strains in Si(1-x)Ge(x) epitaxial layers grown on planar Si substrates were measured for x from 0.2 to 0.015, there being excellent agreement with X-ray diffraction results. Small lattice rotations can also be measured, the technique being sensitive to rotations of 0.01 degrees, which offers an improvement of approximately two orders of magnitude from the more usual EBSD measurements of misorientation. Small lattice rotations were measured in Si(0.85)Geo(0.15) grown on a patterned Si substrate and were consistent with elastic relaxation of the epilayer strain energy.