arXiv subjects

Angus J. Wilkinson

Publications and source records attributed to Angus J. Wilkinson.

17 recordsLinked to original sources

arXiv2023

An iterative method for reference pattern selection in high resolution electron backscatter diffraction (HR-EBSD)

For high (angular) resolution electron backscatter diffraction (HR-EBSD), the selection of a reference diffraction pattern (EBSP0) significantly affects the precision of the calculated strain and rotation maps. This effect was demonstrated in plastically deformed body-centred cubic and face-centred cubic ductile metals (ferrite and austenite grains in duplex stainless steel) and brittle single-crystal silicon, which showed that the effect is not only limited to measurement magnitude but also spatial distribution. An empirical relationship was then identified between the cross-correlation parameter and angular error, which was used in an iterative algorithm to identify the optimal reference pattern that maximises the precision of HR-EBSD.

cond-mat.mtrl-sci↗

arXiv2022

HR-EBSD analysis of in situ stable crack growth at the micron scale

Understanding the local fracture resistance of microstructural features. such as brittle inclusions, coatings, and interfaces at the microscale under complex loading conditions is critical for microstructure-informed design of materials. In this study, a novel approach has been formulated to decompose the J-integral evaluation of the elastic energy release rate to the three-dimensional stress intensity factors directly from experimental measurements of the elastic deformation gradient tensors of the crack field by in situ high (angular) resolution electron backscatter diffraction (HR-EBSD). An exemplar study is presented of a quasi-static crack, inclined to the observed surface, propagating on low index {hkl} planes in a (001) single crystal silicon wafer.

cond-mat.mtrl-sci↗

arXiv2022

Macroscopic analysis of time dependent plasticity in Ti alloys

Component failure due to cold dwell fatigue of titanium and its alloys is a long-standing problem which has significant safety and economic implications to the aviation industry. This can be addressed by understanding the governing mechanisms of time dependent plasticity behaviour of Ti at low temperatures. Here, stress relaxation tests were performed at four different temperatures on three major alloy systems: commercially pure titanium (two alloys with different oxygen content), Ti-6Al-4V (two microstructures with differing beta phase fractions) and Ti-6Al-2Sn-4Zr-xMo (two alloys with different Mo content x= 2 or 6, and portion of beta phase). Key parameters controlling the time dependent plasticity were determined as a function of temperature. Both activation volume and energy were found to increase with temperature in all six alloys. It was found that the dwell fatigue effect is more significant by oxygen alloying but is suppressed by the addition of Mo. The presence of the beta phase did not strongly affect the dwell fatigue, however, it was suppressed at high temperature due to the low strain rate and strain rate sensitivity.

cond-mat.mtrl-sci↗

arXiv2021

Weighted ellipse fitting routine for spotty or incomplete Debye-Scherrer rings on a 2D detector

We introduce a weighted ellipse fitting routine to measure Debye Scherrer rings acquired on 2D area detectors and demonstrate its use in strain determination. The method is relatively robust against incomplete rings due to low number of grains in the diffraction volume (spotty rings), or strong texture (intensity depletion in some azimuths). The method works by applying an annular mask around each diffraction ring and fitting an ellipse, using all pixel positions and their diffracted intensity as weights in the minimisation. We compare this method to the more popular cake integration method, and show that the weighted ellipse method works when the cake integration method fails or works poorly. The lattice strain sensitivity from spotty diffraction rings is in the order or 2E-5 or better. The algorithm has been made available for public use and works with 2D diffraction patterns acquired in a laboratory scale XRD equipment, TEM or a synchrotron.

physics.app-ph↗

arXiv2021

Cold dwell behaviour of Ti$_6$Al alloy: Understanding load shedding using digital image correlation and crystal plasticity simulations

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.

cond-mat.mtrl-sci↗

arXiv2020

High resolution electron backscatter diffraction study on the heterogeneities of tetragonal distortion in Fe-C martensite at the microstructural scale

The spatial variation in martensite tetragonality (c/a ratio) in Fe-0.77C (wt.%) alloy was investigated by means of pattern matching of electron backscatter diffraction patterns combined with high angular resolution electron backscatter diffraction analysis. It was found that the c/a ratio varies within a martensite block and between blocks. The c/a variation within a block is particularly evident in the vicinity of grain boundaries and shear strains are also present in addition to tetragonal distortion. The c/a variation between blocks is more apparent than that within a block. The lattice parameter frequency profile predicted by our approach well matches with the X-ray diffraction profile from the same material by assuming reasonable residual strain acting on a- and b-axes. The heterogeneities of the crystal distortion are brought by a decrease and scatter in solid solution carbon and in carbon ordering as a result of the martensite transformation sequence as well as heterogeneous residual strain.

cond-mat.mtrl-sci↗

arXiv2020

An in-situ synchrotron diffraction study of stress relaxation in titanium: Effect of temperature and oxygen on cold dwell fatigue

There is a long-standing technological problem in which a stress dwell during cyclic loading at room temperature in Ti causes a significant fatigue life reduction. It is thought that localised time dependent plasticity in soft grains favourably 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 understand the complex cold dwell fatigue problem. Knowing the effect of operating temperature and oxygen content on cold dwell fatigue will be beneficial for future alloy design to address this problem. In this work, synchrotron X-ray diffraction during stress relaxation experiments was used to characterise 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, 75C, 145C and 250C). Lattice strains were measured by tracking the diffraction peak shift from multiple crystallographic 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 slip as a function of temperature and oxygen content by fitting a crystal plasticity finite element model to the lattice strain relaxation responses measured along the loading axis for five strong reflections. Higher strain rate sensitivity was found to lead to higher plasticity during cold dwell.

cond-mat.mtrl-sci↗

arXiv2020

Dislocation interactions in olivine control postseismic creep of the upper mantle

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°C or 1150 to 1250°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.

cond-mat.mtrl-sci↗

arXiv2020

Grain Boundary Serration in Nickel Alloy Inconel 600: Quantification and Mechanisms

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.

cond-mat.mtrl-sci↗

arXiv2019

Dislocation interactions during low-temperature plasticity of olivine strengthen the lithospheric mantle

The strength of the lithosphere is typically modelled based on constitutive equations for steady-state flow. However, models of lithospheric flexure reveal differences in lithospheric strength that are difficult to reconcile based on such flow laws. Recent rheological data from low-temperature deformation experiments on olivine suggest that this discrepancy may be largely explained by strain hardening. Details of the mechanical data, specifically the effects of temperature-independent back stresses stored in the samples, indicate that strain hardening in olivine occurs primarily due to long-range elastic interactions between dislocations. These interpretations provided the basis for a new flow law that incorporates hardening by development of back stress. Here, we test this hypothesis by examining the microstructures of olivine samples deformed plastically at room temperature either in a deformation-DIA apparatus at differential stresses of < 4.3 GPa or in a nanoindenter at applied contact stresses of > 10.2 GPa. High-angular resolution electron backscatter diffraction maps reveal the presence of geometrically necessary dislocations with densities commonly above 10$^{14}$ m$^{-2}$ and intragranular heterogeneities in residual stress on the order of 1 GPa in both sets of samples. Scanning transmission electron micrographs reveal straight dislocations aligned along slip bands and interacting with dislocations of other types that act as obstacles. The stress heterogeneities and accumulations of dislocations along their slip planes are consistent with strain hardening resulting from long-range back-stresses acting between dislocations. These results corroborate the mechanical data in supporting the form of the new flow law for low-temperature plasticity and provide new microstructural criteria for identifying the operation of this deformation mechanism in natural samples.

physics.geo-ph↗

arXiv2019

Dislocation density distribution at slip band-grain boundary intersections

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.

cond-mat.mtrl-sci↗

arXiv2019

Warren-Averbach line broadening analysis from a time of flight neutron diffractometer

The well known Warren-Averbach theory of diffraction line profile broadening is shown to be applicable to time of flight data obtained from a neutron spallation source. Without modification, the method is applied to two very different examples; a cold worked ferritic steel and a thermally stressed alumina-30% SiC composite. Values of root mean square strains averaged over a range of lengths for the ferritic steel were used to estimate dislocation densities; values were found to be in good agreement with geometrically necessary dislocation densities independently measured from similarly orientated grains measured from electron backscatter diffraction analysis. An analytical model for the ceramic is described to validate the estimate of root mean square strain.

cond-mat.mtrl-sci↗

arXiv2019

High-angular resolution electron backscatter diffraction as a new tool for mapping lattice distortion in geological minerals

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.

cond-mat.mtrl-sci↗

arXiv2019

Pattern Matching Analysis of Electron Backscatter Diffraction Patterns for Pattern Centre, Crystal Orientation and Absolute Elastic Strain Determination: Accuracy and Precision Assessment

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.

cond-mat.mtrl-sci↗

arXiv2019

Forescattered electron imaging of nanoparticles in a scanning electron microscopy

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, ARGUSTM, 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 ARGUSTM imaging system in 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 ARGUSTM system to investigate microstructures in nano-scale materials.

cond-mat.mtrl-sci↗

arXiv2019

On the depth resolution of transmission Kikuchi diffraction (TKD) analysis

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.

cond-mat.mtrl-sci↗

arXiv2018

Mapping the full lattice strain tensor of a single dislocation by High Angular Resolution Transmission Kikuchi Diffraction (HR-TKD)

The full lattice strain tensor and lattice rotations induced by a dislocation in pure tungsten were mapped using high-resolution transmission Kikuchi diffraction (HR-TKD) in a SEM. The HR-TKD measurement agrees very well with a forward calculation using an elastically isotropic model of the dislocation and its Burgers vector. Our results demonstrate that the spatial and angular resolution of HR-TKD in SEM is sufficiently high to resolve the details of lattice distortions near individual dislocations. This capability opens a number of new interesting opportunities, for example determining the Burgers vector of an unknown dislocation in a fast and straightforward way.

cond-mat.mtrl-sci↗