arXiv subjects

T. Ben Britton

Publications and source records attributed to T. Ben Britton.

At least 19 recordsLinked to original sources

arXiv2026

EBSD and Subtle Crystallographic Differences - A Study of Resolving Interlayer Spacings in Nb-Ni and Nb-Co mu-phases

In ordered intermetallics, slight variations in lattice site occupancy and specific interlayer spacings have been identified as the sources of significant changes in critical resolved shear stress and therefore how a given phase may affect alloy properties. So far, atom positions and lattice site occupancies have traditionally been characterised by high-resolution transmission electron microscopy (HR-TEM) and X-ray diffraction (XRD), which are methods that offer either local detail or high statistical significance but not both. Electron backscatter diffraction (EBSD), by contrast, provides high spatial resolution across large sample areas and therefore, has the potential to enable the local investigation of interlayer spacing and site lattice occupancy with improved statistical reliability. The objectives of the study are to benchmark EBSDs capability for resolving these subtle features and to correlate them with compositional and mechanical properties. In this case study, we therefore show that EBSD can resolve key crystallographic features of mu-phase intermetallics, specifically interlayer spacings. We combine pattern matching with large-scale dynamical simulations of template libraries guided by XRD based information on lattice parameters. For this, we generate structures that vary in the spacing between triple-layer and Kagome layer and in the site lattice occupancy of the 3a site. This approach successfully predicts the change of interlayer spacing between Kagome and triple layers in Nb-Co and Nb-Ni mu-phases, in good agreement with XRD and HR-TEM.

cond-mat.mtrl-sci↗

arXiv2026

Characterizing Dislocation Substructures in Creep-Deformed Olivine Using Electron Channeling Contrast Imaging

Olivine is the dominant mineral in Earth's upper mantle and therefore controls mantle rheology and the mechanics of plate tectonics. The constitutive laws for dislocation-mediated deformation of olivine depend on the nature, density, and arrangements of dislocations within crystals. Hence, imaging and characterizing these defects is important, albeit challenging. Traditional imaging approaches involve (1) transmission electron microscopy (TEM), which samples small areas and requires extensive preparation and (2) oxidation decoration methods that have low spatial resolution and cannot distinguish dislocations of opposite Burgers vectors. Here, we apply electron channeling contrast imaging (ECCI) to unlock insight into the deformation structures within olivine, and combined with electron backscatter diffraction (EBSD) and weighted Burgers vector (WBV) mapping as an informative route to characterize dislocation substructures in bulk materials. Specifically, we have used an ECCI workflow based on selected-area electron channeling patterns (SA-ECPs) and we apply this workflow to a single crystal of San Carlos olivine that was deformed by creep at high temperature. ECCI micrographs reveal subgrain boundaries, surface threading dislocations, and dislocation loops across representative areas. The observations demonstrate that this workflow can reliably reveal the complexity of subgrain boundaries in olivine, which can host multiple dislocation types and exhibit non-planar geometries. Despite the limited number of slip systems in olivine, subgrain boundaries can form complex, mixed assemblies. Overall, such observations can provide a variety of constraints on dislocation types, morphologies, and distributions, which are required to parameterize and calibrate models of transient and steady-state dislocation creep in olivine and other materials.

cond-mat.mtrl-sci↗

arXiv2026

Dynamical Simulation of On-axis Transmission Kikuchi and Spot Diffraction Patterns, Based on Accurate Diffraction Geometry Calibration

Transmission Kikuchi diffraction in the scanning electron microscope has gained popularity as a materials characterization technique for its high throughput and nanometer-level spatial resolution. While conventional diffraction pattern analysis routines focus on Kikuchi bands on the diffraction patterns, the full physical picture of electron scattering and diffraction pattern formation is more complex. Analysis that accounts for additional diffraction features such as diffraction spots and excess-deficiency effects should provide more robust and accurate indexing, if they can be incorporated in pattern indexing or simulation routines. A more accurate understanding of their physics of formation and geometry is required to enable this change. In this work, we demonstrate geometric and full contrast dynamical simulation of on-axis transmission Kikuchi patterns, based on experimental patterns captured using a modular, direct electron detector-based set-up in the scanning electron microscope. First, a diffraction geometry calibration routine is proposed based on the electron channeling pattern of the direct electron detector. This allows us to accurately account for the position of diffraction spots in both geometric and dynamical simulations with good agreement with experimental patterns. Further, by introducing appropriate weight factors, simulation of incoherent diffuse intensity, and calculation of the energy spectra of diffracted electrons, simulated patterns can be obtained which accurately capture the many diffraction features on experimental patterns. Workflows and findings of this work can be used to improve pattern indexing routines, as well as the understanding of the physical processes in the formation of on-axis transmission Kikuchi patterns.

cond-mat.mtrl-sci↗

arXiv2026

Polar Topologies in a Ferroelastic Metal Membrane

Polar metals, materials in which electric polarisation and metallicity coexist, are exceptionally rare because itinerant electrons screen long-range dipoles and favour centrosymmetric structures. Engineering polar textures in a conducting magnet holds promise for reconfigurable spin orbit coupling and magnetoelectric functionality. Here we show that releasing epitaxial SrRuO3 films from their substrates drives a hierarchy of ferroelastic domain refinement from micrometre to nanometre length scales, and that this structural reorganisation spontaneously generates two distinct classes of emergent polar texture that are ubiquitous across the freestanding membrane. Using correlative microscopy from mesoscale electron channelling contrast imaging (ECCI) to atomic resolution scanning transmission electron microscopy (STEM), we demonstrate that electric polarisation emerges selectively at translation-inequivalent antiphase boundaries (APBs). At these boundaries multicomponent aac tilt field undergoes Neel-like interpolation that preserves the in-phase tilt component and amplifies roto flexoelectric coupling, while translation-equivalent boundaries remain nonpolar. The Neel like interpolation at hard APBs and Ising like collapse of all tilt components at easy APBs is corroborated with ab initio calculations. While embedded 90 ferroelastic walls provide an additional mechanistically distinct source of electric polarisation resulting in polar nanoclusters (4 nm). These distinct nanotextures at 90 walls from via elastic accommodation of strain mismatch between variants and rotostriction as the tilt field interpolates across the boundaries. These findings show that, in a membrane form, metal oxides provide a robust platform for hosting nanoscale ferroelastic domains that generate polar textures.

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arXiv2026

Channeling-in channeling-out revisited: selected area electron channeling and electron backscatter diffraction

Scanning electron microscopy combined with electron backscatter diffraction (EBSD) and electron channeling provides rich crystallographic contrast, but the mutual influence of channeling-in and channeling-out is often simplified or neglected in quantitative analyses. In this work, we use selected-area electron channeling patterns (SA-ECPs) acquired from a single-crystal silicon wafer while recording an EBSD pattern at every incident beam direction, thereby directly probing how channeling-in affects the EBSD signal. We show that common Hough-based quality metrics (pattern quality, band contrast, and band slope), pattern-matching cross-correlation coefficients, and Fourier-based signal-to-noise ratios all exhibit strong crystallographic modulations that follow the underlying ECP, in both raw and background-corrected patterns. Similar wide-angle channeling features are also visible in conventional, low-magnification EBSD maps, indicating that channeling-in effects are relevant under routine mapping conditions and not only in specialized ECP experiments. These observations highlight that channeling-in can significantly bias quality-based interpretation of EBSD data, with consequences for methods such as pattern blurring analysis, high-resolution strain mapping, and emerging statistical or machine-learning approaches that rely on subtle variations in diffraction patterns. The combined SA-ECP and EBSD strategy presented here offers a practical framework to visualize and potentially control channeling-in/channeling-out coupling in the SEM, suggesting new routes to design experiments and detector configurations that either mitigate or intentionally exploit these dynamical effects.

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arXiv2025

Characterization of WSe$_2$ films using reflection Kikuchi diffraction in the scanning electron microscope and multivariate statistical analyses

The study of thin films and 2D materials, including transition metal dichalcogenides such as WSe$_2$ offers opportunities to leverage their properties in advanced sensors, quantum technologies, and device to optimize functional performance. In this work, we characterize thin WSe$_2$ samples with variable thicknesses using scanning electron microscope (SEM)-based techniques focused on analysis of backscattered electron signal and Kikuchi diffraction patterns. These data were collected via a pixelated electron-counting direct electron detector positioned below the pole piece primarily configured for reflection Kikuchi diffraction (RKD), and a similar detector placed in the more conventional electron backscatter diffraction geometry. In addition to conventional pattern analysis for orientation microscopy, multivariate statistical methods (MSA) based on principal component analysis were applied to analyze diffraction patterns and differentiate thickness variations and crystal orientations within the thin films through data clustering. These results were compared with atomic force microscopy to validate thickness measurements. Our findings indicate that RKD combined with MSA is highly effective for characterizing 2D materials, enabling simultaneous assessment of thickness and crystallographic orientation. Systematic acceleration voltage variations in RKD experiments and comparisons with EBSD data suggest that the thickness dependency arises from inelastic scattering of diffracted electrons, which affects pattern contrast in the thin film regime. Collection and analysis of patterns obtained from monolayer, bilayer and tri-layer of WSe$_2$ are also demonstrated. This work reinforces the utility of SEM-based techniques, such as RKD, as valuable tools for the materials characterization toolkit, particularly for thin films and 2D materials.

cond-mat.mtrl-sci↗

arXiv2025

AstroECP: towards more practical Electron Channeling Contrast Imaging

Electron channeling contrast imaging (ECCI) is a scanning electron microscopy (SEM) based technique that enables bulk-sample characterization of crystallographic defects (e.g. dislocations, stacking faults, low angle boundaries). Despite its potential, ECCI remains underused for quantitative defect analysis as compared to transmission electron microscope (TEM) based methods. Here, we overcome barriers that limit the use of ECCI including optimizing signal-to-noise contrast, precise determination of the incident beam vector with calibrated and easy to use simulations and experimental selected area electron channeling patterns (SA-ECP). We introduce a systematic ECCI workflow, alongside a new open-source software tool (AstroECP), that includes calibration of stage tilting, SA-ECP field of view, and the energy that forms the ECP/ECCI contrast using dynamical simulations. The functionality of this workflow is demonstrated with case studies that include threading dislocations in GaAs and the cross validation of precession based ECCI-contrast, which is otherwise known as Electron Channeling Orientation Determination (eCHORD). To assist the reader, we also provide best practice guidelines for ECCI implementation to promote high-resolution defect imaging in the SEM.

cond-mat.mtrl-sci↗

arXiv2025

Comparison of Kikuchi Diffraction Geometries in Scanning Electron Microscope

Recent advances in scanning electron microscope (SEM) based Kikuchi diffraction have demonstrated the important potential for reflection and transmission methods, like transmission Kikuchi diffraction (TKD) and electron backscatter diffraction (EBSD). Furthermore, with the advent of compact direct electron detectors (DED) it has been possible to place the detector in a variety of configurations within the SEM chamber. This motivates the present work where we explore the similarities and differences of the different geometries that include on-axis TKD & off-axis TKD using electron transparent samples, as well as more conventional EBSD. Furthermore, we compare these with the newest method called "reflection Kikuchi diffraction" RKD where the sample is placed flat in the chamber and the detector is placed below the pole piece. Through remapping collected diffraction patterns, all these methods can be used to generate an experimental "diffraction sphere" that can be used to explore diffraction from any scattering vector from the unit cell, as well as the ability to perform band profile analysis. This diffraction sphere approach enables us to further probe specific differences between the methods, including for example thickness effects in TKD that can result in the generation of diffraction spots, as well as electron scattering path length effects that result in excess and deficiency variations, as well as inversion of bands in experimental patterns.

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arXiv2024

Improving parent-austenite twinned grain reconstruction using electron backscatter diffraction in low carbon austenite

Thermomechanical controlled processing (TMCP) is widely used to optimize the final properties of high strength low alloy (HSLA) steels, via microstructure engineering. The room temperature microstructures are influenced by the high temperature austenite phase, and the austenite microstructure is commonly accessed by reconstruction using electron backscatter diffraction (EBSD) data of the final microstructure. A challenge for reconstruction of the PAG microstructure and subsequent austenite grain size measurement is the presence of austenite-phase annealing twins, and we address challenge with a new 're-sort' algorithm. Our algorithm has been validated using the retained austenite regions (which were recovered via advanced pattern matching of EBSD patterns). We demonstrate that the re-sort algorithm improves the PAG reconstruction significantly, especially for the grain boundary network and correlation with other methods of grain size assessment and development of TMCP steels.

cond-mat.mtrl-sci↗

arXiv2024

Improved understanding of the growth of blocky alpha in welded Zircaloy-4

Zirconium alloys are widely used in nuclear reactors as fuel cladding materials. Fuel cladding is used to contain the nuclear fuel and cladding tubes are typically sealed using welds. Welding of zirconium alloys can result in changes in the local microstructure, with the potential to grow so called 'blocky α' grains in the welded region during subsequent thermal processing and these blocky α grains have the potential to be detrimental to the integrity of the component. In this work, complimentary heating experiments with ex situ and in situ electron backscatter diffraction (EBSD) analysis are used to aid understanding of the blocky α grain growth within the weld region. These experiments reveal that blocky α grain growth is related to the parent \b{eta} (high temperature) microstructure, as grains grow adjacent to a prior \b{eta} grain boundary and the orientation of the growing α grain can be explained using neighbourhood orientations from this prior \b{eta} grain. This growth mechanism is explained via a simple mechanism which is related to the α grain orientations, grain boundary structures and local stored energy. Ultimately, our findings indicate that the likely grain growth (size and morphology) across the weld region can now be predicted from the initial as-welded microstructure.

cond-mat.mtrl-sci↗

arXiv2023

A simple, static and stage mounted direct electron detector based electron backscatter diffraction system

To engineer the next generation of advanced materials we must understand their microstructure, and this requires microstructural characterization. This can be achieved through the collection of high contrast, data rich, and insightful microstructural maps. Electron backscatter diffraction (EBSD) has emerged as a popular tool available within the scanning electron microscope (SEM), where maps are realized through the repeat capture and analysis of Kikuchi diffraction patterns. Typical commercial EBSD systems require large and sophisticated detectors that are mounted on the side of the SEM vacuum chamber which can be limiting in terms of widespread access to the technique. In this work, we present an alternative open-hardware solution based upon a compact EBSD system with a simple, static geometry that uses an off-the-shelf direct electron detector co-mounted with a sample. This simple stage is easy to manufacture and improves our knowledge of the diffraction geometry significantly. Microscope and detector control is achieved through software application programming interface (API) integration. After pattern capture, analysis of the diffraction patterns is performed using open-source analysis within AstroEBSD. To demonstrate the potential of this set up, we present two simple EBSD experiments using line scan and mapping. We hope that the present system can inspire simpler EBSD system design for widespread access to the EBSD technique and promote the use of open-source software and hardware in the workflow of EBSD experiments.

cond-mat.mtrl-sci↗

arXiv2023

Multi-exposure diffraction pattern fusion applied to enable wider-angle transmission Kikuchi diffraction with direct electron detectors

Diffraction pattern analysis can be used to reveal the crystalline structure of materials, and this information is used to nano- and micro-structure of advanced engineering materials that enable modern life. For nano-structured materials typically diffraction pattern analysis is performed in the transmission electron microscope (TEM) and TEM diffraction patterns typically have a limited angular range (less than a few degrees) due to the long camera length, and this requires analysis of multiple patterns to probe a unit cell. As a different approach, wide angle Kikuchi patterns can be captured using an on-axis detector in the scanning electron microscope (SEM) with a shorter camera length. These 'transmission Kikuchi diffraction' (TKD) patterns present a direct projection of the unit cell and can be routinely analyzed using EBSD-based methods and dynamical diffraction theory. In the present work, we enhance this analysis significantly and present a multi-exposure diffraction pattern fusion method that increases the dynamic range of the detected patterns captured with a Timepix3-based direct electron detector (DED). This method uses an easy-to-apply exposure fusion routine to collect data and extend the dynamic range, as well as normalize the intensity distribution within these very wide (>95°) angle patterns. The potential of this method is demonstrated with full diffraction sphere reprojection and highlight potential of the approach to rapidly probe the structure of nano-structured materials in the scanning electron microscope.

cond-mat.mtrl-sci↗

arXiv2023

Accessing slip activity in high purity tin with electron backscatter diffraction and measurement of slip strength

Beta-tin has been used widely as an interconnect in modern electronics. To improve the understanding of the reliability of these components, we directly measure the critical resolved shear stress of individual slip systems in beta-tin using micropillar compression tests at room temperature with crystal orientations near-[100] and [001] in the loading direction within a large grain high purity tin (99.99%) sample. This activates the (110)[1-11]/2, (110)[1-1-1]/2, (010)[001] and (110)[001] slip systems. Analysis of the slip traces and load-displacement curves enables measurement of the critical resolved shear stress for epsilon=10^(-4) of tau_(CRSS)^({110}<1-11>/2)=10.4+/-0.4 and tau_(CRSS)^({010}<001>)=3.9+/-0.3 MPa.

cond-mat.mtrl-sci↗

arXiv2023

Characterization of local deformation around hydrides in Zircaloy-4 using conventional and high angular resolution electron backscatter diffraction

Zircaloy-4 is used as a fuel cladding material for water reactors, as it has good mechanical properties, corrosion resistance, and a low thermal neutron absorption cross section. However, the mechanical performance of Zircaloy-4 can be reduced during service due to hydrogen uptake and hydride formation. These hydrides are brittle, and often reduce the strength and toughness of materials as well as increase susceptibility to delayed hydride cracking (DHC). In this work, large grain Zircaloy-4 with hydrides was prepared and then cross sectioned using cryo-ion beam polishing, using plasma focused ion beam (pFIB) and broad ion beam (BIB) approaches to enable the preparation of a very high quality flat surface with no preferential etching of either the hydride or zirconium metal (typically metallographic polishing preferentially removes hydrides). Conventional and high angular resolution electron backscatter diffraction (EBSD) analysis were then used to explore morphology, deformation fields, and orientation relationships between the zirconium matrix and hydrides. Four maps were collected for analysis which included hydrides near grain boundaries: (a) where the hydride smoothly decorates across two of the connecting boundaries near a triple junction; (b) where the hydride smoothly decorates the boundary; (c) a mixture of smooth decoration of the interface and protrusion into the grains; (d) fine scale hydride that protrudes into one grain. This work highlights that incompatibility of the hydride within the zirconium matrix is strongly linked to the orientation relationship of the hydride and matrix, and the grain boundary character. These results may enable enhanced understanding of the role of hydrides in fracture as well as stress-induced hydride reorientation and DHC susceptibility.

cond-mat.mtrl-sci↗

arXiv2023

Transmission Kikuchi diffraction mapping induces structural damage in atom probe specimens

Measuring local chemistry of specific crystallographic features by atom probe tomography (APT) is facilitated by using transmission Kikuchi diffraction (TKD) to help position them sufficiently close to the apex of the needle-shaped specimen. However, possible structural damage associated to the energetic electrons used to perform TKD is rarely considered and is hence not well-understood. Here, in two case studies, we evidence damage in APT specimens from TKD mapping. First, we analyze a solid solution, metastable \b{eta}-Ti-12Mo alloy, in which the Mo is expected to be homogenously distributed. Following TKD, APT reveals a planar segregation of Mo amongst other elements. Second, specimens were prepared near Σ3 twin boundaries in a high manganese twinning-induced plasticity steel, and subsequently charged with deuterium gas. Beyond a similar planar segregation, voids containing a high concentration of deuterium, i.e. bubbles, are detected in the specimen on which TKD was performed. Both examples showcase damage from TKD mapping leading to artefacts in the compositional distribution of solutes. We propose that the structural damage is created by surface species, including H and C, subjected to recoil from incoming energetic electrons during mapping, thereby getting implanted and causing cascades of structural damage in the sample.

cond-mat.mtrl-sci↗

arXiv2022

Multi-scale plasticity homogenization of Sn-3Ag-0.5Cu: from β-Sn micropillars to polycrystals with intermetallics

The mechanical properties of $β$-Sn single crystals have been systematically investigated using a combined methodology of micropillar tests and rate-dependent crystal plasticity modelling. The slip strength and rate sensitivity of several key slip systems within $β$-Sn single crystals have been determined. Consistency between the numerically predicted and experimentally observed slip traces has been shown for pillars oriented to activate single and double slip. Subsequently, the temperature-dependent, intermetallic-size-governing behaviour of a polycrystal $β$-Sn-rich alloy SAC305 (96.5Sn-3Ag-0.5Cu wt%) is predicted through a multi-scale homogenization approach, and the predicted temperature- and rate-sensitivity reproduce independent experimental results. The integrated experimental and numerical approaches provide mechanistic understanding and fundamental material properties of microstructure-sensitive behaviour of electronic solders subject to thermomechanical loading, including thermal fatigue.

cond-mat.mtrl-sci↗

arXiv2022

Optimizing broad ion beam polishing of zircaloy-4 for electron backscatter diffraction analysis

Microstructural analysis with electron backscatter diffraction (EBSD) involves sectioning and polishing to create a flat and preparation-artifact free surface. The quality of EBSD analysis is often dependant on this step, and this motivates us to explore how broad ion beam (BIB) milling can be optimised for the preparation of zircaloy-4 with different grain sizes. We systematically explore the role of ion beam angle, ion beam voltage, polishing duration and polishing temperature and how this changes the surface roughness and indexing quality. Our results provide a method to routinely prepare high-quality Zircaloy-4 surfaces, and methods to optimise BIB polishing of other materials for high-quality EBSD studies.

cond-mat.mtrl-sci↗

arXiv2021

Nanoscale characterisation of hydrides and secondary phase particles in Zircaloy-4

The interaction of hydrogen and metals continues to be industrially relevant and is a critical part of creating and supporting a safety case for nuclear reactor operation. In the present work, we explore hydrogen storage and hydride formation in a zirconium alloy. We characterise the structure and interfaces of fine scale hydrides using scanning transmission electron microscopy (STEM) including energy dispersive spectroscopy (EDS/EDX), electron energy loss spectroscopy (EELS), and high-resolution STEM. Chemical characterisation is supported further with atom probe tomography (APT). Samples were prepared with cryo-focussed ion beam machining (cryo-FIB) and contain hydrides in α-Zr matrix and hydrides associated with one FeCrZr secondary phase particle (SPP). Major findings include characterisation of different interface planes based upon the size of the hydrides and chemical redistribution of solute ahead of the hydride-metal interface. We also find significant (up to 6 at%) hydrogen retained in solution within the zirconium matrix and show a hydride with only 17 at% hydrogen, which is well below that of a ξ-phase stoichiometry suggesting it is an embryonic hydride. These findings help us understand the distribution of hydrogen and the nanoscale morphology of hydrides, which may influence the lifetime of zirconium-based nuclear fuel cladding.

cond-mat.mtrl-sci↗