arXiv subjects

James A. D. Ball

Publications and source records attributed to James A. D. Ball.

11 recordsLinked to original sources

arXiv2026

Subgrain-resolved Analysis of Degradation in Cu Metallization via Scanning 3DXRD and Thermomechanical Modeling

Metallization layers play a key role in the performance and reliability of modern power semiconductor devices. During short-circuit events, rapid heating of power metallization layers induces thermomechanical incompatibility stresses, which may contribute to material degradation and impact device performance. In this work, potential degradation hotspots associated with thermomechanical loading in Cu power metallization are investigated using a combined experimental--computational approach. Scanning three-dimensional X-ray diffraction measurements are coupled with thermomechanical crystal plasticity simulations to probe the evolution of grain-resolved plastic deformation during rapid cyclic loading. This integrated approach provides insight into the microstructural processes governing degradation hotspot formation, laying the groundwork for future microstructure-informed, physics-based reliability assessment of Cu metallization.

cond-mat.mtrl-sci↗

arXiv2026

Unravelling the mechanisms underlying crack initiation in additively manufactured steel

Metal additive manufacturing (AM) is increasingly adopted for safety-critical applications across the biomedical, aerospace, and energy sectors. However, many AM alloys exhibit substantially lower fracture toughness and shorter fatigue lives than their wrought counterparts, limiting their structural reliability. The microscale mechanisms governing this deficit remain obscured because the evolution of crack-tip deformation cannot be directly resolved using conventional characteriza-tion techniques. Here, we combine in situ multimodal synchrotron X-ray diffraction with phase-contrast tomography to directly observe the three-dimensional evolution of crack-tip plasticity dur-ing loading. We find that wrought steel develops a localized crack-tip process zone characterized by extensive geometrically necessary dislocation (GND) accumulation, effective stress relaxation, and crack-tip blunting. This plastic zone provides shielding of the crack tip by redistributing defor-mation and reducing the local driving force for crack initiation. In contrast, the AM alloy exhibits suppressed GND evolution, limited crack-tip blunting, and persistent elevated stresses over an ex-tended region ahead of the crack tip, indicating ineffective stress relaxation and premature crack initiation. These findings demonstrate that fracture resistance is governed by the spatial evolution of crack-tip plasticity, providing a mechanistic framework for improving the damage tolerance of AM structural alloys.

cond-mat.mtrl-sci↗

arXiv2026

Revealing 3D orientation and strain heterogeneity in calcite generated by bio-cementation

Bio-cementation uses bacterially induced calcite to bind sand grains, offering a low-carbon approach to soil stabilization. However, the 3D morphology, orientation texture, and internal strain states of individual calcite bonds remain insufficiently characterized. Here, we combine computed micro-tomography, 3D X-ray Diffraction (3DXRD), and Dark-Field X-ray Microscopy (DFXM) to nondestructively characterize grain morphology, crystallographic orientation, and both type II (intergranular) and type III (intragranular) elastic strains in calcite formed at sand-sand contacts during bio-cementation. Tomography establishes the sample morphology and the cemented contact architecture; 3DXRD provides grain-averaged orientation and strain states; and DFXM resolves sub-grain misorientations and localized strain concentrations generated during growth with 100 nm resolution. The combined results show that calcite precipitation through bio-cementation produces anisotropic internal strain and distinct sub-domain structures that can influence bond integrity and load transfer at the macroscopic scale.

cond-mat.mtrl-sci↗

arXiv2026

Revealing 3D Strain and Carbide Architectures in Additively Manufactured Ni Superalloys

Fast directional solidification during Laser Additive Manufacturing (LAM) produces a complex microstructure in nickel-based superalloys, comprising columnar grains with cellular sub-grain structures and carbides. Using non-destructive Scanning 3D X-ray Diffraction (S3DXRD), we reveal spatially complex orientation and intergranular strain relationships that couple strongly to processing-induced cellular sub-grain networks and a primary cubic metal carbide (MC) phase. We have examined 3D orientation and elastic strain tensor fields across 82 $γ$ grains together with the spatial distribution of over 37,000 MC carbides in an ABD-900AM alloy sample manufactured by the Directed Energy Deposition (DED) LAM process. Carbides are spatially associated with the cellular sub-grain network with a weak but present orientation relationship with their parent $γ$ grains. The MC carbides, known to be Ti, Ta and Nb rich, form in regions of high solute segregation, resulting in a significant volumetric lattice parameter patterning in the associated $γ$ phase regions. These chemically distinct solute-rich regions possess a higher associated elastic modulus compared to intercellular regions and determine the local residual stress patterning. These results provide the first non-destructive 3D study of the relationship between rapid solidification-induced segregation, deformation heterogeneity and carbide architectures in an additively manufactured Ni-based superalloy. The insights provide crucial detail to rationalise LAM process parameter optimisation and the coupled spatially governed structural performance.

cond-mat.mtrl-sci↗

arXiv2025

Halogen Chains with One-Dimensional Semi-Metallic Electronic Structure and Peierls Physics in Polymorphs of Na4X5 (X = I, Br, Cl) Compounds

Since the pioneering works of Peierls, one-dimensional materials have attracted great attention. Still, the synthesis of truly monoatomic chains remains elusive. In this study, we explore a novel path of experimental synthesis of monoatomic one-dimensional chains by their chemical stabilization in ionic compounds. We demonstrate that in synthesized at high pressure sodium halides Na4X5 (X = I, Br, Cl) with hP18 Ga4Ti5-type structures, transfer of valence electrons from cations to anions leads to the formation of halogen chains connected with other atoms only by ionic interaction and having one-dimensional electronic structure. The Peierls physics in the systems is confirmed by theoretical calculations, newly synthesized incommensurately modulated i-hP18-Na4X5 (X = I, Br, Cl) compounds, as well as by the discovered hP36 phases of Na4Cl5 and Na4Br5.

cond-mat.mtrl-sci↗

arXiv2025

Bridging Grain Mapping and Dark Field X-ray Microscopy for Multiscale Diffraction Imaging

Resolving how defects emerge and interact within the hierarchical structure of polycrystalline materials remains a core challenge in materials science. Grain-mapping methods such as three-dimensional X-ray diffraction (3DXRD) and diffraction contrast tomography (DCT) provide essential mesoscale context but lack the resolution to image lattice defects. Conversely, high-resolution methods like Dark Field X-ray Microscopy (DFXM) capture lattice distortions but not the surrounding microstructure. Here, we introduce a transferable framework that unifies these complementary approaches into a single, non-destructive workflow. Enabled by open-source software, the method translates grain orientation and position data into precise goniometer settings for DFXM imaging without dismounting or reorienting the sample. Applied to an iron polycrystal containing 1100 grains, DFXM motor positions were calculated for all grains within seconds, enabling on-the-fly targeting of specific grains. This allows reproducible zooming from the millimetre-scale aggregate to individual dislocations. We resolve three-dimensional misorientation fields across grain boundaries with 36 nm pixel size, directly capturing grain-grain interactions within their microstructural context. Finally, we show transferability from LabDCT to synchrotron and XFEL platforms, enabling new ways of studying defect interactions across scales.

physics.app-ph↗

arXiv2025

Ultimate Sensitivity in X-ray Diffraction: Angular Moments vs. Shot Noise

The sensitivity of x-ray diffraction experiments towards Bragg peak parameters constitutes a crucial performance attribute of experimental setups. Frequently, diffraction peaks are characterized by model-free angular moment analysis, which offers a greater versatility compared to traditional model-based peak fitting. Here, we have determined the ultimate sensitivity of angular moments for diffraction data that is limited by photon shot noise. We report experimentally achieved sensitivities of the first moment below $1/1000$th of a detector pixel and below $1μ$rad. We have demonstrated the validity of our theoretical predictions by an excellent agreement with experimental results from three different setups. The provided formulas for the uncertainties of angular moments allow for the rapid determination of experimentally achieved sensitivities from single diffraction frames.

physics.optics↗

arXiv2023

Grain-level effects on in-situ deformation-induced phase transformations in a complex-phase steel using 3DXRD and EBSD

A novel complex-phase steel alloy is conceived with a deliberately unstable austenite, $γ$, phase that enables the deformation-induced martensitic transformations (DIMT) to be explored at low levels of plastic strain. The DIMT was thus explored, in-situ and non-destructively, using both far-field Three-Dimensional X-Ray Diffraction (3DXRD) and Electron Back-Scatter Diffraction (EBSD). Substantial $α'$ martensite formation was observed under 10% applied strain with EBSD, and many $\varepsilon$ grain formation events were captured with 3DXRD, indicative of the indirect transformation of martensite via the reaction $γ\rightarrow \varepsilon \rightarrow α'$. Using $\varepsilon$ grain formation as a direct measurement of $γ$ grain stability, the influence of several microstructural properties, such as grain size, orientation and neighbourhood configuration, on $γ$ stability have been identified. Larger $γ$ grains were found to be less stable than smaller grains. Any $γ$ grains oriented with {100} parallel to the loading direction preferentially transformed with lower stresses. Parent $\varepsilon$-forming $γ$ grains possessed a neighbourhood with increased ferritic/martensitic volume fraction. This finding shows, unambiguously, that $α$/$α'$ promotes $\varepsilon$ formation in neighbouring grains. The minimum strain work criterion model for $\varepsilon$ variant prediction was also evaluated, which worked well for most grains. However, $\varepsilon$-forming grains with a lower stress were less well predicted by the model, indicating crystal-level behaviour must be considered for accurate $\varepsilon$ formation. The findings from this work are considered key for the future design of alloys where the deformation response can be controlled by tailoring microstructure and local or macroscopic crystal orientations.

cond-mat.mtrl-sci↗

arXiv2023

Registration between DCT and EBSD datasets for multiphase microstructures

The ability to characterise the three-dimensional microstructure of multiphase materials is essential for understanding the interaction between phases and associated materials properties. Here, laboratory-based diffraction-contrast tomography (DCT), a recently-established materials characterization technique that can determine grain phases, morphologies, positions and orientations in a voxel-based reconstruction method, was used to map part of a dual-phase steel alloy sample. To assess the resulting microstructures that were produced by the DCT technique, an EBSD map was collected within the same sample volume. To identify the 2D slice of the 3D DCT reconstruction that best corresponded to the EBSD map, a novel registration technique based solely on grain-averaged orientations was developed -- this registration technique requires very little a priori knowledge of dataset alignment and can be extended to other techniques that only recover grain-averaged orientation data such as far-field 3D X-ray diffraction microscopy. Once the corresponding 2D slice was identified in the DCT dataset, comparisons of phase balance, grain size, shape and texture were performed between DCT and EBSD techniques. More complicated aspects of the microstructural morphology such as grain boundary shape and grains less than a critical size were poorly reproduced by the DCT reconstruction, primarily due to the difference in resolutions of the technique compared with EBSD. However, lab-based DCT is shown to accurately determine the centre-of-mass position, orientation, and size of the large grains for each phase present, austenite and martensitic ferrite. The results reveals a complex ferrite grain network of similar crystal orientations that are absent from the EBSD dataset. Such detail demonstrates that lab-based DCT, as a technique, shows great promise in the field of multi-phase material characterization.

cond-mat.mtrl-sci↗

arXiv2023

Per-grain and neighbourhood stress interactions during deformation of a ferritic steel obtained using three-dimensional X-ray diffraction

Three-dimensional X-ray diffraction (3DXRD) has been used to measure, in-situ, the evolution of $\sim 1800$ grains in a single phase low carbon ferritic steel sample during uniaxial deformation. The distribution of initial residual grain stresses in the material was observed to prevail as plasticity builds, though became less pronounced, and therefore less influential as strain increased. The initial Schmid factor of a grain was found to be strongly correlated to the intergranular stress change and the range of stresses that are permissible; a grain well aligned for easy slip is more likely to exhibit a range of stresses than those orientated poorly for dislocation motion. The orientation path of a grain, however, is not only dependent on its initial orientation, but hypothesised to be influenced by its stress state and the stress state of its grain environment. A grain neighbourhood effect is observed: the Schmid factor of serial adjoining grains influences the stress state of a grain of interest, whereas parallel neighbours are much less influential. This phenomenon is strongest at low plastic strains only, with the effect diminishing as plasticity builds. The influence of initial residual stresses becomes less evident, and grains rotate to eliminate any orientation dependent load shedding. The ability of the BCC ferrite to exhaust such neighbourhood interactions, which would otherwise be detrimental in crystal structures with lower symmetric and fewer slip systems, is considered key to the high ductility possessed by these materials.

cond-mat.mtrl-sci↗

arXiv2023

Implementing and evaluating far-field 3D X-ray diffraction at the I12 JEEP beamline, Diamond Light Source

Three-dimensional X-ray diffraction (3DXRD) is shown to be feasible at the I12 Joint Engineering, Environmental and Processing (JEEP) beamline of Diamond Light Source. As a demonstration, a microstructually simple low-carbon ferritic steel was studied in a highly textured and annealed state. A processing pipeline suited to this beamline was created, using software already established in the 3DXRD user community, enabling grain centre-of-mass positions, orientations and strain tensor elements to be determined. Orientations, with texture measurements independently validated from electron backscatter diffraction (EBSD) data, possessed a $\sim 0.1^\circ$ uncertainty, comparable with other 3DXRD instruments. The spatial resolution was limited by the far-field detector pixel size; the average of the grain centre of mass position errors was determined as $\pm \sim 80 μ$m. An average per-grain error of $\sim 1 \times 10^{-3}$ for the elastic strains was also measured; this could be reduced in future experiments by improving sample preparation, data collection and analysis techniques. Application of 3DXRD onto I12 shows great potential, where its implementation is highly desirable due the flexible, open architecture of the beamline. User-owned or designed sample environments can be used, thus 3DXRD could be applied to previously unexplored scientific areas.

cond-mat.mtrl-sci↗